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Method for preparing multi-sulfhydryl carboxylic ester

A technology of polymercaptocarboxylate and mercaptocarboxylic acid, which is applied in the field of preparation of polymercaptocarboxylate, can solve the problems of environmental pollution, difficult recovery of mercaptocarboxylic acid and catalyst, and achieves high purity, good economic value, and industrial wastewater. less effect

Inactive Publication Date: 2012-07-25
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method often produces a large amount of industrial wastewater containing mercaptocarboxylates and catalysts, and the mercaptocarboxylic acids and catalysts are difficult to recycle, which may pollute the environment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] In a 500mL three-neck flask equipped with a mechanical stirrer, a thermometer, a reflux condenser, and a water separator, add 34.8g (0.25mol) of pentaerythritol, 117.0g (1.1mol) of 3-mercaptopropionic acid, and 2.8 g of 70% aqueous methanesulfonic acid. g, 80g of cyclohexane, heated in an oil bath, reflux at 80-110°C to separate water, stop the reaction after reaching the theoretical water output, and lower the temperature. The reacted mixture was placed in a separatory funnel, allowed to stand for stratification, and the supernatant cyclohexane (reusable) was recovered; the crude product of the lower layer was extracted with 100 mL of absolute ethanol each time, extracted three times, and the extraction phases were combined. The raffinate was distilled off under reduced pressure to remove a small amount of residual ethanol to obtain 112.2 g of pentaerythritol tetrakis(3-mercaptopropionate) with a purity of 98.5%. The combined extract phases were distilled to recover th...

Embodiment 2

[0029] In the 500mL there-necked flask equipped with mechanical stirring, thermometer, reflux condenser and water separator, add pentaerythritol 34.8g (0.25mol), the mixture 11.6g of methanesulfonic acid and 3-mercaptopropionic acid that embodiment 1 reclaims, Add 108.3g (1.02mol) of 3-mercaptopropionic acid, 0.5g of 70% methanesulfonic acid aqueous solution, and 80g of cyclohexane, and obtain 110.0g of pentaerythritol tetrakis (3-mercaptopropionic acid) ester by the method in Example 1 , 98.5% purity.

Embodiment 3

[0031] In a 500mL three-necked flask equipped with a mechanical stirrer, a thermometer, a water separator and a reflux condenser, add 34.8g (0.25mol) of pentaerythritol, 101.3g (1.1mol) of thioglycolic acid, 4.0g of 70% methanesulfonic acid aqueous solution, and Hexane 80g, reflux at 80-110°C to separate water, stop the reaction after reaching the theoretical water yield, and lower the temperature. The reacted mixture was placed in a separatory funnel, allowed to stand for stratification, and the supernatant cyclohexane (reusable) was recovered; the crude product of the lower layer was extracted with 90 mL of absolute ethanol each time, extracted three times, and the extraction phases were combined. The raffinate was distilled off under reduced pressure to remove a small amount of residual ethanol to obtain 101.5 g of colorless and transparent pentaerythritol tetramercaptoacetate with a purity of 98%. The combined extract phases were distilled to recover the extractant ethanol...

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PUM

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Abstract

The invention discloses a method for preparing multi-sulfhydryl carboxylic ester. The method comprises the steps of carrying out an esterification reaction on sulfydryl carboxylic acid and polyatomic alcohol under catalysis of an acid catalyst to obtain a crude product of the multi-sulfhydryl carboxylic ester; meanwhile, distilling and bringing out water generated in the esterification reaction through adding an azeotropic water-carrying agent; extracting excessive raw material sulfydryl carboxylic acid and the catalyst in the multi-sulfhydryl carboxylic ester crude product generated through the esterification reaction by using an alcohol extracting agent, purifying to obtain the multi-sulfhydryl carboxylic ester; and recycling the residual sulfydryl carboxylic acid and catalyst after distilling and recovering the extracting agent. The multi-sulfhydryl carboxylic ester prepared by adopting the method disclosed by the invention is high in purity, good in color, weak in odour or odorless, simple in process, green and environment-friendly and has the advantages that the generated industrial effluent is little, the catalyst and the excessive sulfydryl carboxylic acid can be recycled and better economic value is achieved.

Description

technical field [0001] The present invention relates to a kind of preparation method of polymercapto carboxylate. The polymercaptocarboxylate involved in the present invention is the esterification reaction product of polyhydric alcohol and mercaptocarboxylic acid, is the raw material for preparing high-refractive optical devices and crosslinked network materials, and can be used as epoxy resin curing agent and photopolymerization reaction crosslinking agent Wait. Background technique [0002] The thiol-ene photopolymerization system is widely used in biomedicine, polymers, etc. Synthesis, nanolithography, manufacturing of high refractive optical devices, photocurable coatings and inks and other fields (see literature: C.E. Hoyle, etc. J. Poly. Sci., Part A: Poly. Chem. C. E. Hoyle, C. N. Bowman. Angew. Chem. Int. Ed. 2010, 49, 1540-1573). As an important class of mercaptans, polymercaptocarboxylates are often used not only in thiol-ene photopolymerization systems but als...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C319/12C07C319/28C07C323/52
CPCY02P20/582Y02P20/584
Inventor 卢礼灿刘宇蔡远利冯望成
Owner XIANGTAN UNIV
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