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Synthetic process of isooctyl thioglycolate

A kind of technology of isooctyl thioglycolate, isooctyl acetate

Inactive Publication Date: 2018-03-30
杭州更蓝生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The current synthesis routes of TGB all have problems such as high cost and serious environmental pollution, so it is of great significance to study the synthesis process of TGB with low economic cost and environmental friendliness.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Catalyst preparation:

[0025] 1. Take a certain amount of carbon nanotubes with an outer diameter of 2nm, add HNO with a mass fraction of 35% 3 solution and 20ml mass fraction of 15% H 2 o 2 The solution is heated and refluxed at 100° C. for 2 to 3 hours, taken out, cooled to room temperature, washed, filtered, and dried by conventional methods to obtain surface-modified carbon nanotubes;

[0026] II. A certain amount of TiCl 4 and cetyltrimethylammonium bromide, respectively dissolved in 15-50ml of absolute ethanol, mixed and stirred for 0.5h, and then added with a concentration of 0.95mol / L H 2 SO 4 Mix the solution with 2.05mol / L HCl, and finally add 50mg of the surface-modified carbon nanotubes obtained by the above I, stir evenly at 35°C, heat at 110°C for 4h, cool to room temperature and wash by conventional methods , suction filtration, drying, and roasting, the SO with double-pore structure was obtained. 4 2- / TiO 2 @CNTS superacid mesoporous materials....

Embodiment 2

[0028] Catalyst preparation:

[0029] 1. Take a certain amount of carbon nanotubes with an outer diameter of 5nm, and add HNO with a mass fraction of 30% 3 solution and 30ml mass fraction of 15% H 2 o 2 The solution was heated to reflux at 110° C. for 3 hours, taken out, cooled to room temperature, washed by conventional methods, suction filtered, and dried to obtain surface-modified carbon nanotubes;

[0030] II. A certain amount of TiCl 4 and hexadecyltrimethylammonium bromide, respectively dissolved in 35ml of absolute ethanol, mixed and stirred for 1.5h, and then added with a concentration of 1.05mol / L H 2 SO 4Mix the solution with 1.95mol / L HCl, finally add 60mg of the surface-modified carbon nanotubes obtained by the above I, stir evenly at 35-40°C, heat at 115°C for 4h, cool to room temperature and pass through a conventional Method After washing, suction filtration, drying, and roasting, SO with a double-pore structure is obtained. 4 2- / TiO 2 @CNTS superacid m...

Embodiment 3

[0032] (1) The aqueous solution of chloroacetic acid and sodium thiosulfate are reacted at a temperature of 60°C in a molar ratio of 1:1.1 in a continuous and uniform mixing manner;

[0033] (2) add dilute acid in the reaction solution to acidify to a pH value of 3, the concentration of thioglycolic acid in the acidified solution after acidification is 6wt%, adopt isooctyl alcohol to carry out multi-stage continuous extraction, and the extract after extraction contains thioglycolic acid≥ 10wt%;

[0034] (3) Add a certain amount of anhydrous sodium sulfate in the extract, then add 0.8wt% SO prepared in Example 1 4 2- / TiO 2 @CNTS super acid, esterification reaction at a temperature of 30°C for 3 to 5 hours, the esterification rate ≥ 99.9%, and then continuous flash distillation at a temperature of 210°C for 1.5 minutes, to obtain a product with a purity of ≥99.5wt% and a chroma of < 5 isooctyl thioglycolate products.

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Abstract

The invention relates to a synthetic process of isooctyl thioglycolate. A multistage continuous extraction process and a continuous esterification process are used, and isooctyl alcohol is used as a raw material for esterification reaction and an extraction agent, so that the yield of a product is improved. A SO4<2-> / TiO2@CNTS superacid mesoporous material with a dual-pore structure is used as anesterification catalyst in the esterification reaction, and shows better catalytic activity and good performance of reuse to the esterification reaction of mercaptoacetic acid and the isooctyl alcoholat lower temperature.

Description

technical field [0001] The invention relates to the field of organic chemical synthesis, in particular to a synthesis process of isooctyl thioglycolate. Background technique [0002] Isooctyl Mercaptoacetate (TGB), also known as isooctyl thioglycolate, is an important fine chemical product. Molecular formula: HSCH2COOC 8 h 17 , relative molecular weight: 204.33, boiling point: 125°C (1.6KPa), density (g / cm,) 0.969-0.97325°C), refractive index (20°C) 1.459-1.4595. Due to the existence of -SH, its chemical properties are relatively active, but its physical properties are relatively stable. Appearance is colorless, transparent and easy to flow oily liquid, 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] As a fine chemical product, isooctyl thioglycolate is widely used in the synthesis and preparation of pesticides, medicines, and organic interm...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C319/02C07C319/12C07C319/28C07C323/52B01J27/053B01J35/10B01J37/10
CPCC07C319/02C07C319/12C07C319/28B01J27/053B01J37/0009B01J37/10B01J35/615B01J35/617B01J35/647B01J35/69C07C323/52
Inventor 董秋月
Owner 杭州更蓝生物科技有限公司
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