Recovery of alcohols from purification residue
View Patent ↗A method of reclaiming alcohols from purification residue includes hydrolyzing a purification residue with an aqueous medium in the presence of (i) an acid and (ii) an oxidizing agent.
1. A method of reclaiming alcohols from formal or acetal derivatives thereof comprising hydrolyzing an organic mixture containing an alcohol formal derivate or an alcohol acetal derivate in an aqueous medium in the presence of (i) an acid and (ii) an oxidizing agent.
2. The method according to claim 1 , wherein the alcohol derivate is a polyhydric alcohol formal derivate.
3. The method according to claim 1 , wherein said alcohol is selected from trimethylolethane, trimethylolpropane, trimethylolbutane, neopentyl glycol and pentaerythritol.
4. The method according to claim 1 , wherein said alcohol is selected from methanol, ethanol, propanol, isopropanol, butyl alcohol, isobutyl alcohol or sec-butyl alcohol.
5. The method according to claim 1 , wherein said acid is formic acid.
6. The method according to claim 1 , wherein said acid is an acid functional ion exchange resin.
7. The method according to claim 1 , wherein the hydrolysis reaction is carried out at a pH of from 1 to 4.
8. The method according to claim 1 , further comprising neutralizing said aqueous medium with a neutralizing agent.
9. The method according to claim 1 , wherein said oxidizing agent is aqueous hydrogen peroxide.
10. The method according to claim 1 , wherein the oxidizing agent is supplied to the hydrolysis reaction in an amount of from 2 wt % to 40 wt % based on the dry weight of the organic mixture.
11. The method according to claim 1 , wherein the acid is supplied to the aqueous reaction medium in an amount of from 0.5 wt % to 20 wt % based on the total weight of the aqueous medium.
12. The method according to claim 1 , wherein water is supplied to the reaction medium in a weight ratio of water:organic mixture from 0.5 W/W to 4 W/W.
13. The method according to claim 12 , wherein water is supplied to the reaction medium in a weight ratio of water:organic mixture from 1 W/W to 3 W/W.
14. The method according to claim 1 , wherein the hydrolysis temperature is maintained within the range of from 70° C. to 95° C.
15. The method according to claim 1 , wherein the hydrolysis reaction is carried out for a reaction period of from about 1 hour to about 7.5 hours.
16. The method according to claim 1 , wherein reactants, temperature and reaction time are selected such that the yield (weight basis) of alcohol is from 50% to 99% based on the weight of alcohol formal derivate and alcohol acetal derivate in the organic mixture.
17. The method according to claim 1 , wherein reactants, temperature and reaction time are selected such that the yield (weight basis) of alcohol is from 60% to 98% based on the weight of alcohol formal derivate and alcohol acetal derivate in the organic mixture.
18. The method according to claim 1 , wherein reactants, temperature and reaction time are selected such that the yield (weight basis) of alcohol is from 75% to 95% based on the weight of alcohol formal derivate and alcohol acetal derivate in the organic mixture.
19. The method according to claim 1 , wherein reactants, temperature and reaction time are selected such that the yield (weight basis) of alcohol is greater than 80% based on the weight of alcohol formal derivate and alcohol acetal derivate in the organic mixture.
20. A process for reclaiming alcohols from formal or acetal derivatives thereof from purification residue comprising:
(a) continuously feeding a purification residue stream to a reaction vessel, said purification residue stream containing one or more alcohol formal derivate(s) or one or more alcohol acetal derivate(s);
(b) providing water, an acid and an oxidizing agent to the reaction vessel such that a reaction mixture including the purification residue containing one or more alcohol formal derivate(s) or one or more alcohol acetal derivate(s), water, acid and oxidizing agent is formed;
(c) maintaining the reaction mixture in the reaction vessel at a time and temperature such that one or more alcohol formal derivate(s) or one or more alcohol acetal derivate(s) are hydrolyzed to thereby enrich the reaction mixture with reclaimed alcohol; and
(d) continuously withdrawing a reclaimed alcohol stream from the reaction vessel.