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Warm-up project on Ethylene Glycol for ECH 6412







Introduction and Uses3,4





Ethylene glycol (EG) represented by the empirical formula C2H6O2 is a high volume

chemical, with a production capacity of over million pounds annually in the US alone.

It is a clear, colourless and odourless liquid at room temperature.

It is hygroscopic in nature & has a sweet taste. It dissolves in water and is miscible in

alcohol. Its molecular formula can be represented as





Other names for ethylene glycol are 1,2-dihydroxyethane, 1,2-ethanediol, 2-

hydroxyethanol, ethylene alcohol, glycol, and ethylene dihydrate. The CAS registry #

for EG is 107-21-1





It has a wide range of applications some of which are:

 As anti-freeze for automotive coolants

 As de-icing agents for aircrafts, runways and taxiways.

 As a heat transfer medium due to its ability to hold large amount of heat

before boiling.

 As an industrial drying agent due to its hygroscopic nature.

 As semiconductor developers

 As rubber manufacturing softeners

 As intermediates in polymers – for resinous products, polyester fibres like

Dacron and terylene, esters and ethers

 As printing solvents in lithography

 In the paint & plastics industries where it is used as a solvent for preparing

printers’ inks, stamp pad inks, and inks for ball point pens, and as a softening

agent in cellophane

 As an ingredient in hydraulic brake fluids of automobiles

 In fire extinguishers as a stabiliser to the foam

 In pharmaceuticals preparations like skin lotions and powders as a substitute

for glycerine.

According to a report from the Agency For Toxic Substances & Disease Registry

(ATSDR) approximately 39% of all ethylene glycol produced in the United States, is

used to make antifreeze, 29% is used to make polyester fibres, 26% is exported, and

23% is used to make polyethylene terephthalate (PET) bottles, films, resin products,

and in other miscellaneous industrial applications.





Process alternatives





There have been a number of routes taken by the industry to manufacture EG. Some

of them are:





 Direct production from synthesis gas2

 Carbonylation of formaldehyde2

 Hydroformylation of formaldehyde2

 Reductive hydroformylation of formaldehyde2

 Condensation of formaldehyde2

 Redox process2

 Hydration of ethylene oxide1





Direct production from synthesis gas





45g THF 3400atm CO/H2 9.8g EG

o

0.52g Rh(CO)12Acac 4.5h @ 230 C 1.5g Propylene glycol

1.5g Glycerine





According to Kollar processing costs of the syngas are high due to the slow rate of

reaction and material costs.





Carbonylation of formaldehyde





1M H2CO 900atm CO 98% Glycolic acid

1M H2CO + 0.1M HCl

2M HOAc 1h @ 170oC





This is one of the oldest processes adopted by Du Pont , which produces glycolic acid

which was then converted to methyl glycolate, which was then hydrogenated to EG at

high pressures.





Hydroformylation of formaldehyde





1g Paraformaldehyde 1230psi 1:1 CO/H2 0.26g Glycoaldehyde

10ml N-methyl pyrrolidone 0.016 EG

0.06g Rh(CO)12Acac 3.5h @ 150oC 0.08 MeOH





Reductive hydroformylation of formaldehyde





0.5g Paraformaldehyde 4350psi 2.2:1 H2/CO 0.43g EG

5g N-methyl pyrrolidone 0.3g MeOH

0.019g Rh(CO)12Acac 5h @ 150oC





Condensation of formaldehyde





16% H2CO (aq) NaOH – zeolite 12% glycoaldehyde

o

0.33-0.8 hr 94 C





Redox process





2-10 % Methanolic Formaldehyde ROOR 300psi 6 – 8 % EG

0.16 - 0.33 h

140 – 160 oC





The redox reactions can be carried out in either vapour or liquid phase. The vapour

phase reactions do proceed rapidly, thus offering kinetic advantages.

Hydration of ethylene oxide (EO)





This process is by far the latest process, which is carried out using a reactive

distillation setup with a typical reboiler and condenser. The main reaction is non-

isomolar, exothermic and irreversible and is as follows





C2H4O + H2O  C2H6O

EO water EG





The conventional unit of a reactor inline with a series of separation units has its own

advantages but the reactive distillation setup definitely scores well over the reactor-

separator system by cutting down in the number of equipments involved and also

helps the chemistry by separating the EG produced from the EO so as to minimize the

formation of di- and tri- glycol. Okasinski et al1 have modelled and simulated a

reactive distillation setup and have shown that such a system can be run effectively

and can be made a viable processing alternative.





The top of the column could operate at total reflux. Thus allowing direct vaporisation

of the liquid through the heat of reaction, which is generally removed from the

condenser unit at the top of the column. The condensed vapours from the top of the

column are refluxed totally to the reactive stage, below which is the stripping section

of the column is responsible for separating the EG from the EO. Although the feed

ratio of water/EO is pretty much stoichiometric, the large relative volatility difference

ensures the excess of water/EO in the reactive stage.





Thus with the help of simulation techniques Okasinski et al have been able to find the

optimal reflux ratios, operating conditions in terms of temperature, pressure, feed

flows and also carried out energy balance calculations. They did find that the

conventional system used half as much power as the reactive distillation unit but the

equipment costs more than made up for the balance.









Thus process modelling and simulation is an extremely important tool for any

researcher because it does save a lot of time, money and effort by actually running the

pilot plants. It also gives us a good idea of the system under study and can help out in

addressing our concerns namely in terms of the environment, safety, economic

viability, quality of product that is part of the processes.









References and links

1. Okasinski, M.J.; Doherty M.F.; Ind. Eng. Chem. Res., Vol. 37, No. 7, 1998

2. Kollar J.; Chemtech, Aug.1984, 504 -511

3. http://www-personal.engin.umich.edu/~gordonk/module3.html

4. http://www.atsdr.cdc.gov/toxprofiles/tp96-c4.pdf



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