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Application of recyclable efficient ionic liquid auxiliary in carbonyl-methyl esterification reaction of ethylene oxide

A technology of ethylene oxide carbonyl methyl ester and ionic liquid, applied in the direction of carbon monoxide or formate reaction preparation, carbonyl cobalt, organic chemistry, etc., to achieve the effects of high purity, improved performance, and convenient separation and recovery

Inactive Publication Date: 2016-01-27
南京大学扬州化学化工研究院
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Although the addition of catalytic promoters can significantly improve the catalytic activity of cobalt carbonyl, at the same time, how to quickly and effectively separate the promoters in the products after the catalytic reaction has become a new problem

Method used

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  • Application of recyclable efficient ionic liquid auxiliary in carbonyl-methyl esterification reaction of ethylene oxide
  • Application of recyclable efficient ionic liquid auxiliary in carbonyl-methyl esterification reaction of ethylene oxide

Examples

Experimental program
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Effect test

Embodiment 1

[0016] With 1,4-butanediyl-3,3′-bis-1-vinylimidazole dibromide (ILs) as auxiliary agent, 3.4g ethylene oxide, NaCo(CO) 4 THF solution, 20mL methanol, carbon monoxide (CO) replacement 3 times, P co =2MPa, reacted at 75°C for 5h. After the reaction, diethyl ether was added, ILs precipitated, filtered, and the filtrate was analyzed by GC to obtain the conversion rate of ethylene oxide and the selectivity of 3-HPE.

Embodiment 2

[0018] With PILs as additives, 3.4g ethylene oxide, NaCo(CO) 4 THF solution, 20mL methanol, carbon monoxide (CO) replacement 3 times, P co =2MPa, reacted at 75°C for 5h. After the reaction, diethyl ether was added, PILs were precipitated, filtered, and the filtrate was analyzed by GC to obtain the conversion rate of ethylene oxide and the selectivity of 3-HPE.

Embodiment 3

[0019] Embodiment 3 (comparative example)

[0020] Additive-free, 3.4g ethylene oxide, NaCo(CO) 4 THF solution, 20mL methanol, carbon monoxide (CO) replacement 3 times, P co =2MPa, reacted at 75°C for 5h. After the reaction, GC analysis was performed to obtain the conversion rate of ethylene oxide and the selectivity of 3-HPE.

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Abstract

The invention provides an application of a poly(ionic liquid) as an auxiliary agent in a carbonyl-methyl esterification reaction of ethylene oxide to prepare methyl 3-hydroxypropionate. The poly(ionic liquid) can not only be used for improving the conversion ratio of ethylene oxide and the selectivity of methyl 3-hydroxypropionate, but also can be recovered through simple centrifugalization and separation after a catalytic reaction. The method improves the purity of a product, shortens the product purification flow and lowers the cost.

Description

1. Technical field: [0001] The invention relates to a recyclable high-efficiency ionic liquid additive used for cobalt carbonyl to catalyze the carbonyl methylation reaction of ethylene oxide to synthesize 3-hydroxypropionate methyl ester. 2. Background technology: [0002] 1,3-Propanediol (1,3-PDO) is mainly used in the production of new polyester poly(trimethylene terephthalate) (PTT), and can also be used in the synthesis of various drugs, plasticizers, detergents, emulsifiers and other fine Raw material for chemical products. The PTT synthesized by 1,3-PDO and terephthalate (ester) not only has the chemical stability of polyethylene terephthalate (PET), but also has the good resilience and anti-pollution of nylon 6 and nylon 66 It is a new type of polyester fiber with a very wide application prospect. This makes 1,3-PDO have a very large market demand. Currently, 1,3-PDO is prepared by three main processes: acrolein hydration and hydrogenation, ethylene oxide carbonyl...

Claims

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Application Information

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IPC IPC(8): C07C69/675C07C67/36C01G51/02B01J31/20
Inventor 范以宁刘玉炳赵兵张忠良陆海孟周军许波连
Owner 南京大学扬州化学化工研究院
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