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Method for preparing maleic acid isopropyl ester

A technology of diisopropyl maleate and maleic anhydride is applied in the field of preparing diisopropyl maleate, can solve the problems of complex process route, low reaction yield and high cost of raw materials, achieves less dosage and less reaction Effects of lower temperature and shorter reaction time

Inactive Publication Date: 2013-09-18
HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of this invention is to provide a kind of method for preparing diisopropyl maleate, overcome the prior art process route complexity, reaction yield is low, the defect that raw material cost is high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] (1) Preparation of 1-(4-sulfonic acid) butylpyridinium salt

[0026] Dissolve 20g of 1,4-butyl sulfonate sultone in 150mL of acetone, slowly add 20g of pyridine dropwise, and heat under reflux at 30°C for 12h to obtain 1-(4-sulfonic acid)butylpyridinium salt. Diethyl ether and ethyl acetate were washed three times, suction filtered, and vacuum-dried. The measured yield was about 80%.

[0027] (2) Preparation of 1-(4-sulfonic acid) butylpyridine bisulfate

[0028] Dissolve 1-(4-sulfonic acid) butylpyridinium salt in water, add concentrated sulfuric acid in equal amount, reflux reaction at 60°C for 12h, remove water by rotary evaporation, wash with ether, separate liquid, at 50°C After vacuum drying, a light yellow viscous liquid was obtained, which was 1-(4-sulfonic acid) butylpyridine hydrogensulfate.

[0029] (3) Preparation of diisopropyl maleate

[0030] Add 10g of maleic anhydride, 24g of isopropanol, 1g of 1-(4-sulfonic acid) butylpyridine bisulfate, and 20g of ...

Embodiment 2

[0032] (1) Preparation of 1-(4-sulfonic acid) butyl imidazolium salt

[0033] Dissolve 20g of 1,4-butyl sultone sultone in 150mL of ethyl acetate, slowly add 12g of N-methylimidazole dropwise, and heat under reflux at 40°C for 10h to obtain 1-(4-sulfonic acid)butyl The imidazolium salt was washed three times with ether and ethyl acetate, filtered with suction, and dried under vacuum. The measured yield was 60%.

[0034] (2) Preparation of 1-(4-sulfonic acid) butyl imidazole hydrogen phosphate

[0035] Dissolve 1-(4-sulfonic acid) butylimidazolium salt in water, add phosphoric acid in an equal amount, reflux at 60°C for 3 hours, remove water by rotary evaporation, wash with ether, separate liquids, vacuum at 50°C After drying, a light yellow viscous liquid is obtained, which is the ionic liquid catalyst of 1-(4-sulfonic acid) butylimidazolium hydrogen phosphate.

[0036] (3) Preparation of diisopropyl maleate

[0037] Add 10g of maleic anhydride, 24g of isopropanol, 1g of 1-...

Embodiment 3

[0039] (1) Preparation of 1-(4-sulfonic acid) butyl imidazolium salt

[0040] Dissolve 20g of 1,4-butyl sultone sultone in 150mL of ethyl acetate, slowly add 12g of N-methylimidazole dropwise, and heat under reflux at 40°C for 10h to obtain 1-(4-sulfonic acid)butyl The imidazolium salt was washed three times with ether and ethyl acetate, filtered with suction, and dried under vacuum. The measured yield was 60%.

[0041](2) Preparation of 1-(4-sulfonic acid) butylimidazole p-toluenesulfonate

[0042] Dissolve 1-(4-sulfonic acid) butylimidazolium salt in water, add p-toluenesulfonic acid in an equal amount, reflux at 90°C for 8 hours, remove water by rotary evaporation, wash with ether, separate layers, 40 After vacuum drying at ℃, the imidazolidinesulfonic acid p-toluenesulfonic acid salt ionic liquid catalyst is obtained.

[0043] (3) Preparation of diisopropyl maleate

[0044] Add 10g of maleic anhydride, 24g of isopropanol, 1g of 1-(4-sulfonic acid) butylimidazole p-tolue...

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Abstract

The invention discloses a method for preparing maleic acid isopropyl ester. The method comprises the following steps of: (1) preparing sulfonacid ionic liquid onium salt through sultone and nitrogen tertiary amine compounds; (2) dissolving the sulfonacid ionic liquid onium salt into water, slowly dropwise adding acid under ice bath so as to prepare a sulfonacid ionic liquid; and (3) carrying out condensation and reflux reaction on maleic anhydride, isopropanol, the sulfonacid ionic liquid and a water-carrying agent, separating a liquid, circularly catalyzing the sulfonacid ionic liquid at the lower layer, carrying out decompression distillation on an ester layer at the upper layer, then neutralizing with alkali, layering, and carrying out decompression distillation to obtain finished maleic acid isopropyl ester. The sulfonacid ionic liquid catalyst can be recycled and can absorb water, thus being beneficial to forwarding operation of the reaction, and realizing the recovery and recycling of excessive alcohol. The method is simple in procedures, pollution-free and non-corrosion, and has the advantages of being mild in conditions, environment-friendly and economic in benefits.

Description

[0001] technical field [0002] The invention relates to a method for preparing diisopropyl maleate, which belongs to the technical field of fine organic chemistry. Background technique [0003] Diisopropyl maleate, also known as diisopropyl maleate, referred to as DIPM, M is 200.2316, C 10 h 16 o 4 , with a density of 1.027g / cm 3 , with a boiling point of 225.5°C at 760mmHg, can be used as a plasticizer for organic solvents, polymer monomers and synthetic resins, as well as insecticides, fungicides, antirust additives, organic synthesis intermediates, and copolymers with other substances It can synthesize coatings, adhesives, anti-shrinkage finishing agents, etc. with various properties and uses. Due to the existence of double bonds, the diester is more active in nature and can react with various substances. Diisopropyl succinate can be obtained by hydrogenation. Due to its wide range of uses, the demand for diisopropyl maleate has been increasing at home and abroad in...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/60C07C67/08
CPCY02P20/584
Inventor 赵地顺葛京京翟建华刘美端李俊盼汪学良崔云张栓力
Owner HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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