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New method for compounding maleic diacid single low-carbon alcohol ester

A technology of maleic acid monoester and maleic acid monoester, which is applied in the field of organic chemical synthesis, can solve the problems of controlling reaction time, separation and purification, difficulty in obtaining high-purity products, etc.

Inactive Publication Date: 2013-04-17
GUANGDONG UNIV OF PETROCHEMICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The traditional method uses maleic anhydride (maleic anhydride) and alcohol as raw materials to synthesize maleic acid monoester under reflux conditions. When the reaction time is too short, the raw material maleic anhydride is often incompletely reacted, and the reaction time is too long. The by-product maleic acid diester will be generated, which makes it very difficult to control the reaction time and subsequent separation and purification, so it is difficult to obtain a high-purity product

Method used

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  • New method for compounding maleic diacid single low-carbon alcohol ester

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Experimental program
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Embodiment 1

[0017] Dissolve 10.01g (0.102mol) of maleic anhydride in 50mL of anhydrous methanol, add 5.4g (0.51mol) of anhydrous sodium carbonate after the dissolution is complete, and stir at room temperature until the reaction ends when the solution becomes clear, then add 60mL of acetone was recrystallized under slow stirring at 0°C to produce a flocculent white solid, which was filtered and dried to obtain 14.6g of monomethyl maleate sodium salt as a white solid, and then 192mL of dilute hydrochloric acid with a concentration of 0.5mol / L was added and frozen After drying, dissolve with 3 times the volume of tetrahydrofuran, filter to remove sodium chloride, and distill the filtrate under reduced pressure to obtain 11.8 g of monomethyl maleate, a colorless oily liquid, with a purity of more than 99%.

Embodiment 2

[0019] Dissolve 5g (0.051mol) of maleic anhydride in 30mL of absolute ethanol, add 2.7g (0.0255mol) of anhydrous sodium carbonate after the dissolution is complete, stir at 40°C until the solution is clear, and react for 30 minutes End, then add 50mL of acetone and recrystallize under slow stirring at 0 degrees Celsius for half an hour to appear flocculent white solid, filter and dry to obtain 7.7g of white solid monoethyl maleate sodium salt, then add 0.75mol / L Dilute hydrochloric acid 62mL, after freeze-drying, dissolve with 4 times the volume of tetrahydrofuran, filter to remove sodium chloride, the filtrate is distilled under reduced pressure to 6.2g of colorless oily liquid monoethyl maleate, the purity is 99 %above.

Embodiment 3

[0021] Dissolve 5g (0.051mol) of maleic anhydride in 30mL of anhydrous propanol, add 2.7g (0.0255mol) of anhydrous sodium carbonate after the dissolution is complete, stir at 50°C until the solution is clear, then reflux the reaction At the end of 2.5 hours, add 50 mL of acetone and recrystallize under slow stirring at 0 degrees Celsius for half an hour. A flocculent white solid appears, filter and dry to obtain 8.2 g of white solid monopropyl maleate sodium salt, and then add the concentration of 1mol / L 46mL of dilute hydrochloric acid, after freeze-drying, after dissolving with 5 times the volume of tetrahydrofuran, filter to remove sodium chloride, the filtrate is distilled under reduced pressure to 6.5g of colorless oily liquid monopropyl maleate, the purity is More than 99%.

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Abstract

A new method for compounding maleic diacid single low-carbon alcohol ester comprises the following steps: mixing maleic diacid anhydride and low-carbon alcohol; adding alkali or alkalinous inorganic salt into the mixture to form a solution; at the room temperature to a temperature below 110 DEG C, agitating the solution until the solution is clear; filtering after reaction of 0-6 hr and obtaining maleic diacid single ester salt by renewedly crystallizing filtrate; and obtaining maleic diacid single low-carbon alcohol ester via acidification, refrigeration, drying, solid liquid separation and reduced pressure distillation, wherein the mole ratio of maleic diacid anhydride to low-carbon alcohol to alkali or alkalinous inorganic salt is 1:(5-15):(1.6-2). The method has the characteristics of very kindly process conditions, simple operation and high production purity and yield.

Description

technical field [0001] The invention relates to a new method for synthesizing maleic acid mono-lower carbon alcohol ester, which belongs to the field of organic chemical synthesis. Background technique [0002] Maleic acid mono-lower alcohol ester is an important raw material in the chemical industry. [0003] The traditional method uses maleic anhydride (maleic anhydride) and alcohol as raw materials to synthesize maleic acid monoester under reflux conditions. When the reaction time is too short, the raw material maleic anhydride is often incompletely reacted, and the reaction time is too long. The by-product maleic acid diester will be generated, which makes it very difficult to control the reaction time and subsequent separation and purification, so it is difficult to obtain a high-purity product. For this reason, the present invention aims at overcoming the above difficulties, with maleic anhydride (maleic anhydride), lower alcohols (methanol, ethanol, propanol, isoprop...

Claims

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Application Information

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IPC IPC(8): C07C69/60C07C67/08C07C67/30
Inventor 周如金马延龙邱松山聂丽君仇爱波
Owner GUANGDONG UNIV OF PETROCHEMICAL TECH