CONSILIUL project proposal... · Web view- the project proposes catalysts preparation using both classic methods (impregnation) and new techniques (sol-gel). New catalysts will be

Funding Application for Joint Applied Research ProjectsPN-II-PT-PCCA-2011-3

Hydrogen production from hydroxylic compounds resulted as biomass

processing wastes

Acronim HYCAT

PN-II-PT-PCCA-2011-31

1. Importance and Relevance of the Technical and/or Scientific Content

(max 20 pages)1.1. Concept and objectives:

The concept of the project

The project “Hydrogen production from hydroxylic compounds resulted as biomass

processing wastes” is proposed to Joint Applied Research Projects Competition for Domain 2:

Energy Research direction 2.1.4. The project application fits in the above mentioned domain

and direction because it proposes the energetic valorization of waste glycerol obtained in

biodiesel fabrication by its transformation in hydrogen – a very promising energy vector. This

alternative for hydrogen production contributes to the reduction of CO2 emissions, because it

does not bring supplementary CO2 in the environment: the produced CO2 is only that initially

consumed by plants to grow.

Demand for hydrogen (H2) will grow up in the next decades due to the technological

advancements in fuel cell industry which permit its transformation in electricity and heat

without generating polluting gases. On Earth shell, virtually, it does not exist as hydrogen

molecule: it is associated with oxygen in water, with carbon in fossil hydrocarbons and both

with oxygen and carbon in bioresources (carbohydrates, cellulosic and lignocellulosic matter,

lignin, etc). At present, almost 95% of the world’s hydrogen is being produced from fossil fuel

based feedstock. The process is economically viable, but it has two major drawbacks:

(i) the diminution of fossil fuel reserves. According to some recent reports [1,2], if the annual

consumption of fossil fuels will be maintained at the same level, the oil reserves will be

finished in approximately 50 years and natural gases in 65 years;

(ii) steam reforming is not a green process on an environmental point of view, since all (or

almost all) of the carbon from hydrocarbons is transformed into carbon dioxide and released in

the environment.

In these conditions, one alternative is to replace fossil fuels by biofuels as raw materials

for hydrogen production. Biomass is renewable and, although carbon dioxide is still produced,

it may be recycled to new biomolecules by photosynthesis, resulting a carbon neutral cycle. If

the raw materials for hydrogen production are wastes or are produced by wastes, the overall

benefits of the hydrogen production method are even higher.

In this project we propose a laboratory scale technology to produce hydrogen from


glycerol wastes resulted in biodiesel fabrication. In the process of biodiesel fabrication by

transesterification of vegetable oils with methanol, glycerol is generated at a rate of 1 mol at

every 3 mol of methyl esters; approximately 10 wt.% of the total product. Over the last few

years the demand and production of biodiesel has increased tremendously and therefore large

amounts of glycerol (1.5 million tons per year predicted for 2012 in EU and USA) are

available at very low prices [3]. At present, glycerol is just in excess but in the near future it

could become a waste problem. It may create a barrier for the development of this industry

branch and reduce biodiesel applications as well. Although glycerol is a versatile product, the

main problem in the way of a possible usage of the waste glycerol solutions is their

composition: water, glycerol, methanol, free fatty acids, methyl esters, unreacted mono-, di-

and triglycerides, a variety of other organic molecules in low concentrations, plus inorganic

salts remained from the catalysts used in transesterification. As such, crude glycerol, with an

approximately 50 % concentration of glycerol, has no direct uses and its value is very low. The

purification of crude glycerol is very expensive and is not economically viable. The main

scientific and technologic barrier which will be approached in this project is the possible

usage of crude glycerol solutions for hydrogen production. One of the advantages of using

these wastes for hydrogen production is that only a partial purification of these wastes is

needed. Most of the oxygenated molecules contained in crude glycerol can be theoretically

implied in steam reforming reaction in parallel with glycerol, being transformed in hydrogen.

This is the reason for which in our approach of this project we will first study the catalytic

steam reforming of primary alcohols (methanol being the second product after glycerol in

crude glycerol solutions). We will focus our studies on steam reforming of ethanol and not

methanol due to two reasons: (i) the structure of these two alcohols being similar, the catalysts

and the reaction conditions for steam reforming should be similar; (ii) following the catalytic

and technological studies, a technology for hydrogen production from crude bioethanol

obtained from wood waste can be developed, increasing in this way the value of project

results.

The bioethanol will be produced by P2 ICIA by fermentation of wood wastes. Crude glycerol

solutions will be provided by P3 REVIVA, analyzed and partially purified in collaboration

with P2 ICIA.

The chemical process by which the hydroxylic compounds are transformed in hydrogen is

catalytic steam reforming (performed by CO INCDTIM). The main reaction which takes place

for glycerol steam reforming (GlySR) is:

OH-CH2-CH(OH)-CH2-OH + 3H2O → 3CO2 + 7H2 (1)


Practically, beside these reactions a series of other reactions take place simultaneously,

involving:

(i) partially C-C bond breaking resulting in alkanes, alkenes, C1-C2 alcohols;

(ii) partially oxidation of OH groups, resulting aldehydes, acids;

(iii) partially oxidation of the carbon resulted in a mixture of carbon oxides in the

effluent gases;

(iv) carbon deposition as inert graphite on the catalysts surface followed by catalysts

deactivation.

The result is a decrease of hydrogen production combined with an increase of separation and

purification effort. A good selection of catalysts and reaction conditions will diminish the side

reactions and will favor the main reaction (1) with results in overall hydrogen production.

For ethanol steam reforming (EtSR) the main reaction is:

C2H5OH + H2O → CO2 + H2O (2)

The catalytic experiments will be performed at a scale of 1g of catalyst and the following will

be determined: the catalytic activity, the selectivity for hydrogen production, the catalysts life

time, and the reaction conditions. After the reforming process, the resulting gaseous products

will enter in a separation unit based on a Pd membrane filter to finally obtain purified

hydrogen. A set of experimental data will be provided containing the conditions for which the

explored parameters have the optimum values. These data will be further used by P1 UBB to

model and design a catalytic technology at one order of magnitude higher level (tens of grams

of catalyst).

The scheme of the catalytic technology proposed by this project is presented in Figure 1.

Figure 1. Catalytic production of hydrogen from bioethanol and glycerol.

A laboratory scale experimental set-up will be designed and realized on which the catalytic

technology will be tested. The main parts of this experimental set-up are: the evaporator, the

catalytic reactor and the hydrogen separator. This set-up will be designed by P4 ROKURA and


H2Partial

purificationSteam

reformingH2

separationWaste glycerol / (crude bioethanol)

H2O

Liquid byproducts

Gaseousbyproducts

4

realized in collaboration with CO INCDTIM. Technological tests and technology

developments will be realized by CO INCDTIM in collaboration with P4 ROKURA.

The project objectives

The main objective of this project proposal is to develop a laboratory scale technology

and experimental set-up to produce hydrogen by steam reforming of hydroxylic compounds

(monohydroxylic alcohols and glycerol) resulted as wastes in biomass processing or

prepared from wastes of biomass.

Besides this main objective, the project has 7 specific objectives. The objective description,

followed by the novelty and original results expected from each objective, is presented below:

O1. Preparation and structural characterization of oxide supported nickel catalysts

additivated with noble metals and/or rare earth oxides.

- the catalysts which are intended to be prepared are mixed catalysts based on Ni/oxide.

Nickel was chosen for its well known efficiency in hydrocarbon steam reforming reactions.

We propose the addition of noble metals and/or rare earth oxides to improve the selectivity and

stability properties.

- the project proposes catalysts preparation using both classic methods (impregnation) and

new techniques (sol-gel). New catalysts will be prepared using combinations of noble metals

and rare earth oxides which have not been reported before.

- a complete and accurate catalysts characterization is crucial in heterogeneous catalysis in

order to obtain reproducible results. We propose in this project a set of physico-chemical

methods which will provide a complete structural, morphological and surface characterization

of prepared catalysts.

O2. Preparation, determination of the chemical composition and possibilities of partial

purification of crude alcohols and crude glycerol solutions.

- bioethanol is prepared by fermentation of waste wood; a new method will be proposed to

produce crude bioethanol suitable to be used with minimum purification effort for catalytic

steam reforming;

- waste glycerol solutions result in biodiesel production process; a purification method will

be proposed to transform these wastes in raw materials for catalytic steam reforming.

O3. Proposal and evaluation from conceptual design and from technical and environmental

impact perspectives the hydrogen production by steam reforming of hydroxylic compounds

(monohydroxylic alcohols and glycerol).

- the project proposes to develop a detailed and advanced mathematical model for the


hydrogen production process based on catalytic steam reforming of hydroxylic compounds,

simulation of the mathematical model, characterization of the system behavior based on

simulation results;

- the validation of the models will be made using experimental data followed by scale-up

analysis, sensitivity analysis and technology development;

- Based on experimental and simulation results, a techno-economical evaluation and

environmental impact assessment of hydrogen production based on catalytic steam reforming

processes of biomass processing wastes will be performed.

O4. Technological studies of ethanol and glycerol catalytic steam reforming on Ni based

catalysts, additivated with noble metals and/or rare earth oxides.

- Catalytic studies of ethanol and glycerol catalytic steam reforming will be performed in

order to establish the optimum catalyst – reaction conditions system;

- A special attention will be paid to catalysts stability studies (catalysts life-time,

deactivation mechanism, possibilities of regeneration), very modern techniques being used in

this purpose: Thermogravimetry (TGA), Thermo Programmed Oxidation (TPO), Transmission

Electron Microscopy (TEM).

O5. Design, fabrication and testing of a laboratory scale experimental set-up to produce

hydrogen from waste glycerol solutions.

- this objective implies: the design an fabrication of the evaporator and catalytic reactor,

measurement and control of temperatures and flows, on-line analysis of effluent gases.

O6. Dissemination activities: papers, presentations at international conferences, web page,

elaboration of one PhD thesis, patent application.

O7. Project management activities.

The original, novelty and innovative nature of the project

The original and innovative nature of this project proposal is based on its strong

interdisciplinary character which:

(i) combines in a coherent manner knowledge from various fields: chemistry, heterogeneous

catalysis, kinetic analysis, chemical reaction engineering, experimental optimization, thermo-

energy conversion processes, process design and integration, computational techniques

(modeling and simulation of complex systems);

(ii) connects the fundamental and applicative research from National Institutes (CO and P2)

and Universities (P1) with research developed by economical entities (P3) and by end-users of

developed technology (P4).

The project proposes new approaches of some very actual issues like: economically and


environmental friendly hydrogen production, wastes management, elaboration of advanced

technological models, techno-economical and environmental impact assessment of hydrogen

production from glycerol waste.

Expected results and the project end products

The main end product of this project proposal is the experimental set-up and catalytic

technology for hydrogen production from waste glycerol correlated with techno-economical

and environmental impact assessments. In the project implementation we expect to obtain the

following results:

- method for glycerol waste purification by alkaline metals;

- method for preparation of mixed catalysts based on alumina supported nickel;

- evaluation by modeling and simulation of bioethanol steam reforming processes for

hydrogen production;

- experimental model for catalysts testing in ethanol and glycerol steam reforming;

- evaluation by modeling and simulation of glycerol steam reforming processes for

hydrogen production;

- integrating of young PhD students in the research methodology with impact in the

development of their research capacity and potential;

- development of research infrastructure of partners;

- 6 ISI papers, 1 patent application, 10 presentations at international conferences;

- 1 PhD thesis.

1.2. State of the art:

The state of the art on the subject of the project

Importance of energy issue and efficient utilization of energy reserves in the actual

context of human society development are problems that cannot be ignored. The relevance of

energy topic must be considered from two important points of view: (i) the first is linked with

security of primary energy supplies in term of quantity and competitive prices and (ii) the

second one is linked with the necessity of environmental protection and climate change

mitigation by reduction of greenhouse gas emissions. The importance of energy theme and its

connections with environmental pollution lead to the inclusion of this issue within EU 2020

strategy (EU climate and energy package) and “Resource Efficient Europe” initiative for

competitive, sustainable and secure energy (Europe 2020 strategy, 2010). As ways to support

research and innovation in energy and environmental areas, various instruments have been put


in place. For instance, thematic areas regarding the energy chapter, covered by 7-th

Framework Programme include: hydrogen production and fuel cells, fuels and electricity

generation from renewable sources, renewable heating and cooling sources, promotion of

carbon capture and storage technologies, clean coal technologies, etc.

The development of technologies for the production of carbohydrates, valuable

chemicals, biofuels and heat and/or electricity from woody biomass received a special

attention in the last years [4]. Ethanol can be produced from various cellulosic materials. One

of the most promising technologies in terms of second generation biofuels is lingo-cellulosic

treatment underlying to obtain cellulosic bioethanol that is not directly linked to food

production. Wood waste is an abundant feedstock in Romania and can be used to produce

bioethanol through hydrolysis and fermentation. Bioethanol can be produced from cellulose

and hemicellulose [5]. Over the last years, a wide variety of methods for pretreatment,

hydrolysis and fermentation have been employed, but each of them presents advantages and

disadvantages [6]. In the present, there are pilot or demonstrative plants for bioethanol

preparation from cellulose in Sweden, Australia, SUA, Denmark, Spain, Germany and Canada.

Biodiesel, an alternative diesel fuel, is made from renewable biological sources such as

vegetable oils and animal fats. Considerable research has been done on vegetable oils as raw

materials for biofuels fabrication [7]. This research included palm oil, soybean oil, sunflower

oil, coconut oil, rapeseed oil and tung oil. Vegetable oils are transformed in biofuels by

transesterification with an alcohol, to form esters and glycerol. Common alcohols used in this

process are short chain alcohols, most notably methanol. A catalyst is usually used to improve

the reaction rate and yield. After transesterification of triglycerides, the products are a mixture

of esters, glycerol, alcohol, catalyst and tri-, di- and monoglycerides. Several chemical [8] and

enzymatic [9] processes to produce biofuel from vegetables oils are commercially available.

As already mentioned in the previous section, glycerol results as waste in this process; large

amounts (1.5 million tons per year predicted for 2012 in EU and USA) are available on the

market and its value is very low [3]. The overall profitability of biodiesel production is

dependent on the possibility to add value to this by-product.

In the last ten years, many researches have been devoted to the possibility of hydrogen

production from bioethanol [10] and glycerol [11]. Alcohols are raw materials well-adapted to

the production of hydrogen through catalytic reforming processes due to the fact that they are

reactive molecules whose decomposition over catalyst surfaces is much faster than

hydrocarbons.

From the noble metals used for ethanol steam reforming, Rh was recognized to be very


active and was one of the first studied catalysts [12,13]. Its activity depends on the support

nature and catalyst precursor. Other noble metals studied for ethanol steam reforming were: Pt

[14], Pd [15] and Ir [16]. Although noble metals are active and selective for hydrogen

production, they are very expensive, so many studies were focused on nickel catalysts

supported on various oxides: Al2O3, SiO2, MgO, MgAl2O4, La2O3, ZnO, CeO2, CeO2–ZrO2,

CexTi1-xO2 or perovskite-type oxides (LaAlO3, SrTiO3 and BaTiO3) [10]. The major problem to

overcome with nickel catalysts is to avoid the catalyst deactivation due to metal particle

sintering and to coke deposition. To improve the stability of the nickel catalyst, one way is to

modify the nature of the support. The best performances were obtained with the more basic

supports favoring the ethanol dehydrogenation and inhibiting ethanol dehydration leading to

ethylene, which is coke precursor [10]. Another way of improving the stability of Ni-based

catalysts consists of adding small amounts of noble metals such as platinum [17] or palladium

[18]. The addition of promoters caused a decrease in the NiO reduction temperature.

Moreover, the bimetallic catalysts showed a higher ethanol conversion and higher hydrogen

yield than the monometallic one, whatever the nature and concentration of the noble metal.

Until now, crude bioethanol has been very rarely used as ethanol source for EtSR reaction.

There are few literature reports: the SR of crude bioethanol obtained by fermentation of high

starch feed wheat [19], from sugar cane [20] and from wheat straw [21]. Whatever the origin

of the bioethanol, a deactivation of the catalyst was observed during the steam reforming

reaction that was attributed to the formation of carbon deposits.

Hydrogen can be produced from glycerol via steam reforming [22], partial oxidation

(gasification) [23], autothermal reforming [24] and aqueous-phase reforming (APR) [25]

processes. If the goal is to produce hydrogen and not synthesis gas, steam reforming is

preferred due to the advantage of cumulating in the reaction products hydrogen from both

reagents: glycerol and water.

A series of metals were tested in glycerol steam reforming process over ceria-supported

catalysts [26]. Ir/CeO2 catalyst was more active for complete glycerol conversion than

Co/CeO2 and Ni/CeO2. Ruthenium supported on Y2O3 showed good results in glycerol

complete conversion at 600°C and H2 selectivity of 90% [27]. Commercial Ni-based reforming

catalysts were also used for H2 production from glycerol [28]. Studies on several Ni catalysts

supported on different oxides show that Ni/CeO2 was the best performing catalyst compared to

Ni/MgO and Ni/TiO2 under the experimental conditions investigated [29]. Navarro and co-

workers [30] have performed steam reforming of glycerol over Ni catalysts supported on

alumina with various promoters such as Ce, Mg, Zr and La. Their study concluded that the use


of Mg, Zr, Ce and La increases the hydrogen selectivity. Higher activities of those catalysts

were attributed to higher Ni concentration, higher stability and higher capacity to activate

steam. Several noble metal based catalysts have been studied and it was found that

Rh/CeO2/Al2O3 was the best performing catalyst in terms of H2 selectivity and glycerol

conversion under the experimental conditions investigated [31].

The number of studies which reported hydrogen production from crude glycerol is much lower

[32,33].

Compare the product and technology that you aim to develop with existing products and

technologies available worldwide. Analyze how the product and technology that you aim to

develop distinguishes from existing product/technology/services which are already patented

and/or exploited commercially, in Romania or other countries

The laboratory scale technology proposed by this project addresses a very actual topic

which is not exploited yet on large scale. Although the declared objective of most published

studies of glycerol steam reforming was to produce hydrogen from crude glycerol, very few

were focused on this. In these studies the catalysts are noble metals and the main problem is

the presence of impurities in crude glycerol which (i) impeded the performance of the catalyst

and (ii) cause a severe catalyst deactivation. Our technology proposes two approaches to

overcome these problems: (1) to establish an economically viable method to partially purify

the crude glycerol and (2) to test and find new catalysts based on Ni with better activity and

resistance to deactivation.

In Romania there is no commercially exploited technology to produce hydrogen from

crude glycerol. Although there are a number of international patents [34, 35] for hydrogen

production from glycerol, we found no information about a commercially available technology

to produce hydrogen from crude glycerol.

Show any contribution by the partners to the state of the art. Show any preliminary results

The team proposed for this project by P1 UBB has internationally recognized results in

mathematical modeling and simulation of chemical and thermo-chemical processes [36],

modeling of hydrogen production [37], renewable energy sources and energy conversion

processes [38].

Partner P2 ICIA has a significant number of results, nationally and internationally

acknowledged, regarding biofuels such as: biodiesel, bioethanol and biogas, results

materialized in the development of technologies and equipment production. Partner P2 has


elaborated and achieved at laboratory scale three technologies for bioethanol production from

wood waste, based on three hydrolysis types: (Patent: “Technology for obtaining bioethanol

from lignocellulosic biomass (wood waste)”). Wood waste pretreatment reported in literature

has almost exclusively focused on chemical pretreatments. ICIA has an important

contribution in the development of an eco-friendly pretreatment method that uses only water

as solvent to separate the wood waste. Partner P2 ICIA developed in collaboration with P3

REVIVA an original technology for biodiesel production from crude and used vegetable oils

(Patent “Biofuel production technology from crude vegetable oil resulted as secondary

products in manufacturing of texture soy protein - BIOVALP”).

CO INCDTIM has experience and internationally recognized results in hydrogen involving

heterogeneous catalytic processes: hydrogen production from methane, hydrogen storage, H/D

isotopic exchange. The team involved in this project developed an original method to study the

hydrogen spillover phenomena on the metal/oxide catalysts surface [39] contributing to a

better characterization of these types of catalysts. In the last three years the interest was

focused in hydrogen production by methane steam reforming using additivated Ni catalysts

similar with those proposed in this project. The results show that the addition of Au to Ni and

cerium oxide to alumina improves the methane conversion and catalyst stability. The results

were published in internationally recognized journals [40, 41] and presented to international

conferences.

The results published or patented by all members of the consortium in the area proposed in this

project show that they contributed with significant results to the development of these

domains.

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Table 1: Phase listPha

se

no.

Phase titleInvolved

partners

Start

month

End

month

1 General assessment of the catalytic

production of hydrogen from renewable

oxygenates: catalysts preparation and

characterization; evaluation of ethanol and

glycerol steam reforming processes for

hydrogen production in terms of

thermodynamic aspects, conceptual layout;

optimization of bioethanol preparation

method from wood waste; possibilities of

energetic valorization of glycerol.

CO, P1,

P2, P3

1 8

2 Hydrogen production by catalytic steam

reforming of bioethanol obtained from

wood waste: raw bioethanol physico-

chemical characterization, catalysts activity

and selectivity for raw ethanol SR;

modeling and simulation of the process,

model validation.

CO, P1,

P2

9 18

3 Technological parameters for hydrogen

production by catalytic steam reforming of

waste glycerol solutions resulted in biofuels

production: characterization and partial

purification of waste glycerol solutions,

catalytic and reaction parameters for H2

production by waste glycerol SR; modeling

and simulation of the process, model

validation; design and realization of

laboratory scale experimental set-up.

CO, P1,

P2, P3, P4

19 32

4 Laboratory scale catalytic technology and

experimental set-up for hydrogen

CO, P1,

P2, P3, P4

33 36


production by steam reforming of

hydroxylic compounds obtained as biomass

processing wastes; techno-economic and

environmental impact evaluations,

dissemination activities (patent application,

articles etc.)

5 Consortium management activities CO 1 36

Table 2: Phase description (for each Phase-max 2 pages)

Phase no. 1

Phase title General assessment of the catalytic production of hydrogen from

renewable oxygenates: catalysts preparation and characterization;

evaluation of ethanol and glycerol steam reforming processes for

hydrogen production in terms of thermodynamic aspects, conceptual

layout; optimization of bioethanol preparation method from wood

waste; possibilities of energetic valorization of glycerol.

Involved

partners

CO

INCDTIM

P1

UBB

P2

ICIA

P3

Reviva

Total

Person-

months

30 12 16 2 60

Start month 1

End month 8

Objectives

O1.1 The preparation and characterization of new catalysts of type Me-Ni/oxide1-oxide2.

O1.2 Evaluation of ethanol and glycerol steam reforming processes and conceptual

layout;

O1.3 Optimization of bioethanol obtaining method from wood waste;

O1.4 Study of the possible energetic valorization of biomass wastes.

Description of work (possibily broken down into tasks) and role of participants

Task I – related to O1.1 and performed by CO

A1.1 The preparation of mixed catalysts based on alumina and zirconia supported Ni (6-

10 wt.%) and additivated either with noble metals (Au, Ag, Pt, Rh) or with rare earth

oxide (La2O3, CeO2, Y2O3). The concentration of additional metal is less or maximum 1


wt.% and of additional oxide is less or maximum 6%. The catalysts will be prepared by

classic impregnation and/or by sol-gel methods.

A1.2 Structural characterization of the prepared gold catalysts using the following

modern techniques: X-Ray Diffraction (XRD) – determination of metal crystallites sites,

determination of oxide crystallinity, H2 chemisorption – estimation of catalytic active

surface area; N2 adsorption desorption isotherms – determination of total surface area and

porosity; Transmission Electron Microscopy (TEM-EDX) – determination of metal

nanoparticles size and distribution; Thermo Programmed Reduction (TPR) –

determination of metal reducibility on the surface, estimation of type and nature of

catalytic active sites, H/D isotopic exchange – determination of number of surface OH

groups.

Task II – related to O1.2 and performed by P1 (UBB)

A 1.3 Evaluation by thermodinamic modeling and simulation the ethanol and glycerol

steam reforming processes in term of process conditions e.g. temperature, pressure and

catalysts influence on conversion rates, resulted products etc.

A 1.4 Conceptual layout of ethanol and glycerol steam reforming processes for hydrogen

production (this activity implies the collaboration of P1 with CO, P2 and P3).

Task III – related to O1.3 and performed by P2 (ICIA)

A 1.5 Developing the method of bioethanol production from wood waste and improving

process parameters. Experimenting with various types of hydrolysis (acid and enzymatic)

for fermentable sugars. Analysis of intermediary compounds will be done.

A 1.6 Experimenting in order to improve the existing method for bioethanol production:

increasing of fermentable yield, eliminating of the inhibitors, temperature of

fermentation, time of fermentation, pH, concentration of inoculum and nutrients.

Task IV - related to O1.4 and performed by P3 (Reviva)

A 1.7 Energetic evaluation of biomass wastes.

A 1.8 Study of possible usage of glycerol wastes in energetic purpose.

Deliverables (brief description and month of delivery)

D1.1 Preparation method for mixed catalysts – 3rd month

D1.2 Alumina supported Ni based mixed catalysts samples complete characterized from

morphological and structural point of view – 8th month

D1.3 Report for evaluation of ethanol and glycerol steam reforming processes for

hydrogen production and conceptual layout – 8th month

D1.4 Optimized method for bioethanol production from wood waste – 8th month


D1.5 Report of energetic valorization of biomass wastes – 8th month

Phase no. 2

Phase title Hydrogen production by catalytic steam reforming of bioethanol obtained

from wood waste: raw bioethanol physico-chemical characterization,

catalysts activity and selectivity for raw ethanol steam reforming;

modeling and simulation of the process, model validation.

Involved

partners

CO

INCDTIM

P1

UBB

P2

ICIA

Total

Person-

months

30 15 30 75

Start month 9

End month 18

Objectives

O2.1 Bioethanol preparation and physico-chemical characterization.

O2.2 Establishing the technological parameters, catalytic system and reaction conditions

for hydrogen production by bioethanol steam reforming.

O2.3 Modeling and simulation of bioethanol steam reforming process, model validation,

process integration aspects, energy consumptions.


Task I – related to O2.1 and performed by P2 (ICIA)

A 2.1 Obtaining of fermentation medium and bioethanol as raw material for biohydrogen

production.

A 2.2 Physico-chemical characterization of fermentation medium and bioethanol.

The composition of fermentation medium (content of secondary alcohols, acids, furfural,

HMF) and composition of obtained ethanol (ethanol – water ratio, alchohol concentration,

esters content) will be estabilished.

Task II – related to O2.2 and performed by CO

A 2.3 The Ni based catalysts prepared and characterized in the previous phase are tested

in ethanol steam reforming at atmospheric pressure and temperatures ranging from 200 to

400°C. The ethanol – water ratio will be correlated with the information received from P2

to better mimic the bioethanol composition obtained from wood waste.

A 2.4 The following parameters will be established for each catalyst and reaction

conditions: ethanol conversion, H2 selectivity, H2 production, catalyst deactivation


(decrease of ethanol conversion with time on stream).

A 2.5 In parallel with A2.4, the catalysts with promising results in H2 production by

synthetic ethanol-water mixture reformation will be tested for hydrogen production by

catalytic steam reforming of crude bioethanol obtained from wood waste. Altenativelly

the ethanol solution can be diluted to reach the point with optimum maximum conversion

– minimum coke deposition. The catalalytic process with the optimum balance between

ethanol conversion, hydrogen production and catalyst stability will be used for further

technological assays. Experimental data will be provided to P1 for model validation.

Task III – related to O2.3 and performed by P1 (UBB)

A 2.6 Mathematical modeling and simulation of bioethanol steam reforming process

using dedicated process flow modeling software packages (e.g. ChemCAD, Aspen Plus

etc.).

A 2.7 Model validation using experimental data, interpretation of simulation results.

Evaluation of process integration issues (mass and energy), utilities and energy

consumptions.


D2.1 Bioethanol obtained and characterized – starting with 11th month

D2.2 Report of evaluation by modeling and simulation of bioethanol steam reforming

processes for hydrogen production – 18th month

D2.3 Technological parameters for laboratory scale H2 production by steam reforming of

crude bioethanol obtained from wood waste – 18th month

D2.4 2 papers in international recognized journals (ISI ranked) – 18th month

D2.5 3 presentations at an international scientific meeting – up to the 18th month

Phase no. 3

Phase title Technological parameters for hydrogen production by catalytic steam

reforming of waste glycerol solutions resulted in biofuels production:

characterization and partial purification of waste glycerol solutions,

catalytic and reaction parameters for H2 production by waste glycerol

SR; modeling and simulation of the process, model validation; design

and realization of laboratory scale experimental set-up.

Involved

partners

CO

INCDTIM

P1

UBB

P2

ICIA

P3

Reviva

P4

Rokura

Total


Person-

months

40 20 24 10 34 128

Start month 19

End month 32

Objectives

O3.1 Physico-chemical characterization and possibility of partial purification of waste

glycerol solutions from bio-diesel production using original BIOVALP technology.

O3.2 Establishing the optimum technological parameters (raw material composition,

catalysts performances and stability, reaction conditions) for laboratory scale H2

production by waste glycerol solutions steam reforming.

O3.3 Modeling and simulation of glycerol steam reforming process, model validation,

process integration aspects, utilities and energy consumptions.

O3.4 Design and realization of laboratory scale experimental set-up.


Task 1 – related to O3.1 and performed in collaboration by P2 and P3

A 3.1 Development of original BIOVALP technology in order to obtain wastes (washing

waters) with higher concentration of glycerol.

A 3.2 Determination of chemical composition of residual washing waters resulted in

biodiesel fabrication.

A 3.3 Identification and quantitative determination of compounds with possible poisoning

effect on steam reforming catalysts (activity performed in collaboration with CO).

A 3.4 The extraction of catalysts dangerous compounds from waste glycerol solutions. A

purification method will be provided.

Task 2 – related to O3.2 and performed by CO

A 3.5 Establishing the experimental conditions and the reaction products analyzing

conditions for glycerol steam reforming at atmospheric pressure and temperatures ranging

from 500 to 700°C using 1g of noble metal and/or rare earth oxide promoted Ni catalysts.

The catalytic set-up will be configured to permit the catalytic reaction and on-line

analysis of both, gaseous and liquid fractions of the reaction products; an analytical

method will be provided.

A 3.6 Establishing the catalytic parameters. The following parameters will be determined

for each catalyst: glycerol conversion, composition of reaction products mixture, H2

selectivity, H2 production, catalyst deactivation and characterization of deposited coke (in

order to better describe the catalyst deactivation process). The following methods will be


used for characterization of deposited carbon: Thermogravimetry (TGA), Thermo

Programmed Oxidation (TPO), Electron Microscopy (TEM). A correlation between the

type and amount of deposited coke, catalyst nature and reaction conditions will lead to

improvement of catalyst lifetime with direct consequences in economic efficiency of the

hydrogen production.

A 3.7 The catalytic system with best performances found in A 3.4 is tested in catalytic

steam reforming of crude glycerol partial purified provided by P4. The best conditions for

hydrogen production will be established. A special attention will be paid to the

determination of catalysts deactivation mechanisms in order to improve the catalyst

lifetime. If the hydrogen production is much lower comparing with results obtained in A

3.6 further purification or changing of catalytic system will be performed.

A 3.8 Design, production and experimentation of hydrogen separator based on Pd

membrane.

Task 3 – related to O3.3 and performed by P1 (UBB)

A 3.9 Mathematical modeling and simulation of glycerol steam reforming process using

dedicated process flow modelling software packages (e.g. ChemCAD, Aspen Plus etc.),

A 3.10 Model validation using experimental data, interpretation of simulation results.

Evaluation of process integration issues (mass and energy), utilities and energy

consumption.

Task 4 – related to O3.4 and performed by P4 (Rokura) and CO (INCDTIM)

A 3.11 Design the experimental set-up for using of 10 g of catalysts in glycerol steam

reforming at atmospheric pressure and temperatures ranging from 500 to 700°C catalyzed

by noble metal and/or rare earth oxide promoted Ni catalysts.

A 3.12 Building the experimental set-up composed by: evaporator, catalytic reactor and

hydrogen separator.

A 3.13 Experiment the laboratory scale catalytic technology for hydrogen production by

steam reforming of waste glycerol.


D3.1 Partialy purified waste glycerol solutions – starting with 24th month

D3.2 Report of evaluation by modeling and simulation of glycerol steam reforming

processes for hydrogen production – 32nd month

D3.3 Technological parameters for laboratory scale H2 production by steam reforming of

waste glycerol solutions from biodiesel fabrication – 32nd month

D3.4 Experimental set-up for hydrogen production from waste glycerol solutions


D3.5 2 papers in international recognized journals (ISI ranked) – 32nd month

D3.6 2 presentations at an international scientific meeting – up to the 32nd month

Phase no. 4

Phase title Laboratory scale catalytic technology and experimental set-up for

hydrogen production by steam reforming of hydroxylic compounds

obtained as biomass processing wastes; techno-economic and

environmental impact evaluations, dissemination activities (patent

application, articles etc.)

Involved

partners

CO

INCDTIM

P1

UBB

P2

ICIA

P3

Reviva

P4

Rokura

Total

Person-

months

12 6 12 3 12 45

Start month 33

End month 36

Objectives

O 4.1 Presentation of laboratory scale technology for hydrogen production from

hydroxylic compounds obtained as biomass processing wastes by steam reforming.

O 4.2 Dissemination activities, intellectual property rights, future development


The activities of this phase are related to one major task: presentation of the proposed

laboratory scale technology with techno-economical, environmental and scale-up

analyses. These activities imply the colaboration of all parteners.

A 4.1 Development of laboratory scale technology for hydrogen production from waste

glycerol solutions resulted in biodiesel fabrication.

A 4.2 Techno-economical and environmental assessment of hydrogen production from

hydroxylic compounds obtained as biomass processing wastes by steam reforming.

A 4.3 Scale-up analysis of the proposed technology.

A 4.4 Potential implementation of developed technology.

A 4.5 Intelectual property aspects (patent application), dissemination of project results

(articles, conference comunications).


D4.1 Laboratory scale technology for hydrogen production from waste glycerol solutions

resulted in biodiesel fabrication – 36th month

D4.2 Techno-economic and environmental impact evaluations of hydrogen production by


hydroxylic compounds steam reforming – 36th month

D4.3 2 pantent applications – 36th month

D4.4 1 ISI article – 36th month

Phase no. 5

Phase title Consortium management activities

Involved

partners

CO

INCDTIM

Total

Person-

months

33 33

Start month 1

End month 36

Objectives

O5.1 Coordination of Consortium activities


A 5.1 Ensure good communication between partners, organize the partners meetings and

workshops.

A 5.2 Manage the overall project plan and assure the good timing of partners activities.

A 5.3 Manage the exploitation of the generated results and information; assure the

attribution of the intellectual property rights in accordance with the Colaboration

agreement.

A 5.4 Prepare and edit the scientific and economic reports for each project phase.


D5.1 Detailed work plan

D5.2 Scientific and economic reports for each phase – 4 reports

D5.3 Final report

Table 3: Deliverables List


Delivera

ble No.Deliverable Name

Phase

no.

Type of

Deliverable*

Phase delivery

date

(1 ... n)

D1.1Preparation method for mixed

catalysts 1 Method 8th month

D1.2

Alumina supported Ni based

mixed catalysts samples

complete characterized from

morphological and structural

point of view

1Product

samples8th month

D1.3

Report for evaluation of

ethanol and glycerol steam

reforming processes for

hydrogen production and

conceptual layout

1 Report 8th month

D1.4

Optimized method for

bioethanol production from

wood waste

1 Method 8th month

D1.5Report of energetic

valorization of biomass wastes 1 Report 8th month

D2.1Bioethanol obtained and

characterized 2

Product

samples18th month

D2.2

Report of evaluation by

modeling and simulation of

bioethanol steam reforming

processes for hydrogen

production

2 Report 18th month

D2.3

Technological parameters for

laboratory scale H2 production

by steam reforming of crude

bioethanol obtained from wood

waste

2Technical

report18th month

D2.4 2 papers in international

recognized journals (ISI

2 Article 18th month


ranked)

D2.53 presentations at an

international scientific meeting 2

Conference

presentation18th month

D3.1

Partialy purified waste glycerol

solutions – starting with 24th

month

3Product

Samples32nd month

D3.2

Report of evaluation by

modeling and simulation of

glycerol steam reforming

processes for hydrogen

production

3 Report 32nd month

D3.3

Technological parameters for

laboratory scale H2 production

by steam reforming of waste

glycerol solutions from

biodiesel fabrication

3Technical

report32nd month

D3.4

Experimental set-up for

hydrogen production from

waste glycerol solutions

3Laboratory

instalation32nd month

D3.5

2 papers in international

recognized journals (ISI

ranked)

3 Article 32nd month

D3.62 presentations at an

international scientific meeting 3

Conference

presentation32nd month

D4.1

Laboratory scale technology

for hydrogen production from

waste glycerol solutions

resulted in biodiesel

fabrication – 36th month

4 Technology 36th month

D4.2 Techno-economic and

environmental impact

evaluations of hydrogen

production by hydroxylic

4 Report 36th month


compounds steam reforming

D4.3 2 pantent applications 4 Patent 36th month

D4.4 1 ISI article – 36th month 4 Article 36th month

D5.1 Detailed work plan 1 Work plan 2nd month

D5.2

Scientific and economic

reports for each phase – 4

reports

1,2,3,4 Phase report

Phase1–8th month

Phase2–18th

month

Phase3–32nd

month

Phase4–36th

month

D5.3 Final report 4 Report 36th month

* according to Annex 6 – results indicators of the Programme (patent, technology, article etc)


2. Implementation

(max 10 pages)2.1. Management structure and procedures

Project management involves the coordination of research among the 5 partners, the

delivery of all outputs through the activities of the phases, as well as the organization of

meetings and project communication. The project management structure will ensure that

deadlines are met and that financial information including cost-statements is submitted and

audit certificates obtained. The management structure is illustrated in the figure below as a

hierarchical structure, but this is for project accountability purposes; the equality and integrity

of all academic and economic partners in the project is respected.

Accountability line Communication line

Figure 1. Project accountability and communication hierarchy.

The management structure of the project will consist of:

a. Steering Group – formed by the coordinators of each partner institution in the consortium.

This group will meet several times during the time span of the project in order to oversee and

take all key decisions on the progress of the research, including methodological issues, ethical

issues, outcomes and dissemination. These meetings will be scheduled as follows: a meeting at

the beginning of the project (month 2), a meeting corresponding to each phase (month 9, 19,

33), and a meeting at the end of the project. Two steering group meetings will coincide with 2

broader meetings of all the researchers involved. The steering group will monitor progress

against agreed milestones and oversee deliverables. It will resolve any problems arising from

the project, and will meet in emergency sessions, either through telephone/video conferences or

additional meetings where necessary.

b. Coordinator. INCDTIM as the coordinator of the project will take responsibility for the

overall project coordination and for liaising with the National Authority of Scientific Research.

The coordinator has extensive experience of project management, including international


CO - INCDTIM

P1 - UBB P2 - ICIA

P3 – S.C. REVIVA S.R.L

P4 – S.C. ROKURA S.R.L

26

projects. It will be responsible for organizing 5 steering group meetings, maintaining

communication with partners, ensuring there is a shared understanding of the work,

coordinating the activities during the established phases and ensuring deadlines are met and

deliverables are produced. It will ensure that the project is undertaken in accordance with the

highest standards of research ethics and scientific quality.

Timetables are crucial to the successful achievement and dissemination of research. The role of

the coordinator is thus important, in particular to the maintenance of regular contact, both

electronically and by regular meetings. INCDTIM will ensure that regular communication takes

place between all partners. The coordinator has responsibility for monitoring work outputs and

will establish internal deadlines for draft and final versions of reports.

c. Decision-making process. The key decision-making body is the project steering group,

which will oversee the implementation of research objectives and milestones. In certain

circumstances additional decisions may have to be taken at short notice by the project

coordinator and reported to the partners.

d. Meetings. In addition to the steering group meetings all researchers will meet in 2 one day

workshops, in month 2 and 19. This will allow all researchers to have an input into the project

and to engage in key discussions on methods and project development. The first research

workshop will set out the detailed research methodology, establish common ground rules and

ethical guidelines; confirm milestones and detailed timetables. The 2nd workshop will focus on

critical analysis towards the development of the catalytic steam reforming process of bioethanol

and the development of the waste glycerol steam reforming process for H2 production will be

discussed. Moreover, this meeting will ensure continued consensus about research objectives

and project outcomes and consistency in presentation of results. The 6 project meetings (4

steering group meetings and 2 workshops) will all take place in Cluj-Napoca, the home city of

4 from among the 5 partners of the consortium, at INCDTIM, the coordinating institution.

e. Communication during the project will be both internal, as well as external. Internal

Communication involves communication (electronic or phone) among partners between 2

consecutive meetings in order to allow information to be shared on a regular basis, as well as to

ensure consultation on key issues. The communication language will be Romanian. External

Communication includes communication with the National Authority for Scientific Research

through reports as scheduled, as well as with the interested public through the project website.

The Project website will be the public face of the project, where information of interest

regarding the project will be submitted on a regular basis.


f. Consortium Agreement. Before the start of the project a Consortium Agreement will be

signed by its members. This Agreement will cover the following issues: management of

knowledge, research and innovation activities, a code of conduct addressing copyright and

intellectually property right issues, ethical issues, and scientific quality standards.

2.2. Individual participants

CO – INCDTIM is a national research institute dedicated to research and development in

natural sciences and engineering. The research activity unrolled in the Institute is developed on

the following directions: (i) fundamental research in physics of stable isotopes, molecular

physics, biophysics, solid state physics; (ii) applied research: separation of stable isotopes;

applications of isotopic labeled compounds; preparation and characterization of nanostructured

systems; catalysis; investigation at molecular level of the processes occurring in ecosystems;

modern spectroscopic techniques for the investigation of composition and structure.

INCDTIM will participate in this project with its expertise in H2 production by catalytic steam

reforming processes. The team involved has experience and expertise in catalytic methane

steam reforming (see the project leader CV) which imply: catalysts preparation, catalysts

characterization, performing of catalytic reactions, catalysts deactivation studies, etc. Some

preliminary results were also obtained in ethanol catalytic steam reforming. The heterogeneous

catalysis team coordinated 3 national and 2 international projects in the last years in the area of

H2 production from CH4, H2 storage and environmental catalysis.

P1 – Babes-Bolyai University (UBB) is an academic educational public institution aiming to

promote and sustain the development of specific cultural components within the national and

international community. UBB is ranked within the first 2 universities of Romania taking into

account the research activity. In the proposed project UBB will be involved with the Faculty of

Chemistry and Chemical Engineering, Department of Chemical Engineering and Oxide

Materials Science, Thus, the team of P1-UBB will be involved with its expertise in advanced

modeling and simulation in energy conversion processes (e.g. catalytic steam reforming,

gasification, combustion), H2 production and purification processes, chemical engineering

expertise, model validation with experimental data collected from the project partners, complex

process integration schemes for improvement of energy efficiency, techno-economic and

environmental impact evaluations etc.

P2 – INCDO-INOE 2000, ICIA, is a national research institute dedicated to applied analytical

chemistry in three main directions: bioenergy – biofuels, analytical instrumentation, and


analytical chemistry of the environment. It has two laboratories with RENAR accreditation:

laboratory for biofuel quality certification (CABIO) and environmental analysis laboratory

(LAM). Based on the previous experience of ICIA, its main task in the present project is to

develop and optimize the technology for bioethanol obtaining, using an acid hydrolysis of

wood waste, enzymatic hydrolysis and a combination of simultaneous saccharification and

fermentation of cellulosic waste. The research activities will focus on ecological pre-treatment

of feedstocks, and hydrolysis and fermentation of woody biomass to the conversion of biomass

into fuel ethanol and the bioethanol characterization according to SR EN 15376.

P3 – S.C. REVIVA Import Export S.R.L. Apahida, Cluj, is a SME working since 2002 with

significant results in the area of food industry. The main products are soy based foods produced

using an original REVIVA technology. Another direction of REVIVA activity is the production

of soy oil and its use to produce biodiesel. REVIVA was involved in a Parteneriate 2008

research project - “Biofuels production by valorization of secondary products resulted in

vegetable proteins fabrication”, resulting in an original technology named BIOVALP. The

present project proposal is a continuation of the researches in this direction through valorization

of glycerol wastes resulted in BIOVALP technology. REVIVA will participate with activities

for: optimization of biodiesel production to result washing waters with higher glycerol

concentrations, the analysis and partial purification of glycerol wastes.

P4 – SC ROKURA SRL is a SME involved since 1992 in communication projects, data

acquisition and distance transmission, H2 rich gas production, energetic valorization of

biomass. ROKURA has 2 major development directions: (i) monitoring and automation of

industrial processes, and (ii) H2 rich gas production through aqueous-alkaline solutions, and

cogeneration, based on biogas sources, biomass gasification, biomass direct combustion, and

natural gas. In this project ROKURA will participate with activities related to design and

realization of experimental set-up, experimentation and optimization of H2 production

technology from biomass wastes.

The project leader is Senior Researcher Dr. Mihaela Diana Lazar, who received the

PhD degree in chemistry at Babes-Bolyai University, Cluj-Napoca with the thesis “Studies of

supported metal catalysts by H/D isotopic exchange”. Dr. Mihaela Diana Lazar has 12 years of

experience in heterogeneous catalysis involving: (1) preparation of supported metal catalysts

using various methods: impregnation, coprecipitation, deposition-precipitation, sol-gel

technique; (2) catalysts characterization by determination of total surface area and metal

surface area (BET method, chemisorption), particles size (TEM, XRD), metal oxidation state


(XPS); (3) surface reactions by temperature-programmed techniques: desorption (TPD),

reduction (TPR), oxidation (TPO); (4) determination of catalytic parameters (activity,

selectivity, deactivation rate, carbon deposition, re-activation) in heterogeneous catalytic

processes (hydrogenations, H/D isotopic exchange, steam reforming, water-gas shift, NOx

reduction, etc). The most important results were obtained in the areas of: H2 production and

storage; the study of hydrogen adsorption, activation and spillover on oxide supported gold

catalysts using H/D isotopic exchange; the study of isocyanide adsorption on gold surface;

catalytic properties of non-nanostructured gold; nanocarbon structures prepared by catalytic

techniques. Dr. Mihaela Diana Lazar coordinated 3 research projects: (1) PN II “Parteneriate”

Program: “Research and Development of a membrane reactor for ultra pure H2 production for

fuel cells applications” (2007-2010); (2) Romania–Dubna, Russia Agreement; Theme:

“Investigations of Nanosystems and Novel Materials by Neutron Scattering Methods” (2009-

2011); and (3) NUCLEU Program: “Multifunctional nanostructured molecular systems” –

coordinator of the heterogeneous catalysis topic (2003-2005). Moreover, she participated as

team member in: 3 “CEEX” projects, 2 “PN II Parteneriate” projects, 3 “PN II Idei” projects; 2

international projects (one in INCDTIM Cluj-Napoca, and one at the Iowa State University).

The team from INCDTIM also includes: one senior researcher CSI Dr. Eng. Valer Almăşan, 3

PhD students and two technicians.

Assoc. Prof. Eng. Dr. Calin – Cristian Cormos will coordinate research team from P1-UBB.

He has got his PhD degree in 2004 in chemical engineering.. He has more than 15 years of

experience with scientific research, having also experience as a chemical engineer, plant

manager and product development manager in chemical and pharmaceutical sector. He is

responsible for 4 academic disciplines in chemical engineering, and published 62 scientific

articles in international journals and peer-review conferences devoted to energy conversion. He

coordinated or was involved in several national or international research projects in the field of

energy with carbon capture and storage. Also, he is working as scientific referent for

prestigious international journals and is involved as project evaluator for national and

international (e.g. FP7) project competitions. The team proposed by UBB also includes: one

Lecturer, Dr. Ana-Maria Cormos, one associated professor and one professor.

Senior researcher Dr. Cecilia Roman will lead the research team from P2-ICIA. She has got

her PhD degree in 1997 from UBB Cluj-Napoca, and is currently the head of Research

Department of ICIA. Her rich scientific experience includes technologies for bioethanol

obtaining from lignocellulosic biomass. She coordinated 10 national projects, and was


responsible for other 10, from which 3 are international ones. She is author of 2 patents, 3

books, 52 ISI articles, and participated at more than 90 national and international conferences.

The team proposed by ICIA also includes: 1 scientific researcher and 1 PhD Student.

Eng. Koncz Carol will coordinate the research team from P3-REVIVA. He is currently the

head of Technical Department at SC REVIVA SRL. His experience includes: fabrication of

protein texture from soybean, fabrication of soy oil, fabrication of biofuels from soy oil. He

coordinated one research project in PN II Parteneriate Program.

The team of SC REVIVA SRL also includes: 1 engineer and 1 economist.

Dr. Eng. Petcu Cristian Mihai will lead the research team from P4 ROKURA. He has got his

PhD degree in 1998 in engineering in the field of thermal engines. His current position is R&D

and Scientific manager at SC ROKURA SRL. His work experience includes: renewable energy

projects, co-generation system projects, hydrogen combustion in engines, producing of

hydrogen rich gas for fuels treatment. He coordinated 4 research projects in PN II Parteneriate

program. The team of SC ROKURA SRL also includes: 3 engineers and 1 PhD student.

2.3. Consortium as a whole

The consortium involved in the implementation of this project proposal is well balanced

between 2 National Institutes of Research and Development: INCDTIM as coordinator (CO)

and INCDO-INOE 2000, ICIA as P2, 1 Romanian top university, Babes-Bolyai University,

Cluj-Napoca as P1, and 2 economic companies: SC REVIVA SRL, Cluj-Napoca as P3,

specialized in biodiesel fabrication, and SC ROKURA SRL, Bucuresti as P4, implied in

alternative energy market. The proposed research approach requires a multidisciplinary team,

thus the involved partners of the Consortium comprise experts in the fields of heterogeneous

catalysis, chemical engineering, biomass processing, process optimization and integration,

control and automation of industrial processes, etc.

The project will be highly interactive, all partners being involved with very specific tasks which

are interconnected and in most cases interdependent. All partners have demonstrated the ability

to co-operate productively with other consortium members and most have collaborated

previously, either with each other or with the coordinator.

The available infrastructure at each partner institution ensures the successful achievement of

most specific tasks scheduled in the workplan (see “Available research infrastructure” section).

Thus, equipment available at CO ensures catalyst preparation, characterization and testing; IT

infrastructure available at P1 will be used for process modelling and simulation; analysis


infrastructure at P2 will be used for bioethanol and waste glycerol characterization, while the

fermentation equipment will be used for bioethanol production; P3 has all the equipment for the

preparation of biodiesel (crude glycerol is a biodiesel waste); IT infrastructure available at P4

will be used for the design of experimental set-up, scale-up, etc. However, several equipments

will also be purchased in order to improve the research infrastructure.

The project objectives presented in Section 1.1 imply the activity and commitment of all

partners. Based on the previous results obtained by the consortium members in collaborative

research projects we have all the reasons to affirm that the partners will create a strong research

network which incorporates all the necessary expertise in biomass transformation in hydroxylic

compounds, catalytic studies for H2 production, chemical engineering, mathematical modeling

of chemical processes, design and elaboration of laboratory technology, project and financial

management required to meet the project objectives.

2.4. Resources to be committed.

Successful development of the project requires the commitment of the following resources:

Human resources involved in the project comprise specialists of various qualifications in

accordance with the multidisciplinary character of the topic proposed. Each partner institution

of the consortium will involve a research team consisting in both senior researchers and young

ones. The involved personnel are in accordance with the implication of each partner in the

development of the project.

Involved partner CO P1 P2 P3 P4 Total

Person-months 145 53 82 15 46 341

Infrastructure resources include all the available equipment at each partner institution as

presented in the “Available research infrastructure” section. However, an integrated system for

catalyst characterization and a gas chromatograph for the online analysis of reaction products

will be purchased.

Financial resources necessary for the implementation of the project include both finances

from the Public Budget (92.5%) and Private cofinancing (7.5%). The total budget is of

3.243.400 lei, which will be divided by destination as presented in the table below.

Personnel

costs

LogisticsTravel

Indirect

CostsEquipments Materials Subcontracting

54.7% 14.6% 11.7% 0.6% 2% 16.4%

Time resources refer to the available time for the implementation of the project. The project is


meant to be accomplished in 36 months. The allocated time for the development of each phase

is in good agreement with the complexity and amount of the activities involved.

2.5. Methodology and associated work plan:

The main objective of this project proposal is to develop a laboratory scale technology and

experimental set-up for the production of hydrogen by steam reforming of hydroxylic

compounds (monohydroxylic alcohols and glycerol) resulted as wastes in biomass processing

or prepared from waste of biomass. All efforts will be concentrated towards the obtaining of the

main end product of the project that is the experimental set-up and catalytic technology for

hydrogen production from waste glycerol correlated with techno-economical and

environmental impact assessments.

Work Plan Strategy. The work plan will be delivered in four research-development (RD)

phases, each with demonstrable deliverables, while a fifth phase of project management and

coordination will support the previous four phases (Table 1).

Figure 2. HYCAT Work Plan.

A detailed description of the phases is presented below.

Phase 1 (month 1 to 8) aims to set a solid foundation for the development of the entire project.

Thus, research activities will focus on the preparation and characterization of novel mixed

catalysts based on alumina and zirconia supported Ni, promoted by either noble metals (Au,

Ag, Pt, Rh) or rare earth oxides (La2O3, CeO2, Y2O3), after a thorough literature survey.

Thermodynamic analysis of ethanol and glycerol steam reforming processes by evaluating the

influence of process parameters such as temperature, pressure and catalyst on the conversion

rates, and reaction products will ensure the basis for the future development of the proposed

technology. Conceptual layout of the steam reforming process will be discussed and established

by the involved partners. Hydrogen production by steam reforming of renewable oxygenates is

basically economically feasible if H2 yields are high and if catalysts can be used in numerous

catalytic cycles without loss of activity. Thus, optimization of bioethanol production in order to

obtain a product as clean as possible for future use in steam reforming will be accomplished. A


Phase 5Project Management

Phase 1RD

Phase 2RD

Phase 3RD

Phase 4RD

33

thorough study aiming the investigation of energetic valorization of biomass wastes will also be

presented.

Phase 2 (month 9 to 18) will focus on developing a technology for H2 production by catalytic

steam reforming of bioethanol obtained from wood waste. Thus, catalysts prepared in the

previous phase will be tested in EtSR reaction (atmospheric pressure, and reaction temperature

in the range 200-400°C) and reaction parameters such as ethanol conversion, H2 selectivity, H2

yield, and catalyst deactivation will be established. Based on the information provided by P2-

ICIA in charge of optimizing the bioethanol production process and of characterizing the

product from the physico-chemical point of view, a reactant ratio ethanol-water as similar as

possible with the bioethanol product, will be used. Catalysts demonstrating maximum

conversion and minimum catalyst deactivation in EtSR will be further used in the bioethanol

steam reforming process. Meanwhile, partner P1-UBB will perform mathematical modeling

and simulation of bioethanol steam reforming process using specific software (ChemCad,

AspenPlus). Model validation will be performed using the experimental data obtained by CO-

INCDTIM in the bioethanol steam reforming process.

Phase 3 (month 19 to 32) is the key phase of the project aiming the development of a

technology for H2 production by waste glycerol catalytic steam reforming. Thus, prepared

catalysts will be tested in the GlySR reaction (atmospheric pressure, and reaction temperature

in the range 500-700°C) by CO-INCDTIM, and reaction parameters will be established for

maximum glycerol conversion, and maximum H2 selectivity and yield. The experimental set-up

will be configured in such a way as to permit analysis of both gaseous and liquid reaction

products. A special attention will be paid to the enhancement of the catalyst life time by

studying the catalyst deactivation process. Deposited coke will be characterized by several

techniques (TGA, TPO, and TEM) in order to establish a correlation between type and amount

of deposited coke, catalyst nature and reaction conditions. All these will enhance the economic

efficiency of the hydrogen production process. Raw material for the process will be provided

by P3-Reviva, after optimization of their original BIOVALP technology for biodiesel

production in order to obtain wastes with higher concentrations of glycerol. Moreover,

provided raw material will be fully characterized from the chemical composition point of view

in colaboration with P2-ICIA. Compounds with possible poisoning effect on the catalyst will be

identified and separated from the waste glycerol solutions. For the separation of the reaction

product of interest – H2, a hydrogen separator based on a Pd membrane will be designed, and

tested by the CO-INCDTIM. P1-UBB will perform the mathematical modeling and simulation


of the waste glycerol steam reforming process using dedicated software packages (ChemCad,

AspenPlus) and validate the model using the experimental data provided by CO-INCDTIM.

Process integration issues (mass and energy) will also be addressed. P4-ROKURA in

collaboration with CO-INCDTIM will design and test the experimental set-up for using a

greater amount of catalyst for the waste glycerol steam reforming process that is 10-50 g of

catalyst.

Phase 4 (month 33 to 36) aims a thorough analysis of the developed laboratory scale

technology from the techno-economical, environmental and scale-up point of view.

Achievement of these goals implies the involvement of each partner of the consortium.

Potential implementation of the developed technology will be also investigated and proposed.

Phase 5 (month 1 to 36) covers the management and scientific coordination and will last for the

entire duration of the project. Activities include project management, the organisation of four

steering group meetings and two workshops, ensuring communication between partners and

with the National Authority for Scientific Research, ensuring a shared understanding of the

work and timetables, as well as submitting scientific and financial reports.

Planning timetable of the HYCAT project is presented below, with the timing for each phase

and each activity (see Table 2 Phase description for each activity description).

Figure 3. GANT diagram of the HYCAT project.

Each phase will provide a series of deliverables such as: methods, products, scientific and

technical reports, laboratory technology, papers, conference presentations, and patents (see


Table 3. Deliverables List).

Key persons list (their CVs are uploaded on the web platform)

Name and surname*

Scientific title

Phase Person-month

Coordinator (CO)

Lazar Mihaela Diana

CS II Dr. 1,2,3,4 33

Almasan Valer CS I Dr. Eng.

1,2,3,4 12

Partner 1 Cormos Calin Cristian

Assoc. Prof. Dr.

Eng.

1,2,3,4 18

Cormos Ana Maria

LecturerDr.

1,2,3,4 12

Partner 2 Roman Cecilia CSI Dr. 1,2,3,4 20

Senila Lacramioara

Drd. Eng 1,2,3,4 30

Partner 3 Koncz Iuliu-Carol

Eng. 1,3,4 10

Dan Radu Cristian

Eng. 1,3,4 4

Partner 4 Petcu Cristian Mihai

Dr. Eng 3,4 18

Dumitrescu Anca Madalina

Dr. Eng 3,4 18

Total 180


Available research infrastructureThere will be made a distinction between the infrastructure of ICT and the rest of the research infrastructure (equipments and facilities for experimentation, own or available through cooperation relationship with other institutions)

(max 1 page)CO INCDTIM has in its laboratory all the equipment and knowhow necessary to prepare

nanostructured supported metal catalysts. For catalysts characterization: Sorptomatic 1990

by Thermoelectron Corporation for adsorption desorption measurements; Bruker D8 XRD

advanced diffractometer; Specs spectrometer for XPS measurements; SDT Q 600 (TA

Instruments) thermogravimetric analyzer. For catalysts testing, the necessary set up

composed by: Microreactivity Reference Catalytic Reactor (PID Eng.&Tech) online with

gas chromatograph (produced by ITIM) and Quadrupole Mass Spectrometer (Prisma Plus

from Pfeiffer Vacuum) to analyze the gaseous products, and a Waters HPLC

chromatograph equipped with ultraviolet and refractive index detectors to analyze the liquid

products.

P1 UBB The infrastructure used by P1 in this project is divided in (1) Information

technology (IT) infrastructure composed by Computers: Intel 2000-4000 MHz, 2-6 GB

RAM, and Software: ChemCAD, Aspen, Thermoflow, GaBi4, Matlab etc and (2)

Experimental infrastructure: Chemical Reaction Engineering laboratory and whole

infrastructure of control and analytical monitoring of chemical processes; Modeling,

Simulation, Optimization and Control of Chemical Processes laboratory .

P2 ICIA performs analyses for biofuels quality certification through its laboratory CABIO

according to the European standard EN 14214 for biodiesel and European standard SR EN

15376 for bioethanol. The relevant infrastructure of CABIO consists in gas chromatograph

(Agilent 6890N) with mass detector (Agilent 5975B), ECD and MPD detectors (Agilent

6890N), FID detector (Agilent 7890A), liquid chromatograph (Agilent 1200 Series)

coupled to mass spectrometer (Applied Biosystem 3200 Qtrap), HPLC (Perkin Elmer 1801-

037 series), FT-IR Spectrometer (Perkin Elmer, Spectrum BX).

P3 Reviva developed an original technology for biodiesel production from soy oil. The

relevant infrastructure consists in: horizontal oil press – pressing capacity 1t/h, 380 V

electric power; tehnological line for preparation of raw materials – capacity 2t/h; pumps for

viscous liquids – capacity 100 l/h, pumping high 5m; POLSTIF tanks – capacity 30t

P4 Rokura The infrastructure used by P4 in this project is: (i) Software Labview industrial

monitoring option; Lab AMESIM – software; Data Acquisition portal 1,8 GB Intel PM;


(ii)Autoclave Mahoney Robinson; Spinning Catalyst Basket Reactor 350 bar, 350 ⁰C;


Budget breakdown by year (lei)Public Budget Private cofinancing (PC) Total PC

2012 2013 2014 2015 Total 2012 2013 2014 2015 Total 2012 2013 2014 2015 Total %

CO 450000 350000 400000 100000 1300000 0 0 0 0 0 450000 350000 400000 100000 1300000 0

P1 80000 110000 110000 100000 400000 0 0 0 0 0 80000 110000 110000 100000 400000 0

P2 185000 315000 200000 100000 800000 0 0 0 0 0 185000 315000 200000 100000 800000

P3 25000 0 200000 25000 250000 12000 0 97700 12000 121700 37000 0 297700 37000 371700 32.7

P4 0 0 200000 50000 250000 0 0 61700 60000 121700 0 0 261700 110000 371700 32.7

Total 740000 775000 1110000

375000 3000000 12000 0 159400

72000 243400 752000 775000 1269400 447000 3243400 7.50

Budget breakdown by category of expensesBudget breakdown / destination (lei)1

Personnel costs

Logistics Travel Indirect costs

Total

Equipments Materials Subcontracting

Coordinator (CO)

Public Budget 603666 345000 18000 0 15000 318334 1300000

Private cofinancing 0 0 0 0 0 0 0

Partner 1 Public Budget 212000 85000 15000 0 25000 63000 400000








1According to Chapter 8 – Budget


Total 1769366 475000 382700 20000 64000 532334 3243400

Table 4. Justification of purchasing major pieces of equipmentEquipment name and characteristics Justification

(CO) Integrated system for catalysts

characterization

Posibility to have constant temperature,

controled increase temperature, constant

and controled flows. Analyser is FID

coupled with mass spectrometer.

We intend to acquire at the beginning of the project (Stage 1) an integrated

system for catalysts characterization. This equipment will enable us to have

more rapid and accurate results to describe: (i) the surface (adsorptive) and

catalytic (nature of catalytic sites) properties of a catalytic material by

performing TPD and TPR measurements and (ii) the catalyst deactivation by

determining the nature and quantity of deposited materials on the catalytic

surface after catalyzed reaction (TPO and TPR measurements). For additivated

catalysts used in this proposal these parameters are not fully explored at this

hour and the results obtained by using the mentioned equipment are extremely

important to fulfill the project objectives.

Gas chromatograph

Two columns, FID and TCD detectors

This equipment will be used for on-line detection of reaction products in phase

of catalysts testing. It will be part of the experimental set-up used to produce

hydrogen.

Partner 1 Information technology

(computer/notebook, IT accessories)

Software licenses (Thermoflex;

ChemCAD, Aspen, GaBi4, Matlab etc.)

These equipments will be used for mathematical modeling and simulation of

hydrogen production by catalytic reforming processes (IT and softwares

aquisition), model validation vs. experimental results, research and

dissemination activities (writing project deliverables, articles, patent

applications etc.).


On-line gas-chromatograph with

multiple chanels

This equipment will be used for experimental evaluations to complete the

existing experimental infrastructure devoted to study the carbon capture

processes.

Partner 2 Fermentor

♦ Power mains: 190-245 V AC/50-60

Hz;♦ Display: LDC 4 × 40♦ fermentor

vessel Pyrex glass ♦Temperature: control

special radiation heat source with gilded

reflector 100 W

Can be used for fermentation of sugars solution for bioethanol production.

Fermentor ensures optimal conditions for the production of bioethanol from

lignocellulosic biomass: pH, temperature, time, etc. Fermentor has 1 liter

capacities, ideal for heat induction, growth of S. cerevisiae, as well as traditional

anerobic and aerobic culture from recombinant microbial, yeast and fungal cells.

Set-up and start-up assistance is included in fermentor


3. Expected impact

(max 3 pages)3.1. Added value of the project results at National, European and International levelExplain how the project results will contribute to increase the social-economical competitivness.

One of the modern world’s major problems is finding new renewable energy resources,

without emissions of poluting gases. The valorization of biomass wastes either by bioethanol

or by biofuels will have an economic impact due to the availability and low value of these

wastes. Implementation of clean technologies for hydrogen production contributes to

approaching the goal of green energy production. Even if the production of green energy is not

cheap at this moment, the oveall profitability on a long term is higher due to the fact that

environment cleaning technologies and infrastructures will not be needed anymore.

Development of new research directions in the area of the biomass wastes utilization as

renewable energy resources has a social component by involving and training of young

researchers in the field of unconventional energy resources development. There are PhD

students in the teams proposed by CO, P2 and P4. The activities developed in the project

implementation can represent the basis for other PhD thesis, contributing to the motivation of

young researchers to remain in the national research field.

The implementation of this project will contribute to increasing the research capacity of

research units (CO and P2) and academic partner (P1) and will widen the international

visibility of Romanian research.

3.2. Dissemination and/or exploitation of project results, and management of intellectual property rights

The project partners intend to publish and disseminate their results, as can be seen in the work

plan description and deliverables list. On the whole, all partners will take responsibility for

scientific publications. Dissemination of obtained scientific results will be accomplished

through: (1) scientific journals; (2) presentations at appropriate international conferences; (3) a

web page and a discussion forum on the Internet. All the results will also be reported to the

Romanian Authorities funding the project.

Publication of the project results will respect the stipulated intellectual property rights,

according to the Author Rights Law no. 8/1996. CO will manage the connection of the

information generated in common by the partners of this project, and will generate the


publications agreed at the partners Meetings and workshops. Acceptance rules will be defined

in the Consortium Agreement.

A dedicated web space will be set-up by CO for the intra-consortium communication and

continuously updated. A project internet page will also be set up for wider dissemination and

as an efficient tool for specialists, accessible also for the possible end-users of the technology

provided through this project.

Management of knowledge (intellectual property)

Dissemination of knowledge and intellectual property rights (IPR) will be specified in detail in

the Consortium Agreement to be signed among all participating institutions to the HYCAT

project. The project results will be protected in acordance with Law nr 8/1996 regarding the

Author Rights published in „Monitorul Oficial” no. 060/06.03.1996, therefore:

(1) The original results (patentable) obtained and developed by each partner on the period

of project implementation are and remain its property according to the actual

legislation.

(2) The scientific results, technologies, know-how, etc obtained in collaboration by two or

more members of the Consortium will belong to each partner in the proportion

established by agreement in acordance with the Consortium Agreement.

(3) Each partner has the right to disseminate its own results.

Confidential information to be provided to the Managing Authority will be appropriated

marked, stating the information is confidential and may be used only for information purposes.

Overall, the proposed basic concept concerning ownership of results and intellectual property

rights (IPR) is that the institution generating such results is the owner of the results and of IPR

and is responsible for their legal protection and transfer. Results jointly developed shall be

jointly owned.

3.2. Business case – only for Type 2 projects (max 1 page, included in the maximum 3 pages for the section)

The project proposal integrates in the proposed Consortium 2 small enterprises, each having

very well defined tasks in the project implementation. These tasks are correlated with their

expertise and economic area in which they activate.

SC REVIVA SRL has a good position at national level in the processing of soybean and

producing of biofuels from soy oil. The resulting wastes consist in solutions of glycerol and

other components with no economic value in the present. By participation in this consortium


the company sought to solve two problems: to manage in an environmental friendly way the

wastes resulted in the technological process (which are now burned to produce some of the

necessary heat) and to add more economic values to these wastes. The fulfillment of both

objectives will enhance the overall profitability of the company and will create new jobs.

SC ROKURA SRL is well known by its implication in green energy projects. One of their

activities is situated in the area of fuels and coal processing using hydrogen in order to reduce

SO2 atmosphere pollution. The interest in the present project is related to their researches for

new, more economic and more ecologic way to produce hydrogen and hydrogen rich gases.

No similar technology for hydrogen production is exploited in our country.

The capacity of our laboratory scale technology is of about 6 t/year which in our estimation

will enhace the profit of each company with about 50.000 lei/year.

Both companies can also obtain profit from this project by a future valorization of the

technology by scale up and the construction of an industrial scale pilot.

The information in this application is hereby certified to be correct.

Project leader,

Dr. Lazar Mihaela Diana

Signature:

Date: 07.11.2011


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