A kind of preparation method of high-concentration isooctyl thioglycolate

The technology of isooctyl thioglycolate and isooctyl chloroacetate is applied in the field of preparation of organic chemical raw material mercaptocarboxylate, can solve the problems of high pollution, cumbersome steps, high cost and the like, and achieves high conversion rate and comprehensive waste liquid. The effect of reduced volume and shorter reaction time

Inactive Publication Date: 2011-12-07
湖州市菱湖佳润化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method uses concentrated sulfuric acid as a catalyst, and the steps are cumberso

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0023] 1. Preparation of isooctyl chloroacetate

[0024] Mix 100g chloroacetic acid and 130g isooctyl ester, add 2g SO4 2- / TiO 2 / La 3+ Rare earth solid superacid catalyst, reacted at 70°C for 0.5h to generate 199g of isooctyl chloroacetate;

[0025] 2. Preparation of bunte salt

[0026] Sodium thiosulfate (Na 2 S 2 o 3 ·5H 2 (2) 264g, 190g of isopropanol, under stirring, gradually heated to reflux, keeping the temperature at 120°C, after reacting for 0.5h, bunte salt was prepared, recovered isopropanol through primary and secondary condensation, and cooled to 70°C~ 90°C, set aside. After testing, the recovery rate of isopropanol is 93%;

[0027] 3. Preparation of isooctyl thioglycolate

[0028] In the above reaction solution, add 1000ml of dilute hydrochloric acid with a mass concentration of 9.5% to 10.5%, stir and react under boiling for 0.8h, let the layers stand and cool to 30°C, separate the lower water layer, and the thioglycolic acid obtained in the upper la...

example 2

[0030] 1. Preparation of isooctyl chloroacetate

[0031] Mix 100g chloroacetic acid and 130g isooctyl ester, add 5g SO4 2- / TiO 2 / La 3+ Rare earth solid superacid catalyst, react at 90°C for 0.7h, and generate 203g of isooctyl chloroacetate;

[0032] 2. Preparation of bunte salt

[0033] Add sodium thiosulfate (Na 2 S 2 o 3 ·5H 2 (2) 308g, 190g of isopropanol, under stirring, gradually heated to reflux, kept at 160°C, reacted for 0.8h, prepared bunte salt, recovered isopropanol through primary and secondary condensation, cooled to 70°C~ 90°C, set aside. After testing, the recovery rate of isopropanol is 96%;

[0034] 3. Preparation of isooctyl thioglycolate

[0035] In the above reaction solution, add 1000ml of dilute hydrochloric acid with a mass concentration of 9.5% to 10.5%, stir and react under boiling for 1.1h, let the layers stand and cool to 30°C, separate the lower water layer, and the thioglycolic acid obtained in the upper layer is The octyl ester was wa...

example 3

[0037] 1. Preparation of isooctyl chloroacetate

[0038] Mix 100g chloroacetic acid and 150g isooctyl ester, add 5g SO4 2- / TiO 2 / La 3+ Rare earth solid superacid catalyst, react at 80°C for 0.6h to generate 200g of isooctyl chloroacetate;

[0039] 2. Preparation of bunte salt

[0040] Add sodium thiosulfate (Na 2 S 2 o 3 ·5H 2 (2) 322g, 190g of isopropanol, under stirring, gradually heated to reflux, kept at 140°C, reacted for 0.8h, prepared bunte salt, recovered isopropanol through primary and secondary condensation, and cooled to 70°C~ 90°C, set aside. After testing, the recovery rate of isopropanol is 92%;

[0041] 3. Preparation of isooctyl thioglycolate

[0042] In the above reaction solution, add 1000ml of dilute hydrochloric acid with a mass concentration of 9.5% to 10.5%, stir and react under boiling for 1h, let the layers stand and cool to 30°C, separate the lower water layer, and the isooctyl thioglycolate obtained in the upper layer The ester was washed...

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Abstract

The invention relates to a method for preparing high-concentration isooctyl thioglycolate with short reaction time, high conversion rate, low cost and little pollution, comprising esterification, salt formation, hydrolysis and reduction, and the specific steps are (1) in a weight ratio of (1.3 ~ 1.5): 1 isooctyl alcohol and chloroacetic acid solution, add 2% ~ 5% rare earth solid superacid catalyst by weight of chloroacetic acid, react at 70°C ~ 90°C for 0.5h ~ 0.7h, generate chloroacetic acid (2) Under the condition of normal pressure and 120°C to 160°C, add sodium thiosulfate to the above-mentioned isooctyl chloroacetate, and reflux the mercaptolation reaction in isopropanol solvent for 0.5h to 0.8h, Prepare bunte salt; by weight, the consumption ratio of isooctyl chloroacetate, sodium thiosulfate and isopropanol is 1: (1.33~1.61): 0.98; (3) add dilute sulfuric acid to the prepared bunte salt Hydrolyze and reduce for 0.8h to 1.1h, then wash with water and rectify to obtain high-concentration isooctyl thioglycolate.

Description

technical field [0001] The invention relates to a method for preparing organic chemical raw material mercaptocarboxylate, in particular to a method for preparing isooctyl thioglycolate. Background technique [0002] Isooctyl thioglycolate, also known as 2-ethylhexyl thioglycolate, is a colorless oily liquid with a boiling point of 125°C (16KPa) and a density (g / cm 3 ) is 0.969-0.973 (25°C), and the refractive index (20°C) is 14593-14598. Insoluble in water, soluble in ether, alcohol and other organic solvents, soluble in dilute lye; has an unpleasant smell; it is decomposed when boiled in acid and alkali. [0003] Isooctyl mercaptoacetate is an important class of fine chemicals. It is the main raw material for preparing heat stabilizers for polyvinyl chloride (PVC) plastic products. catalyst. With the rapid growth of the market demand for organotin heat stabilizers, the industrialization research of the important raw material (isooctyl thioglycolate) as its commercializat...

Claims

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Application Information

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IPC IPC(8): C07C323/52C07C319/02
Inventor 翟玉强
Owner 湖州市菱湖佳润化工有限公司
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