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Preparation method of mercaptopropionate series compounds

A technology of mercaptopropionate and compound, applied in the field of compound preparation, can solve the problems of low reaction yield, unfavorable large-scale industrial production, long reaction time and the like, and achieve the effects of simple synthesis route, low cost and simple operation

Active Publication Date: 2021-11-05
唐山金坤化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this method is that the reaction time is long and the reaction yield is low, which is not conducive to large-scale chemical industry production.

Method used

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  • Preparation method of mercaptopropionate series compounds
  • Preparation method of mercaptopropionate series compounds
  • Preparation method of mercaptopropionate series compounds

Examples

Experimental program
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Effect test

Embodiment 1

[0031] Example 1 Preparation of methyl mercaptopropionate Compound embodiment

[0032] (A) mass ratio of 1: 1.62: Preparation of sodium sulfite solids ratio 2.47, 10wt% aqueous ammonia solution and the feed ester, the feedstock ester mass of R-S-S-R of 33.7% by mass R-S-S-S-R accounted for 66.3%, wherein R is -CH 2 CH 2 COOCH 3 ; Aqueous ammonia and solid sodium sulfite solution was thoroughly mixed to obtain a liquid mixture after the ester starting material is placed with a stirrer, a thermometer, an autoclave, the mixture was added to a stirred solution of ester starting material, sealed, heated with stirring to 55 ℃ when -60 deg.] C, quickly into the autoclave to a hydrogen sulfide gas filling pressure and the pressure at 0.4Mpa, 30min after the reaction gas cooling, the liquid was allowed to stand in the kettle liquid separation to obtain an intermediate ester; (b) mass ratio of 1 : 1.62: the ratio of preparing sodium sulfite solids is 2.47, 10wt% aqueous ammonia solution and...

Embodiment 2

[0034] Preparation of ethyl 2-mercapto-compound of Example

[0035] (A) mass ratio of 1: 1.62: Preparation of sodium sulfite solids ratio 2.87, 10wt% aqueous ammonia solution and the feed ester, the feedstock ester mass of R-S-S-R of 60.2% by mass R-S-S-S-R accounted for 39.8%, wherein R is -CH 2 CH 2 Cooc 2 Hide 5 ; Aqueous ammonia and solid sodium sulfite solution was thoroughly mixed to obtain a liquid mixture after the ester starting material is placed with a stirrer, a thermometer, an autoclave, the mixture was added to a stirred solution of ester starting material, sealed, heated with stirring to 55 ℃ when -60 deg.] C, quickly into the autoclave to a hydrogen sulfide gas filling pressure and the pressure at 0.4Mpa, 30min after the reaction gas cooling, the liquid was allowed to stand in the kettle liquid separation to obtain an intermediate ester; (b) mass ratio of 1 : 1.62: the ratio of preparing sodium sulfite solids 2.87, 10wt% aqueous ammonia solution and step (a) of the...

Embodiment 3

[0037] Preparation of 3-mercaptopropionic acid ester compound in Example

[0038] (A) mass ratio of 1: 1.62: Preparation of sodium sulfite solids ratio is 3.67, 10wt% aqueous ammonia solution and the feed ester, the feedstock ester mass of R-S-S-R of 75.4% by mass R-S-S-S-R accounted for 24.6%, wherein R is -CH 2 CH 2 Cooc 4Hide 9 (-C 4 Hide 9 N-butyl); the resulting mixture was a solid sodium sulfite and aqueous ammonia solution was mixed well, the raw material ester was placed with a stirrer, a thermometer, an autoclave, the mixture was added to a stirred solution of ester starting material, sealed, when heated with stirring to 55 ℃ -60 ℃, rapidly introduced into the autoclave to a hydrogen sulfide gas filling pressure and the pressure at 0.4Mpa, after 30min the reaction gas cooling, the liquid was allowed to stand in the kettle liquid separation to obtain an intermediate ester; (b ) mass ratio of 1: 1.62: ratio of 3.67 prepared sodium sulfite solids, 10wt% aqueous ammonia solut...

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Abstract

The invention provides a preparation method of a mercaptopropionate series compound, which comprises the following steps of: (a) fully mixing a sodium sulfite solid and an ammonia water solution to obtain a mixed solution a, adding the mixed solution a into a stirred raw material ester which is R-S-S-R, R-S-S-S-R or a mixture thereof in any proportion (R is -CH2CH2COOR1 and R1 is alkyl), stirring and heating, after the temperature is raised to 40-80 DEG C, introducing hydrogen sulfide gas for pressurizing, keeping the pressure at 0-1 Mpa, and reacting for 20-40 minutes to obtain intermediate ester; and (b) fully mixing a sodium sulfite solid and an ammonia water solution to obtain a mixed solution b, adding the mixed solution b into the intermediate ester obtained in the step (a), continuing to stir and heat, introducing hydrogen sulfide gas for pressurizing after the temperature rises to 40-80 DEG C, keeping the pressure at 0-1 Mpa, reacting for 20-40 minutes to obtain a crude mercaptopropionate product, and purifying the crude mercaptopropionate product to obtain a mercaptopropionate product. The method is suitable for a high-pressure kettle or a pipeline type continuous reactor, and is simple to operate, low in cost, high in yield and suitable for industrial production.

Description

Technical field [0001] The present invention relates to a method for preparing mercaptopropionate series compound, belonging to the field of preparation of the compounds. Background technique [0002] Mercaptopropionate series of compounds are an important class of organic solvents and chemicals. For example, methyl mercaptopropionate is a good organic solvent, is prepared isothiazolin-ketone intermediate; mercapto propionate as a raw material to make perfume; butyl mercaptopropionate was used as an acrylic resin, a styrene , neoprene, styrene latex processing aid; isooctyl mercaptopropionate useful as plastics additives, which are very versatile. Currently, the method of preparing mercaptopropionic acid esters of mainly the following two compounds: [0003] ① In the basic guanidine functional group of the solid support is present, for mercaptopropionic acid ester compounds (CN 1185431A) synthesized by the addition reaction of hydrogen sulfide and acrylic acid esters. A disadvant...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C319/06C07C319/28C07C319/22C07C323/52
CPCC07C319/06C07C319/28C07C319/22C07C323/52
Inventor 袁沩明潘锦张玉华范明磊杨忠义张满中
Owner 唐山金坤化工有限公司