Ethylene glycol bis(4-trimellitate anhydride) synthesis
- Product Name:Ethylene glycol bis(4-trimellitate anhydride)
- CAS Number:1732-96-3
- Molecular formula:C20H10O10
- Molecular Weight:410.29
107-21-1
552-30-7
1732-96-3
Trimellitic anhydride (1.0 mol, 192 g) was mixed with ethylene glycol (0.55 mol, 34 g) in a reactor and nitrogen was vented to remove air. The reaction mixture was heated to 230-240°C under continuous nitrogen protection, during which water was generated and distilled. When the amount of water distilled approached the theoretical value (18 g), the system pressure was reduced to 10-15 mmHg while the temperature was raised to 260°C and the reaction was maintained at this condition for 2 hours. Upon completion of the reaction, the reaction mixture was cooled and recrystallized from 900-1200 g of acetone to afford the intermediate ethylene glycol trimellitate as a white powder (176 g, 86% yield). Subsequently, the intermediate was dissolved in 5% aqueous sodium hydroxide solution and hydrolyzed by adjusting the pH to 1-3 with dilute hydrochloric acid, and dried after completion of the reaction to obtain the final product ethylene glycol trimellitate as white powder (211.8 g, 95% yield).
107-21-1
1370 suppliers
$10.00/25g
552-30-7
423 suppliers
$16.00/25g
1732-96-3
90 suppliers
$9.00/250mg
Yield:1732-96-3 86%
Reaction Conditions:
at 230 - 260; under 10 - 15 Torr; for 2 h;Inert atmosphere;
Steps:
1
A solution of trimellitic anhydride (1.0 mol)192 g was mixed with ethylene glycol (0.55 mol) of 34 g,Nitrogen emptying. In nitrogen holdContinued protection to a temperature of 230-240 ° C,This time will continue to have water distillate,Close to the theoretical amount of water (18 grams) after the distillation,Vacuum 10-15mmHg down to 260 for 2 hours, cooling,Refined with 900-1200 grams of acetone,The intermediate trimellitic anhydride ethylene glycol ester, white powder 176 grams, the yield of 86%. The intermediate was hydrolyzed with a 5% aqueous solution of sodium hydroxide,Dilute hydrochloric acid to pH = 1-3,Dried to the final product trimellitic acidEthylene glycol esters,White powder 211.8 g, yield 95%.
References:
CN105968050,2016,A Location in patent:Paragraph 0060; 0061