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Chemical Reactors Project

Negoita – Giras Silvia

Group 1244 E

Project Coordinator: conf.dr.ing. Tiberiu Danciu

1.Literature..................................................................................................................................3

1.1. General Aspects................................................................................................................................3

1.2. Synthesis of DME……………………………………………………………...………..………………………………………………4

1.3. Process Tehnology………………………………………………………………………………………………………………………4

1.3.1. Process

Description………………………………………………………………………………………………………………4

1.3.2. Process Details……………………………………………………………………………………………………………..

………5

1.4. Catalysts……………………………………………………………………………………………………………………………………..8

1.5. Aim of the Project……………………………………………………………………………………………………………………….9

1.6. Material Balance…………………………………………………………………………………………………………………………9

1.7.Kinetics and Thermodynamics.......................................................................................................11

2.Mathematical Model of the Reactor..........................................................................................15

2.1.Equations and Preliminary Calculation...................................................................................15

3.Simulation of the Reactor under different Operating Conditions................................................19

3.1.HYSYS Simulation………………………………………………………………………………………………………19

2. References……………………………………………………………………………………………………………………………………23

2

1. Literature 1.1. General Aspects

Dimethyl Ether (DME) is an organic compound with the formula CH3OCH3. Being the simplest ether, it is a colourless gas that is a useful precursor to other organic compounds and an aerosol propellant. Dimethyl ether is also promising as a clean-burning hydrocarbon fuel.

Dimethyl ether is a colorless gas with a faint ethereal odor.Its vapor pressure is about 0.6 MPa at room temperature and the boiling point islow, more precisely - 25.1°C.It was soon realised that its physical properties were so similar to those of liquefied petroleum gas (LPG), that DME can be distributed, stored and transported using LPG handling technology. It is easily ignited,its vapors are heavier than air. Any leak can be either liquid or vapour.

In present, DME’s main application is as a propellant for spray cans for paints, agricultural chemicals, cosmetics etc. Its annual production cand reach as much as 150,000 t/year worldwide. A toxicity study of its use as propellant to replace fluorocarbons has confirmed that its toxicity is extremely low, similar to that of LPG, lower than that of methanol. As a good quality DME is relatively inert, non-corrosive and non-carcinogenicm meaning that is almost non-toxic, and does not form peroxides by prolonged exposure to air.As it was already been said, similar to LPG, it requires mild pressurization to be stored as a liquid. Some physical properties of DME in comparison with some main constituents of LPG are presented in Table 1. DME burns with a clean blue flame over a wide range of air/fuel ratios.

Table 1. Physical Properties of DME and otherComponents of DME

Properties DME Propane Methane Diesel fuelChemical formula CH3OCH3 C3H8 CH4Boiling Point (C) -25.1 -42.0 -161.5 180 - 370Liquid density (g/cm3 @20C) 0.67 0.49 0.42 0.84Liquid viscosity (kg/ms @25C) 0.12-0.15 0.2 - 2 - 4Specific gravity of gas (vs. Air) 1.59 1.52 0.55 -Vapor pressure (MPa @25C) 0.61 0.93 - -Explosion limit (%) 3.4 - 17 2.1 - 9.4 5 - 15 0.6 - 6.5Cetane number 55-60 5 0 40 - 55Net calorific value (kcal/Nm3) 14,200 21,800 8,600 -Net calorific value (kcal/kg) 6,900 11,100 12,000 10,000

From ecologically point of view, it can be said that DME is decomposed in a troposphere for several ten hours and has no concern on the greenhouse effect and ozone layer depletion. The Cetane number of DME is high, so that it can be used in diesel engines. The diesel engine test with DME showed that no black diesel exhaust smoke was emitted at all, Nox emissions were much lower than with diesel fuel and fuel consumption as measured by calories was identical to diesel fuel.

3

1.2. Synthesis of DME

Today, DME is primarily produced by converting hydrocarbons, predominantly sourced from natural gas (and to a lesser extent via gasification of coal), to synthesis gas (syngas). Synthesis gas is then converted into methanol in the presence of catalyst (usually copper-based), with subsequent methanol dehydration in the presence of a different catalyst (for example, silica-alumina) resulting in the production of DME. As described, this is a two-step (indirect synthesis) process that starts with methanol synthesis and ends with DME synthesis (methanol dehydration). The same process can be conducted using organic waste or biomass. Approximately 50,000 tons were produced in 1985 in Western Europe using the methanol dehydration process. Alternatively, DME can be produced through direct synthesis, using a dual catalyst system that permits both methanol synthesis and dehydration in the same process unit, with no methanol isolation and purification, a procedure that, by eliminating the intermediate methanol synthesis stage, the licensors claim promises efficiency advantages and cost benefits.

The reaction formulas concerning DME synthesis are as follows:

3CO+3H2 → CH3OCH3 +CO2 (1)2CO+4H2 → CH3OCH3 + H2O (2)2CO+4H2 → 2CH3OH (3)2 CH3OH → CH3O CH3+ H2O (4)CO+H2O → CO2 +H2 (5)

From the reactions written above, by combining some methanol and dehydration catalysts in the same reactor, reactions (1) and (2) can proceed simultaneously, resulting in direct synthesis of DME. The water-gas-shift reaction is also involved, since methanol catalyst is also an effective water-gas-shift catalyst:

H2O + CO → H2 + CO2 (6)

The single-step DME synthesis chemistry can be represented as a combination of Equations (1), (2), and (3):

3CO + 3H2 → CH3OCH3 +CO2 (7)

1.3. Process Tehnology

1.3.1 Process Description

Figure 1 is a preliminary process flow diagram (PFD) for the dimethyl ether production process. The raw material is methanol, which may be assumed to be pure. The feed plus recycle is pumped in P-201;

4

heated, vaporized, and superheated in a heat exchanger (E-201); and then sent to the reactor (R-201) in which dimethyl ether (DME) is formed. The reaction that occurs is shown below. The reactor effluent is cooled and partially condensed in a heat exchanger (E-202), and it is then sent to the separation section. In T-201, “pure” DME is produced in the top stream (distillate), with methanol and water in the bottom stream (bottoms). In T-202, the distillate contains methanol for recycle, and the bottoms contains waste water. The desired dimethyl ether production rate is 100,000 tonne/y.

1.3.2. Process Details

Feed Stream- Stream 1: methanol, from storage tank at 1 atm and 25°C, may be assumed pure Effluent Streams- Stream 7: dimethyl ether product, required 100,000 tonne/y, may be assumed pure- Stream 10: waste water stream, may be assumed pure in material balance calculations, is not

pure, so there is a cost for its treatment Equipment- Pump (P-201): The pump increases the pressure of the feed plus recycle to a minimum of 15 bar- Heat Exchanger (E-201): This unit heats, vaporizes, and superheats the feed to 250°C at 15 bar.

The source of energy for heating must be above 250°C. - Reactor (R-201):

The following reaction occurs:

(8)

The reaction is equilibrium limited. The conversion is 80% of the equilibrium conversion at the pressure and exit temperature of the reactor. Based on the catalyst and reaction kinetics, the reactor must operate at a minimum of 15 bar. The reactor operates adiabatically, and, since the reaction is exothermic, the reactor effluent temperature will be above 250°C. If you choose, you may run the reactor isothermally, in which case you need a medium to remove the heat generated, and that medium must always be at a lower temperature than that of the reactor.The equilibrium expression for the reaction in Eq. (8) is:

(9)

- Heat Exchanger (E-202): This unit cools and partially condenses the reactor effluent. The valve before this heat exchanger reduces the pressure. This exit pressure may be at any pressure below the reactor pressure, but must be identical to the pressure at which T-201 operates.

- Distillation Column (T-201): This distillation column separates DME from methanol and water.- Heat Exchanger (E-203): In this heat exchanger, the contents of the top of T-201 (pure dimethyl

ether) are condensed from saturated vapor to saturated liquid at the column pressure at a rate three

5

times the flow of Stream 7. One-third of the condensate becomes Stream 7 and the remainder is returned to the column. The cost is for the amount of cooling medium needed to remove the necessary energy. The cooling medium must always be at a lower temperature than the stream being condensed.

- Heat Exchanger (E-204): In this heat exchanger, you may assume that one-half of the flow of Stream 8 is vaporized from saturated liquid to saturated vapor at the column pressure and is returned to the column. The temperature of the stream being vaporized is the bubble point temperature of the methanol-water mixture at the column pressure. The cost is for the amount of steam needed to supply the necessary heat. The steam temperature must be above the temperature of the vaporizing stream.- Distillation Column (T-202): This distillation column separates methanol for recycle from water.

The separation may be assumed to be perfect. However, since we know this cannot be true in practice, the water stream is actually a waste water stream, and there is a cost for its treatment. The temperature of the distillate is the temperature at which methanol condenses at the chosen column pressure. The valve before T-202 is optional. It is needed if the pressure of T-202 is chosen to be lower than that of T-201. If the pressures are the same, the valve can be eliminated. If you desire a higher pressure in T-202, you must add a pump in place of the valve.- Heat Exchanger (E-205): In this heat exchanger, the contents of the top of T-202 (pure methanol)

are condensed from saturated vapor to saturated liquid at the column pressure at a rate three times the flow of Stream 9. One-third of the condensate becomes Stream 9 and the remainder is returned to the column. The cost is for the amount of cooling medium needed to remove the necessary energy. The cooling medium must always be at a lower temperature than the stream being condensed.- Heat Exchanger (E-206): In this heat exchanger, you may assume that one-half of the flow of

Stream 10 is vaporized from saturated liquid to saturated vapor at the column pressure and is returned to the column. The temperature of the stream being vaporized is the boiling point of water at the column pressure. The cost is for the amount of steam needed to supply the necessary heat. The steam temperature must be above the temperature of the vaporizing stream.- Other Equipment : For two or more streams to mix, they must be at identical pressures. Pressure

reduction may be accomplished by adding a valve. All of these valves are not necessarily shown on the attached flowsheet, and it may be assumed that additional valves can be added as needed at no cost. Flow occurs from higher pressure to lower pressure. Pumps increase the pressure of liquid streams, and compressors increase the pressure of gas streams.

The schema of the process in presented in the figure below:

6

Figure 1: Installation schema for DME process

7

1.4. Catalysts

DME can be synthesized via the dehydration of methanol over solid-acid catalysts such as γ-alumina (γ-Al2O3), alumina that has been modified with silica and phosphorus, Al2O3-B2O3, and zeolites in a temperature range of 523-673 K and at pressures up to 18 bar.3-6 Alumina is a common catalyst for the dehydration of methanol. However, despite its high activity, alumina has a tendency to adsorb water, which is one of the products, and thereby loses its activity in the presence of water, because of its hydrophilic nature. In order to establish the role of solid-acid catalysts, a series of commercial γ-Al2O3

catalysts were prepared, tested, and screened for methanol dehydration to DME under the same operating conditions. The BET surface area, pore volume, and pore diameter of the catalysts are obtained are similar, which implies that the samples have similar porous structures. The XRD patterns of samples (Figure 2) clearly indicate that the catalysts are highly amorphous in nature, with a low level of crystallinity in the form of cubic aluminum oxide.

Figure 2.

Table 3 shows the catalytic performance for the dehydration of methanol over γ-Al2O3 catalysts at T of 573 K, P of 16 bar, 26.07 h-1, under steady-state conditions. As reported in Table 3, all the γ-alumina catalysts were reasonably active and selective for DME formation. The MDH-4 exhibited the lowest activity for DME formation among all of the samples. It can be observed that samples MDH-3 and MDH-5 exhibited the highest conversion and activity among other samples. Sample MDH-1 is slightly more active than sample MDH-2 under the same reaction conditions.

Table 2. Textural Properties of the Fresh Catalysts

1.5. Aim of the Project

The aim of theproject is to design an installation for obtaining dimethylether from methanol as basic raw

material, having the following characteristics:

Annual production capacity: 52100 t/year

Molar Flowrate of DME 205.89 kmole/h

Mass Flowrate 6512.5 kg/h

Work Hours: 8000 h/year

Temperature of the Feed at the Entrance in the Reactor: 239oC (510oK)

Pressure at the Entrance in the Reactor: 15.2 atm

Raw materials composition, in mass percent: 98.5% methanol, 1.5% water

Final Product Purity: 99.92% (mass)

1.6. Material Balance

In order to compute the mass balance, some data are assumed (computed concerning the value „n” imposed at the seminary):

Mass flow of DME: 6512.5 kg/h Composition of the methanol at the entrance in installation: w11= 0.985; Composition of DME at the entrance in installation: w12=0; Purity of DME at the exit : w72 =0.9992; Purity of H20 in the steam 7: w73 =0; The composition of waste for methanol: w101 =0.033; The composition of waste for DME: w102=0 (no DME); Composition for recycle (most of the MeOH and almost no water):

w91=0.905 w93=0.015

Using the well known program MathCad together with normalization, the partial and overall mass

balance could be easily solved. The solution is given as it follows:

And the final solutions also solved in MathCad are:

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And the final solutions also solved in MathCad are:

1.7. Kinetics and Thermodynamics

As it is well known also from other lectures, using thermodynamics, the conversion of different forms of energy is studied, while the kinetics gives us information about the rate of a reaction.

10

sol

0

0

1

2

3

4

5

6

7

8

9

10

11

12

13

14

15

16

17

18

9289.83022

2777.33022

4600.73544

13890.56566

13890.56566

7378.06566

0.015

0.0008

0.967

0.08

0.30672

0.49497

0.19831

0.9585

0.0265

0.015

0.57675

0.04989

0.37336

=

These main reactions listed below are fundamental also for problem solving in other chemical reactors problems and their main definition is written next to it as follows:

The thermal effect of chemical reactions at constant pressure is the enthalpy. The above signs signifies:

T0 – standard temperature

HT0,i – standard enthalpy of species i

cp(T0) – specific heat of species i at standard temperature

The sign for enthalpy was written in thermodynamic convention; however in engineering is needed the

opposite, so a minus should appear.

The Kirchhoff law is applied in order to determine the enthalpy of a reaction at a certain temperature.

The 0 index stands for standard parameters (20°C and 1 atm).

Table 3.Compounds properties (Reid R.C, Prausnitz J.M., 1987)

Component i

Domeniu temp [K]

Entalpie de formare [J/mol]

Entropie [J/mol/K]

Caldura molara [J/mol/K]

CPA CPB CPC CPDCH3OH 298-1000 -201200.00 239.7 2.12E+01 7.09E-02 2.59E-05 -2.85E-08

CH3OCH3 298-1000 -184200.00 266.6 1.70E+01 1.79E-01 -5.23E-05 1.92E-09

H2O 298-2500 -241840.00 188.74 3.22E+01 1.92E-03 1.06E-05 -3.60E-09

The free enthalpy (Gibbs) is the thermodynamic criteria of the possibility of

(spontaneous) chemical reactions.

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For all three parameters described below I chose the temperature in the range 298 – 700 K.

Thermodynamic of Chemical ReactionTable 4.

Temperatura [K]

Reaction Heat [J/mol]

Reaction Entropy[J/mol/K]

Free Energy [J/mol]

298 -2.36E+04 -2.41E+01 -1.65E+04300 -2.36E+04 -2.40E+01 -1.64E+04350 -2.30E+04 -2.22E+01 -1.53E+04400 -2.25E+04 -2.07E+01 -1.42E+04450 -2.19E+04 -1.94E+01 -1.32E+04500 -2.14E+04 -1.83E+01 -1.23E+04550 -2.09E+04 -1.74E+01 -1.14E+04600 -2.05E+04 -1.66E+01 -1.05E+04650 -2.00E+04 -1.59E+01 -9.71E+03700 -1.97E+04 -1.53E+01 -8.93E+03

Equilibrium ConstantTable 5.

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Temperature [K]

Reaction Heat [J/mol]

Reaction Entropy [J/mol/K]

Free Energy [J/mol]

Equlibrium Constant

Kp

298 -2.36E+04 -2.41E+01 -1.65E+04 773.47300 -2.36E+04 -2.40E+01 -1.64E+04 725.80350 -2.30E+04 -2.22E+01 -1.53E+04 190.54400 -2.25E+04 -2.07E+01 -1.42E+04 71.64450 -2.19E+04 -1.94E+01 -1.32E+04 34.11500 -2.14E+04 -1.83E+01 -1.23E+04 19.11550 -2.09E+04 -1.74E+01 -1.14E+04 12.03600 -2.05E+04 -1.66E+01 -1.05E+04 8.25650 -2.00E+04 -1.59E+01 -9.71E+03 6.03700 -1.97E+04 -1.53E+01 -8.93E+03 4.64

Convertion of Chemical ReactionTable 6.

Temperature [K]

Reaction Heat [J/mol]

Reaction Entropy [J/mol/K]

Free Energy [J/mol]

Equlibrium Constant

Kp

Conversion

298 -2.36E+04 -2.41E+01 -1.65E+04 773.47 0.98300 -2.36E+04 -2.40E+01 -1.64E+04 725.80 0.98350 -2.30E+04 -2.22E+01 -1.53E+04 190.54 0.97400 -2.25E+04 -2.07E+01 -1.42E+04 71.64 0.94450 -2.19E+04 -1.94E+01 -1.32E+04 34.11 0.92500 -2.14E+04 -1.83E+01 -1.23E+04 19.11 0.90550 -2.09E+04 -1.74E+01 -1.14E+04 12.03 0.87600 -2.05E+04 -1.66E+01 -1.05E+04 8.25 0.85650 -2.00E+04 -1.59E+01 -9.71E+03 6.03 0.83700 -1.97E+04 -1.53E+01 -8.93E+03 4.64 0.81

13

The two vertical lines above show the catalytic activity in the chemical process.

2. Mathematical Model of the Reactor 2.1. Equations and Preliminary Calculation

14

The aim of this step is to establish the mathematical model of the process. This is made with the aid of MathCad Programme. Firstly, the equlibrium reaction is being computed:

(10)

The stochiometric matrix is:

The charactersitic of the compounds are taken and used in the software from „The Properties of Gases & Liquids, 4th ed., Robert C. Reid, John M. Prausnitz, Bruce E. Poling, McGraw-Hill, New York, 1987.”

The equlibrium temperature must be in the range 200 -400 K. The equlibrium convertion is established like it follows:

(11)

A regression is made and the activation energy is established:

(12)

15

1 0.5 0.5( )=

Xechk

4 Kpk 2 Kpk

4 Kpk 1

=

Ea

1.728 104

8.487 103

5.07 103

1.254833 103

=

An estimation is made upon the increase of the adiabatic temperature:

(13)

A graph is obtained using convertion in function of temperature:

Figure 3

A change in the input mass flow in the reactor is done which is taken from the material balance:

The temperature at entrance of the mixture: TI = 538⁰C

The average molar mass at the input is computed using the following formula:

(14)

16

T ad yI1

H r TI Cp TI =

T ad 161.229064= K

GmI 13890.56= kg/h

MmedIj

yIjMj =

being the solution.

The initial molar concentration is also computed as it follows:

(15)

Kmol/m3

From this point it can easily be computed the previously mentioned parameters: kS, KM, KW and also K:

(16)

KmoleM/kgcat h∙

(17)

m3/kmoleM

(18)

m3/kmoleW

17

MmedI 31.92672= kg/kmol

CI medI gI=

CI

0.32473

6.24434 103

9.03871 103

=

ks k01exp

Ea1

TI

=

ks 0.601544=

KM k02exp

Ea2

TI

=

KM 3.82494 103=

KW k03exp

Ea3

TI

=

KW 1.048538 103=

(19)

The geometrical charactersticis are computed as follows:

m/s is choosen from the range 0.2 – 0.3 m/s

where vf is the fictive rate

The interior diameter of the reactor is computed with the formula:

(20)

m

The catalyst diameter particle is considered to be: dp = 3 mm (taken from Bercic, I.E.C. Res., 1992)

Also the density of the catalyst is considered to be : ρcat = 3268 kg/m3 (taken from Bercic, I.E.C. Res., 1992)

The concentration (with respect to the volume) in function of the variable z (the height) and X (the convertion) is determined after some auxiliary functions are defined:

kmole/m3 (21)

The reaction rate r1(z,X) is determined:

(22)

18

K k04exp

Ea4

TI

=

K 3.767444=

vf 0.275=

dint

4 GmI

3600 vf medI=

dint 1.28284=

C z X( ) med z X( ) g z X( )=

r1 z X( )

ks z X( ) KM z X( )2 C z X( )1 2 C z X( )2 C z X( )3

K z X( )

1 2 KM z X( ) C z X( )1 KW z X( ) C z X( )3 4=

But this is finalised by computation of some other parameters:

The values between which we integrate, the dependent variable z are:

The step is 0.01 m.

By using the Runge – Kutta integration with variable step, the derivatives of convertion with respect to z and X(deryXM(z,X)) are determined:

(23)

1/m

The derivatives of temperature with respect to z and X can also be determined: (deryT(z,X)):

deryT z X( ) 7.623888= K/m

19

vf z X( ) 0.275=

p z X( ) 1.284324 103=

dp z X( ) 3 103=

z1 0

z2 6.5

deryXM z X( )Atr z X( )

GMI1r z X( )1 strat z X( )=

deryXM z X( ) 0.047248=

deryT z X( )i

H r z X( )i

r z X( )i strat z X( )4 KT z X( ) T z X( ) Ta z X( )

dint z X( )

Gm z X( )

Atr z X( )cpmed z X( )

= (24)

The derivatives of pressure with respect to z and X (dery p(z,X)) is computed:

(25)

atm/m

Finally, the Runge – Kutta integration is done:

sol Rkadapt init z1 z2 npoints D( )=

For a convertion of 0.6052, using the integration above it results that the height of the reactor is 6.21 m.

3. Simulation of the Reactor under Different Operating Conditions

The process of dimethyl etheis syntesis from methanol is submitted to different simulating

operations, in order to determine the proper and optimum working conditions regarding the design of a

real plant in the future. This step is mandatory after doing all the the previous steps described above.

The simulation is done in a plant simulator program, more precisely HYSYS 3.2. The simulation data are

put with some assumptions with economic aspects but also by the productivity that must be obtained

and the quality of the final product. As it was previously mentioned,from economic point of view, an

important factor is that the recycling must be as low as possible, thus a major condition imposed by this

fact is the recylced amount of methanol.Also from economical point of view the operating conditions

are important, thus the working temperature and pressure has to be as low as possible but in the same

time high enough to ensure a good convertion and quality of the final product.

In order to establish the optimum data for the proper operating of the plant, beside the simulator

program HYSYS 3.2. also the soft MathCad will be used to establish a mathematical model as close as

possible to reality.

20

deryp z X( ) f z X( )vf z X( )

2

dp z X( ) med z X( ) 1.0125 10

5=

deryp z X( ) 0.030797=

D z X( )

deryXM z X( )

deryT z X( )

deryp z X( )

=

3.1. HYSYS Simulation

In order to make the simulation some values are needed listed as follows:

Mass Flowrate: 6512.5 kg/h

Stream 1: input temperature and pressure: 25⁰C and 1 atm (101.3 kPa)

Input composition in mass fraction: 0.985 methanol, 0.015 H2O

Stream 4: The input temperature in the reactor is 239⁰C

Distillation Column T-201: to have the initially given purity of DME of 99.92% some modifications

have to be made in the „Monitor ” field it was redefined a Comp Fraction of 0.9992. Also the

Comp Recovery was changed in 0.9600 in order to establish a proper liquid recovery.

Stream 7: Verification is made upon the final DME product of 99.92% purity.

Stream 9: The recycled liquids composition must attain a certain value in order that the recovery

of the methanol to be as high as possible, otherwise the nstallation cost will not be economically

viable (mass fraction methanol: 0.901433).

The installation scheme is presented in Figure 3:

Figure 3: Installation Scheme in HYSYS Simulator

Also some data form the simulator are presented as follows:

Figure 4: Temperature Change in Simulator

21

Figure 5: Compositon Fraction and Recovery Change in T-201 Column

Finally the material streams, energy streams and compositions established in HYSYS simulator are as

follows:

Figure 6:Material Stream, Energy Stream and Compositions

22

4. References

23

Reid R.C, Prausnitz J.M., The properties of gases and Liquids,1987

M. Mollavali, F.Yaripour, H.Atashi, S. Sahebdelfar, Intrinsic Kinetics Study of Dimethyl Ether Synthesis

from Methanol on γ-Al2O3 Catalysts, Ind. Eng. Chem. Res. 2008, 47, 3265-3273

G. Bercic, J. Levec, Intrinsic and global reaction rate of methanol dehydration over γ -Al2O3 pellets

www.cemr.wvu.edu/~wwwche/publications/projects

www.wikipedia.org/dimethyl ether

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