A REGIONAL PROGRAM FOR PRODUCTION OF MULTIPLE AGRICULTURAL FEEDSTOCKS AND PROCESSING TO BIOFUELS AND BIOBASED CHEMICALS

AFRI-CAP Award No. 2011-69005-30515

Advisory Board MeetingSeptember 9, 2013

*Agenda

Administrative Update Carlen Ensley

Sweet Sorghum Update Sonny Viator

Energy Cane Update Paul White

Overall Project Update Donal Day

General Discussion

*Administrative Update

• Project Director Transition• Year 3 Reapplication

• Approved for full amount $3,489,667• Will be required to reapply every year

Audubon Sugar52%

Other AgCenter Departments

24%

LSU10%

Subawards14%

Grant Year 3 Funding

Sustainable Feedstock

Production Systems

Sweet Sorghum

H.P. Viator, W. Alison, M. Blazier, K.J. Han, D. Harrell and H. Liechty

*Mission Statement

*Evaluate sweet sorghum hybrids for agronomic performance, inclusive of their ability to maintain juice quality into the fall season, produce commercial yields on marginal soil, respond to low-input sustainable production practices and deliver quantities of feedstock on a schedule that sustains the viability of the biorefinery.

*Utilization of Winter Legumes for N Fertilizer Credit

(Alison and Han)Hairy vetch

Crimson clover

C o n t a i n e d a n ave r a g e o f 9 9 l b N / A

*Sweet sorghum production following legume incorporation in

the soil

*Soil C sequestration(Blazier and Liechty)

Giddings probe to collect the soil samples Sampled to depth of 90 cm

*Evaluation of nutrient management under tillage regimes

(Harrell)Treatment Biomass

t/AFermentable

sugar t/A

Conv. till No fert.

28.4 a 2.7 a

Conv. till + P and K

29.8 a 2.9 a

No tillNo fert.

23.5 b 2.1 b

No till + P and K

26.5 ab 2.5 ab

*Planting hybrids of different maturity (90-days to 150-days) from early April to June allowed for the harvesting from late July through October (Viator)

*Harvesting initiated at hard-dough stage

*Fresh-weight biomass yield ranged from an average of 18 tons/A to an average of 43 tons/A last year. This year yields ranged from 9.1 to 26.8 tons/A ………. Considerably less than last year thus far, and may be due to N leaching.

*Issues of Concern

Lodging

Ergot

*Unresolved issue is relationship of fan speed and trash extraction

Fan Speed 0 Biomass > 37%

Fan Speed 800 rpm Biomass > 24%

Fan Speed 1100 rpm Biomass is least

*Another unresolved issue is estimating fermentable sugar

between clean stalks and full trash samplesSucrose % Difference

14.34

24.57

10.95

29.52

12.40

18.92

19.80

26.73

20.94

29.42

28.67

27.29

47.08

33.80

33.38

37.25

Brix % Difference

8.54

11.06

15.99

16.58

9.48

14.61

11.51

19.18

13.17

18.26

11.92

15.62

29.35

21.61

19.91

19.18

Based on maturity curves and biomass yield from year one of the project it is projected to take approximately 6,000 acres to provide feedstock to meet the needs of a 1,000 metric ton per day biorefinery

*Changes to Project

• An early planting date in March was accomplished this year

• An attempt will be made to ratoon the hybrids in the early planting date

*Preliminary observations Disappointed in performance of full-season hybrids; expected highest

yields with later maturity

Yield potential of 90-day hybrids is relatively low, but offer early harvest

Soluble solids (Brix) readings appeared to be low relative to other studies (16.5 to 10.9 range). Investigating effects of ergot on Brix.

Unexpected overlap in maturity for medium and late hybrids, which caused gap in feedstock delivery

Sustainable Feedstock

Production Systems

Energy Cane

Paul White

*Macon Ridge Location*Energycane plots were planted in July 2012 with several energycane

varieties, predominately Ho 02-113. We also planted a small demonstration plot area for Dr. Kenneth Gravois containing Ho 02-113, Ho 02-144, Ho 08-9076, Ho 01-07, Ho 06-9001, Ho 06-9002 and CoCP 04-838. For the ratooning test (Task 2.1), we covered the Ho 01-113 with three depths of packed soil: 2, 3, or 4 inches. We did this to determine if the cane needed extra insulation to survive the winter. We also planted a side by side compassion of Ho 02-113 and HoCP 04-838 to test the effects of growing in northern areas of Louisiana on sugar juice and syrup characteristics. All of the cane was sprayed with 3 lbs. of Senor as a preemergence herbicide.

*In June, Dr. Richard Johnson went to Winnsboro to apply nitrogen (N) fertilizer to the fertility study (Task 2.2). The cane was already too tall for a regular height tractor so they had to put out the fertilizer by hand.

*Preliminary Results*For the ratooning study (Task 2.1), stand counts and cane heights

were collected in July 2013. All stalks on a 10 foot section of row in each plot were counted and 10 randomly selected stalks were measured for height from the soil surface to the top dewlap. For counts, data indicated no differences in depth of cover at planting, with averages for 2, 3 and 4 inches of 87,100; 85,500, and 85,700 stalks/Acre, respectively. The p-value for the statistical test was 0.84. Stalk heights were the same for each depth of cover as well with an overall average of 69 inches. The p-value for the statistical test was 0.91. Simulated yields are scheduled for September 2013.

*Houma Location

*The date of harvest test (Task 2.3) was planted in October 2012 at the Spanish Trail Farm in Schriever, La. The following varieties were planted: Ho 72-114, L 79-1002, Ho 02-113, Ho 02-144, Ho 02-147, Ho 08-9076, Ho 01-07, Ho 06-9001, Ho 06-9002, Ho 00-961, HoCP 04-838 and HoCP 96-540. Four replicates of each variety were planted in 50 foot Rows. Sencor applications were used to control weeds. The cane was cultivated, fertilized and layed by in the spring of 2013. The first harvest was August 15, 2013.

*Summary of August HarvestVariety Popluation

Stalks/AYieldTons/A

Brix%

Fiber%

Dry MatterTons/A

L 79-1002 100,200 30 4.1 22 8

Ho 72-114 83,900 38 4.8 24 11

Ho 00-961 66,100 37 5.4 22 10

Ho 01-07 83,900 45 4.9 17 10

Ho 02-113 84,200 42 5.7 21 11

Ho 02-144 85,700 24 4.9 23 7

Ho 02-147 76,800 34 5.6 19 8

Ho 06-9001 79,700 23 4.8 23 6

Ho 06-9002 79,300 26 4.6 23 7

Ho 08-9076 64,800 35 5.1 26 11

HoCp 04-838 50,500 40 6.7 16 9

HoCp 96-540 51,700 37 6.5 16 8

Avg. ECane 80,460 33 5 22 9

Avg. Sugarcane 51,100 39 7 16 9

Overall Project Update

Donal Day

* Feedstock Development

* Sustainable Production

* Logistics and processing

* Conversion and Refining

* Economics, Markets and Distribution

* Education

* Extension

Expand the Southern Regional Agricultural Sector by utilizing sweet sorghum and energy cane for production of butanol, gasoline, bioplastics, isoprene and by-product chemicals.

Dollars per acre to be sustainably earned by a farmer for each feedstock ?

Dollars per gallon of fuel (or per pound of chemical) paid by the consumer ?

Sweet Sorghum July - September

Energy Cane October - March

Bagasse, syrup,woodchips,molasses, etc. April - June

Agricultural ModelStaggered Harvest, Complementary Crops, producing

fermentable sugars and biomass.

Industrial ModelPrimary processing plants supplying centralized biorefineries

Storable syrups as feedstocksPrimary plants drawing on local acreage

*Feedstock Development

* Energy cane- seven molecular markers have been found, four for leaf greenness and three for regrowth damage. Genetic variability was created by cross hybridization between a set of distinct species

* Cross pollination between sugarcane and miscanthus, F1 in field tests across Louisiana

* Cold tolerance testing of Energy cane in North Louisiana location

* Low input testing in North Louisiana

*Sustainable Productionenergy cane

*Plots established

*Cold tolerance trials ongoing

*No herbicide testing

*No diseases detected

Energy cane grows faster than sugar cane

*Sustainable Productionsweet sorghum

*Biomass yield not affected by N&P supplementation

*Legume addition 99 lb N/acre

*Yield average 34-38 ton/acre wet wgt

*No till trials on –going

*C capture by soil –on-going

*Rapid Screening for Biomass Parameters by NIR

400050006000700080009000Wavenumber cm-1

0.4

0.6

0.8

1.0

1.2

1.4

1.6

Abs

orba

nce

Uni

ts *Calibration constructed for sweet sorghum using 218 samples of varying maturity and strains

*Calibration being constructed for energy cane

*NIR being used for screening breeding samples of sweet sorghum and sugarcane

NIR spectra of full stalk sweet sorghum.

Calibration ComponentsBrix, Sucrose, Glucose, Fructose, and Ash in JuiceCellulose, Hemicellulose, Lignin, and Ash in FiberStarch in Sweet Sorghum% Fiber and % Juice in Stalk

Preliminary Sorghum NIR Calibration Models

Component Cellulose % Fiber Hemicellulose % Fiber Acid Soluble Lignin % Fiber

Acid Insoluble Lignin % Fiber

Data Set Calibration Validation Calibration Validation Calibration Validation Calibration Validation

No. of Samples 30 20 30 20 30 20 30 20

R2 84.32 75.35 76.13 40.72 64.25 77.25 54.10 64.52

RMSEE 1.48 1.15 0.272 1.04

RMSEP 1.28 1.5 0.204 0.875

RPD 2.53 2.16 2.05 1.35 1.67 2.15 1.48 1.69

Bias 0.460 -0.395 0.0453 0.119

*Calibration-sweet sorghumBiomass Components

Only data for 50 samples used in these models. Need to add more samples to the model to increase predictive ability.

Overview of Sorghum NIR Calibration ModelComponent Brix in Juice Sucrose % Juice Glucose % Juice Fructose % Juice Juice % stalk Fiber % Stalk

Data Set Validation External Validation External Validation External Validation External Validation External Validation External

No. of Samples 48 13 44 13 44 13 44 13 44 13 43 13

R2 96.34 93.06 94.79 94.14 84.1 85.01

RMSEP 0.512 0.364 0.879 0.48 0.45 0.409 0.426 0.339 2.11 1.87 2.07 1.53

RPD 5.23 8.88 3.84 6.15 4.48 4.96 4.14 5.54 2.58 3.01 2.69 3.65

Bias 0.0294 -0.0482 0.125 -0.254 0.0924 0.186 0.031 0.128 -0.493 0.523 0.572 -0.388

Correlation Coefficient 0.9943 0.9871 0.9797 0.9836 0.9438 0.9617

*Calibrationsweet sorghum

Samples included leaf, stalk and seed heads

This calibration currently being used in breeding program

*Calibration- energy canemodel development

Overview of Energy Cane NIR Calibration Models

Component Brix in Juice Sucrose % Juice Glucose + Fructose % Juice Ash % Juice Juice % stalk Fiber % Stalk

Test Set Validation External Validation External Validation External Validation External Validation External Validation External

No. of Samples 38 17 38 17 38 17 38 17 38 17 38 17

R2 95.62 92.91 78.82 90.49 91.61 93.21

RMSEP 0.374 0.782 0.667 0.788 0.251 0.34 0.0902 0.099 1.26 1.68 1.12 1.73

RPD 5.13 2.39 3.76 3.27 2.18 1.65 3.24 3.06 3.5 2.65 3.86 2.62

Bias -0.135 0.183 0.0259 0.0358 -0.0175 0.107 0.00261 -0.00291 -0.215 0.527 0.132 -0.609

Correlation Coefficient 0.913 0.9541 0.8036 0.9486 0.9262 0.9256

*Feedstock Logistics and Pre-processing

Bagasse storage & fluidization

*Pile storage best for short-term biomass storage

*Bagasse can be fluidized for drying

Harvesting

Harvesting trials with John Deere for sweet sorghum begin in August

*Harvesting

*Sweet Sorghum

Weight loss- 6-7% over 72 hr period on harvesting

3 trials, one acre lots (about 18 rows) 8 inch billets, 3 different fan speeds evaluated

For 2 lots all material, leaves, seed heads delivered to ASI mill, for one lot clean billets only delivered

Analysis of results in progress

*Energy Cane

*7-9% weight loss over a 72 hr period

*Harvesting starts in October

*Demonstrate ScalabilityProduce products for industrial testing

Plant operational- initial process run (sweet sorghum) July 2013

Flexible Pilot Plant Education, Extension and Training Facility

*Milling- Sweet Sorghum*Three runs with 5 ton lots of sweet sorghum( 8 inch billets) conducted.

For two runs the whole plant was harvested, for one the seed heads and leaves were removed.

Feed rate ¼ to ½ T/hr. It was not possible to mill the clean billets because of choking (not enough fiber). A diffuser would be better for sweet sorghum.

*Sweet Sorghum Syrup samples ready for shipment to industrial partners

8-7-2013 %

Brix 70.3

sucrose 14.3

glucose 27.5

fructose 22.7

fermentables 64.5

ash (cond) 13.5

8-19-2013 %

Brix 72.9

sucrose 68.6

glucose 13.2

fructose 11.2

fermentables 93

Ash (cond) 8.4

*Feedstocks Partition into Sugar and Fiber (complex sugars)

Crop Simple sugars(dry lbs)

Fiber(dry lbs)

Sweet Sorghum 184 275

Energy Cane 103 474

Sugarcane Bagasse 0 980

Sugar and Fiber Yields per wet ton of crop

How much is available for fuel conversion if some of the fiber is used to fuel the plant?

*Fiber utilizationsugar and/or power

Mill tandem DiffuserA B A B

Bagasse for power and steam (%)

100 44.8 100 54.5

Bagasse for LC sugars (%) - 24.3 - 19.0Bagasse to storage (%) - 29.9 - 27.5Sugars produced in primary plant (ton/h)

33.8 33.8 34.9 34.9

LC sugars produced (ton/h)

- 9.0 - 6.9

Excess power (MW) 96.7 17.7 101.8 25.7

Modeled on a 420 t/hr processing plant

Partition will be driven by economics

*Pretreatment Options Under Investigation

*High Temperature- water, ammonium hydroxide

*Intermediate Temperature- lime

*Low Temperature –oxidizers

*Enzyme conversion partner (Genencor)

*Lignocellulosic Pre-processing Alkaline Pretreatments

*Composition Changes Pretreatment

Cellulose Hemicellulose Lignin0

10

20

30

40

50

60

Energycane

Untreated Lime treated

Com

posi

tion

(%)

A similar pattern is observed for both crops and all alkaline pretreatments

* Pre-Processing- LignocelluloseHigh Temperature

*Ammonia- 150 C

*The use of ammonium hydroxide as catalyst for biomass pretreatment. An improved recovery of ammonia of up to 70% of recoverable ammonia with sugar yields of at least 75%.

*Pre-Processing LignocelluloseIntermediate Temperature

*Chemical loading: 0.2 g of Lime /1.0 g of dry solid bagasse

Temp. & Time: 120 ˚C, 1 hr

*Total weight : 72 kg

*Total solid : 17.6 % (w/w)

43 hr from start, beginning fermentation, 30 C, 8 rpm

* Pre-Processing- LignocelluloseAmbient Temperature

*Dry ground bagasse were treated with solutions of peroxy-hypochlorite (OxB) or bleach for 30 min, at a pH of 8.

0 1 2 3 4 5 60

10

20

30

40

50

60

70

80

90

% Lignin removed, HCl03

% enz Hydr-HCl03

% lig rem-oxB

%enz Hyr-oxB

Hours

*Alkaline Pretreatment Status

Pretreatment Scale Temp oC Glucose Yield%, on enzyme

treatment

Prime Roadblocks

Water Lab 130-220 NA NA

Ammonia Pilot 115-175 75-85 Reagent loss

Lime Pilot 120 90 effluent

Oxidizers Lab 25 95 cost

*Fuel and By-Product Development

Company Feedstock Process Product

Virent sugars Proprietary fuel

Optinol glucose fermentation butanol

DuPont sugars Proprietary plastics

ASI/LSU Aconitic acid chemical plastics

*Comparing Batch vs. Immobilised Cultures

Batch Fermentation with 4% glucose

Continuous Culture (0.6 ml/min) with 4% glucose

0.42% butanol 0.61% butanol

0.60% OptinolTM 0.99% OptinolTM

Anoxic conditions needed Anoxic conditions maintained

1.5 L media used (5 days) 4.32 L media used (5 days)

3 L reaction vessel 400 ml reaction vessel

0.6 g solvents/L/day 21.384 g solvents/L/day

*Biodegradable polyester from Aconitic Acid

50% glycerol, 48% aconitic acid, and 2% cinnamic acid.

Blue dot is a piece of silicone mat the polymer is cured on.

Bubbles form through the polymer when cured on silicone.

*Economics

*Initial estimates of production cost for energy cane through second stubble are complete

*Energy cane establishment costs being estimated

*Developing a biomass production feasibility index

*EducationCourses are being offered starting with ‘Essentials of Chemical Engineering for Non-Chemical Engineers” and introductory biology for chemical process operators. These courses will be electronically captured and archived for general, on demand availability through the internet.

Two further courses are planned and /or scheduled:“Sustaining the Earth: An Engineering Approach”“Bioreactors and Bioprocessing”

Bioenergy Workshop and Bioenergy Symposia was conducted for K-12 teachers from surrounding areas. A summer sustainability camp (3rd-5th grade) was conducted as part of the Center for Energy and Environmental Studies (CEES).

Four laboratory experiments have been designed and incorporated into the chemical engineering program that will utilized the Audubon Pilot Facility.

*Environmental-LCA

*Effluent water reuse for growing algae was demonstrated.

*Updated LCA model on revised milling model.

*Calculated GHG for gasoline, jet fuel and diesel.

*Set up data collection plan for energy cane milling.

* Field Days were used to highlight both energy cane and sweet sorghum crops as feedstocks for biofuels.

* A Producer Survey was completed to gauge attitudes regarding developing feedstocks for a biofuels industry.

* Sugarcane/Energy cane Variety Identification Guide was updated and published. Presentations were given at annual meetings of the Louisiana Soil and Water.

* Conservation Districts and the Louisiana Agriculture Technology and Management Association. An article was written in the Crops Newsletter trade journal.

*Extension

It has been established that sweet sorghum and energy cane are suitable crops for the production of biofuel and biobased chemicals in the Southeastern Region, and that the approach of using crops with staggered harvest times is feasible. The pilot plant facility has been constructed and is ready on schedule. Plant breeding programs have made a number of successful energy cane crosses which are being evaluated for cold tolerance and range of cultivation. Preliminary economic analysis has been conducted on the proposed crops. An extension program has been established to familiarize farmers with these crops and an education program is being established for training people for work in the biofuels industry.

*Progress Year 2