Method for preparing anti-vulcanization reversion agent 1,3-bis(citraconimidomethyl)benzene

A technology of citrafurimide methyl and anti-sulfurization reversion agent, which is applied in the direction of organic chemistry, can solve the problems of low equipment corrosion, environmental protection, and high yield, and achieve reduced corrosion, good practicability, and high yield. high effect

Active Publication Date: 2014-04-23
WUHAN JINGHE CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to overcome the raw material pollution that the raw material that 3-bis(citrafurimidomethyl)benzene adopts in the prior art is polluted greatly, the defect that is

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0016] Example 1

[0017] 1) Add 500g of itaconic acid, 450ml of dimethyl sulfoxide as a solvent, and 10g of disodium hydrogen phosphate as a catalyst into a 1000ml three-necked flask connected with a water separator, a condenser and a mechanical stirrer. After stirring and mixing, the temperature is rapidly raised to 180°C Insulation reaction for 1 to 2 hours to make itaconic acid into a clear and transparent solution, cyclization under the catalysis of disodium hydrogen phosphate to obtain a mixed solution containing 2-methylmaleic anhydride, remove the solvent and dehydrate to obtain 345 grams Liquid 2-methylmaleic anhydride.

[0018] The process of solvent removal and dehydration is as follows: use a water separator to roughly separate the water in the mixed solution containing 2-methylmaleic anhydride, then add 150ml of xylene to the three-necked bottle, and mix it with the rough water-separated mixed solution. Further water separation (due to the density of xylene is sm...

Example Embodiment

[0023] Example 2

[0024] 1) Add 450g of itaconic acid, 450ml of dimethyl sulfoxide as a solvent, and 5g of disodium hydrogen phosphate as a catalyst into a 1000ml three-necked flask connected with a water separator, a condenser and a mechanical stirrer. After stirring and mixing, quickly heat up to 175°C Insulation reaction for 1-2 hours to make itaconic acid into a clear and transparent solution, cyclization under the catalysis of disodium hydrogen phosphate to obtain a mixed solution containing 2-methylmaleic anhydride, remove the solvent and dehydrate to obtain 320 grams Liquid crude 2-methylmaleic anhydride.

[0025] The process of solvent removal and dehydration is as follows: use a water separator to roughly separate the water in the mixed solution containing 2-methylmaleic anhydride, then add 150ml of xylene to the three-necked bottle, and mix it with the rough water-separated mixed solution. Further water separation (due to the density of xylene is smaller than water...

Example Embodiment

[0030] Example 3

[0031] 1) Add 550g of itaconic acid, 600ml of dimethyl sulfoxide as a solvent, and 15g of disodium hydrogen phosphate as a catalyst into a 1000ml three-necked flask connected with a water separator, a condenser and a mechanical stirrer. After stirring and mixing, the temperature is rapidly raised to 190°C Insulate and react for 1-2 hours to make itaconic acid into a clear and transparent solution, and cyclize it under the catalysis of disodium hydrogen phosphate to obtain a mixed solution containing 2-methylmaleic anhydride, remove the solvent and dehydrate to obtain 400 grams Liquid crude 2-methylmaleic anhydride.

[0032] The process of removing the solvent and dehydrating is as follows: use a water separator to roughly separate the water in the mixed solution containing 2-methylmaleic anhydride, then add 200ml of xylene to the three-necked bottle, and mix it with the rough water-separated mixed solution. Further water separation (due to the density of xy...

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PUM

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Abstract

The invention discloses a method for preparing anti-vulcanization reversion agent 1,3-bis(citraconimidomethyl)benzene. The method comprises the following steps: mixing itaconic acid, dimethylsulfoxide and disodium hydrogen phosphate according to a ratio, raising the temperature to be 175-195 DEG C, keeping the temperature and reacting for 1-2 hours, removing a solvent, subsequently dehydrating so as to prepare liquid 2-methyl maleic anhydride, further mixing 2-methyl maleic anhydride, m-xylylenediamine, xylene and pyridine according to a ratio, performing reaction under reflux for 3-4 hours at 120 DEG C, distilling under reduced pressure to obtain a crude product, finally recrystallizing the crude product, cooling down, filtering and drying so as to obtain 1,3-bis(citraconimidomethyl)benzene. As no acetic anhydride is used, no acetic acid is generated in the process, so that corrosion on equipment and environmental pollution are greatly reduced; in addition, the product prepared by using the method is high in yield and good in purity, and no equipment needs to be additionally arranged, so that the method is high in practicability.

Description

technical field [0001] The invention relates to a preparation method of an anti-reversion agent, in particular to a preparation method of an anti-reversion agent 1,3-bis(citramidomethyl)benzene. Background technique [0002] Anti-reversion agent is a new type of functional rubber additive, which can keep the vulcanized network stable, and the performance of vulcanized rubber will not decrease when it is used under heat or dynamic conditions. Among them, the anti-reversion agent 1,3-bis(citraimidomethyl)benzene has the most significant effect, and its role is gradually being recognized by domestic tire companies. [0003] In the prior art, the method for producing the anti-reversion agent 1,3-bis(citrafurimidomethyl)benzene generally adopts itaconic acid and acetic anhydride in toluene solvent, and uses formamide as a catalyst to prepare 2 -Methylmaleic anhydride, and then use 2-methylmaleic anhydride to catalyze the synthesis of 1,3-bis(citrafurimide methyl)benzene, but thi...

Claims

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Application Information

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IPC IPC(8): C07D207/448C07D307/60
CPCC07D207/448
Inventor 王腊生严建国熊斌胡利峰
Owner WUHAN JINGHE CHEM
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