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Method for preparing pentaerythritol tetra (3-mercaptopropionic acid) ester

A pentaerythritol tetra, mercaptopropionic acid technology, applied in the preparation of mercaptan, chemical instruments and methods, preparation of organic compounds and other directions, can solve the problems of long synthesis route, equipment corrosion, low yield and the like

Pending Publication Date: 2021-03-26
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 reaction time of the transesterification method is long and the yield is low; the raw material conversion of the acid chloride method is high, but the organic solvent consumption is large, the equipment is corroded seriously, and the raw material acid chloride needs to be prepared and used immediately, the removal of by-product HC1 is troublesome, the synthesis route is long, and the yield is low and other defects; the esterification method is currently the most studied method, but it generally has problems such as high reaction temperature and large energy consumption.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] A method for preparing pentaerythritol tetrakis (3-mercaptopropionate), the concrete steps are as follows:

[0026] (1) Add raw materials 118.28g 3-mercaptopropionic acid, 34.04g pentaerythritol, 15.23g 4-dimethylaminopyridine (DMAP), 182.79g N,N'bicyclic to a 500ml four-necked flask equipped with a stirrer and a thermometer. Hexylcarbodiimide (DCC) and 156.32 g of dichloromethane;

[0027] (2) Turn on the heating to 40°C, dissolve the catalyst under stirring, turn off the heating after the pentaerythritol is completely dissolved, and start the reaction after it drops to room temperature. During the reaction, the temperature is controlled at room temperature, and the reaction time is 4-6h. The end point of the reaction is judged by the content of 3-mercaptopropionic acid in the liquid chromatography;

[0028] Concrete: Pentaerythritol will have the generation of by-product pentaerythritol tris (3-mercaptopropionate) ester in the process of carrying out esterification r...

Embodiment 2

[0032] A method for preparing pentaerythritol tetrakis (3-mercaptopropionate), the concrete steps are as follows:

[0033] (1) Add raw materials 118.28g 3-mercaptopropionic acid, 34.04g pentaerythritol, 15.23g 4-pyrrolidinylpyridine, 182.79g N,N'dicyclohexylcarbodiol to a 500ml four-necked flask equipped with a stirrer and a thermometer. imide (DCC) and 156.32 g dichloromethane;

[0034] (2) Turn on the heating to 40°C, dissolve the catalyst under stirring, turn off the heating after the pentaerythritol is completely dissolved, and start the reaction after it drops to room temperature. During the reaction, the temperature is controlled at room temperature, and the reaction time is 4-6h. The end point of the reaction is judged by the content of 3-mercaptopropionic acid in the liquid chromatography;

[0035] Concrete: Pentaerythritol will have the generation of by-product pentaerythritol tris (3-mercaptopropionate) ester in the process of carrying out esterification reaction wi...

Embodiment 3

[0039] A method for preparing pentaerythritol tetrakis (3-mercaptopropionate), the concrete steps are as follows:

[0040](1) Add raw materials 118.28g 3-mercaptopropionic acid, 34.04g pentaerythritol, 7.83g 4-dimethylaminopyridine (DMAP), 182.79g N,N'dicyclohexyl to a 500ml four-necked flask equipped with a stirrer and a thermometer. Carbodiimide (DCC) and 182.79 g of dichloromethane;

[0041] (2) Turn on the heating to 40°C, dissolve the catalyst under stirring, turn off the heating after the pentaerythritol is completely dissolved, and start the reaction after it drops to room temperature. During the reaction, the temperature is controlled at room temperature, and the reaction time is 4-6h. The end point of the reaction is judged by the content of 3-mercaptopropionic acid in the liquid chromatography;

[0042] Concrete: Pentaerythritol will have the generation of by-product pentaerythritol tris (3-mercaptopropionate) ester in the process of carrying out esterification reac...

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Abstract

The invention relates to the field of chemical synthesis, in particular to a method for preparing pentaerythritol tetra (3-mercaptopropionic acid) ester, the method comprises the following steps: using dichloromethane as a solvent, N, N '-dicyclohexylcarbodiimide (DCC) as a water-carrying agent and 4-dimethylaminopyridine (DMAP) as a catalyst, carrying out esterification reaction on pentaerythritol by using 3-mercaptopropionic acid to obtain pentaerythritol tetra (3-mercaptopropionic acid) ester; the preparation method is simple in process, easily available in raw materials, high in added value of products and suitable for industrial production.

Description

technical field [0001] The invention relates to the field of chemical synthesis, in particular to a method for preparing pentaerythritol tetrakis(3-mercaptopropionate). Background technique [0002] Pentaerythritol ester is an important neopentyl polyol ester compound. Pentaerythritol ester has good heat resistance, oxidation resistance and UV resistance, and is often used as an intermediate in organic synthesis, as a modifier in polymerization reactions such as UV coatings, inks, and adhesives, as a crosslinking agent, as an acidic ion exchange catalyst, and as a low temperature Curing agent and other fields. [0003] At present, the synthesis methods of pentaerythritol esters include esterification, acid chloride and transesterification. The reaction time of the transesterification method is long and the yield is low; the raw material conversion of the acid chloride method is high, but the organic solvent consumption is large, the equipment is corroded seriously, and the...

Claims

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Application Information

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IPC IPC(8): C07C319/12C07C319/28C07C323/52
CPCC07C319/12C07C319/28C07C323/52
Inventor 段秀智鲁超操江德阳梁万根崔卫华卞文
Owner SHANDONG EFIRM BIOCHEMISTRY & ENVIRONMENTAL PROTECTION CO LTD
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