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Preparation method of high-content pentaerythritol tetra (3-mercaptopropionic acid) ester

A technology of pentaerythritol tetramer and mercaptopropionic acid, which is applied in the chemical industry, can solve the problems of increasing equipment complexity and low main content, and achieve the effects of improving selectivity and conversion rate, high main content, and reducing side reactions

Inactive Publication Date: 2020-03-10
SHANDONG EFIRM BIOCHEMISTRY & ENVIRONMENTAL PROTECTION CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation of pentaerythritol tetra-3-mercaptopropionate in the prior art has a low main content, and at the same time, it is necessary to add a water remover to remove water from the solvent in the reflux system, which increases the complexity of the equipment

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] A method for preparing high-content pentaerythritol tetrakis (3-mercaptopropionic acid) ester, comprising the following steps: the mass ratio of pentaerythritol, 3-mercaptopropionic acid, acylating agent and organic base catalyst is 1:3.9-4.3:4.5 -8: 0.4-2

[0023] (1) Reaction stage: add 1 mol of pentaerythritol, 4 mol of 3-mercaptopropionic acid, 7 mol of thionyl chloride, 0.4 mol of DMAP into the reactor, add 200 g of dichloroethane, heat up to 80°C, and react for 2 hours;

[0024] (2) Post-treatment: add sodium sulfite solution to the reaction solution and wash until pale pink, separate the liquid, wash the organic phase once with hydrochloric acid, adjust the pH to 2-3, separate the liquid, wash the organic phase once with water, and finally remove the solvent under negative pressure. get the target product. The reaction yield is 98%, the tetraester content of the main component is 97%, low odor, and the chroma is 4.1.

Embodiment 2

[0026] A preparation method of high-content pentaerythritol tetrakis (3-mercaptopropionic acid) ester, is characterized in that, comprises the following steps:

[0027] (1) Reaction stage: add 1mol pentaerythritol, 3.9mol 3-mercaptopropionic acid, 4.5mol phosphorus oxychloride, 2mol DMAP into the reactor, add 200g toluene, raise the temperature to 120°C, and carry out the reaction for 1.5h;

[0028] (2) Post-treatment: add sodium bicarbonate solution to the reaction solution and wash until pale pink, separate the liquid, wash the organic phase once with sulfuric acid, adjust the pH to 2-3, separate the liquid, wash the organic phase once with water, and finally remove it under negative pressure. solvent to obtain the target product. The reaction yield is 97%, the tetraester content of the main component is 96%, the odor is low, and the chroma is 4.3.

Embodiment 3

[0030] A preparation method of high-content pentaerythritol tetrakis (3-mercaptopropionic acid) ester, is characterized in that, comprises the following steps:

[0031] (1) Reaction stage: add 1 mol of pentaerythritol, 4.3 mol of 3-mercaptopropionic acid, 8 mol of phosphorus trichloride, 1 mol of DMAP into the reactor, add 200 g of chloroform, raise the temperature to 65°C, and carry out the reaction for 2.5 hours;

[0032] (2) Post-treatment: add sodium bicarbonate solution to the reaction solution and wash until pale pink, separate the liquid, wash the organic phase once with sulfuric acid, adjust the pH to 2-3, separate the liquid, wash the organic phase once with water, and finally remove it under negative pressure. solvent to obtain the target product. The reaction yield is 98%, the tetraester content of the main component is 94%, low odor, and the chroma is 5.3.

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Abstract

The invention belongs to the field of chemical industry, and particularly relates to a preparation method of high-content pentaerythritol tetra (3-mercaptopropionic acid) ester, and the method comprises the following steps: reacting pentaerythritol, mercaptopropionic acid and an acylating reagent as raw material and organic alkali as a catalyst in a certain solvent at a certain temperature, and finally carrying out alkali washing, acid washing, water washing and negative pressure solvent recovery to obtain the target product. The preparation method disclosed by the invention has the advantagesof high reaction rate, low product chromaticity, small smell, high main content and the like.

Description

technical field [0001] The invention belongs to the field of chemical industry, and in particular relates to a preparation method of high-content pentaerythritol tetrakis(3-mercaptopropionate). Background technique [0002] Pentaerythritol tetra(3-mercaptopropionate) ester, alias: pentaerythritol mercaptopropionate, pentaerythritol tetra-3-mercaptopropionate, tetrakis(3-mercaptopropionate) pentaerythritol ester, tetrakis(3-mercaptopropionate) pentaerythritol ester (PETMP), colorless liquid, insoluble in water, widely used in intermediates of organic synthesis, modifiers in polymerization reactions of UV coatings, inks, adhesives, etc., crosslinking agents, acidic ion exchange catalysts, low-temperature curing agents Wait. At present, the main production method is the catalytic esterification of pentaerythritol and mercaptopropionic acid, such as Japanese Patent No. 56-20530 and U.S. Patent US6201099. Most of the catalysts used are methanesulfonic acid and p-toluenesulfonic ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C319/12C07C323/52
CPCC07C319/12C07C323/52
Inventor 于龙张超梁万根崔卫华费潇瑶刘龙飞江德阳
Owner SHANDONG EFIRM BIOCHEMISTRY & ENVIRONMENTAL PROTECTION CO LTD
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