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Method for preparing 3-mercapto-propionate

A technology of mercaptopropionate and water-carrying agent, which is applied in the production field of 3-mercaptopropionate, can solve the problems of difficult industrialization, high equipment requirements, and large industrial wastewater discharge, and achieve high raw material utilization rate Effect

Inactive Publication Date: 2015-11-25
SHANXI QIYOU BUILDING MATERIALS TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] 3-mercaptopropionate has been widely used as a raw material for mercapto monomers in the production of high-performance epoxy resin curing agents and polyurethane high-refractive index optical materials. However, the conventional method for synthesizing 3-mercaptopropionate requires It is carried out in an autoclave, which has high requirements for equipment, and there is a certain danger in feeding gas under high pressure conditions, and the operation is complicated, and the industrialization is difficult. In addition, the traditional production process of 3-mercaptopropionate compounds exists. Defects such as a lot of industrial wastewater, catalysts and excess raw materials that cannot be reused
[0005] In conclusion, the current methods for producing 3-mercaptopropionate are complicated in process, large in discharge of industrial wastewater, and low in yield.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] A preparation method of 3-mercaptopropionate includes the following steps:

[0027] a) Add 700kg of 3-mercaptopropionic acid, 17.4kg of p-toluenesulfonic acid catalyst, and then add 480kg of toluene to a 3000L enamel reactor equipped with a stirrer, reflux cooling water separator, and thermometer. After the dissolution is complete, 211kg of alcohol compound CH 3 OH was added to the reaction solution, heated, and refluxed at 110°C. The water produced during the reaction was continuously drained out of the system. After no more water came out, the reaction was stopped, the temperature was lowered, and the temperature was cooled to room temperature;

[0028] b) After the reaction is over, after cooling to room temperature, 400kg of toluene is added to the reaction solution for dilution to obtain a crude product;

[0029] c) Place the crude reactant in a 3000L enamel kettle and wash it with saturated sodium bicarbonate solution for three times. The amount of saturated sodium bicar...

Embodiment 2

[0033] A preparation method of 3-mercaptopropionate includes the following steps:

[0034] a) Add 700kg of 3-mercaptopropionic acid, 15kg of p-toluenesulfonic acid catalyst, and then add 480kg of toluene to a 3000L enamel reactor equipped with a stirrer, reflux cooling water separator and thermometer. Dissolve the acid catalyst and the catalyst. After completion, 204kg of alcohol compound C 6 H 14 O 3 Add to the reaction solution, heat, and reflux at 110°C. During the reaction, the water produced is continuously drained out of the system. After no more water comes out, stop the reaction, lower the temperature, and cool to room temperature;

[0035] b) After the reaction is over, after cooling to room temperature, 400kg of toluene is added to the reaction solution for dilution to obtain a crude product;

[0036] c) Place the crude reactant in a 3000L enamel kettle and wash it with saturated sodium bicarbonate solution for three times. The amount of saturated sodium bicarbonate solutio...

Embodiment 3

[0040] A preparation method of 3-mercaptopropionate includes the following steps:

[0041] a) Add 700kg of 3-mercaptopropionic acid, 17.4kg of p-toluenesulfonic acid catalyst, and then add 300kg of toluene to a 3000L enamel reactor equipped with a stirrer, reflux cooling water separator, and thermometer. After the dissolution is complete, 224kg of alcohol compound C 5 H 12 O 4 Add to the reaction solution, heat, and reflux at 110°C. During the reaction, the water produced is continuously drained out of the system. After no more water comes out, stop the reaction, lower the temperature, and cool to room temperature;

[0042] b) After the reaction is over, after cooling to room temperature, 400kg of toluene is added to the reaction solution for dilution to obtain a crude product;

[0043] c) Place the crude reactant in a 3000L enamel kettle and wash it with saturated sodium bicarbonate solution for three times. The amount of saturated sodium bicarbonate solution is 600L each time. Coll...

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Abstract

A method for preparing 3-mercapto-propionate is as below: subjecting a main raw material of 3-mercaptopropionic acid and an alcohol compound to a heating esterification reaction in the presence of an acidic catalyst to prepare a 3-mercaptopropionic acid ester compound crude product; and then extracting and purifying the target product by using the differences in solubility of 3-mercaptopropionate and 3-mercaptopropionic acid residue and catalyst to choose the appropriate solvent. Compared with the prior art, the invention has the beneficial effects that the preparation process of 3-mercaptopropionic ester avoids the defects of dangerous operation of hydrogen sulfide introduction under high pressure and difficult treatment of wastewater in the traditional production process of 3-mercaptopropionate. The method provided by the invention is a green chemical synthesis method, which has no pollution and high raw material utilization rate.

Description

Technical field [0001] The invention relates to a chemical raw material used in the production of high-performance epoxy resin curing agents and polyurethane high-refractive-index optical materials, and more specifically, a production method of 3-mercaptopropionate. Background technique [0002] 3-mercaptopropionate as a kind of mercapto-based monomer raw material has been widely used in the production of high-performance epoxy resin curing agent and polyurethane high refractive index optical materials, etc., but the conventional method of synthesizing 3-mercaptopropionate requires the reaction It is carried out in an autoclave, which requires high equipment, and the gas is passed under high pressure, which is dangerous, and the operation is complicated, and the industrialization is difficult. In addition, there are traditional processes for producing 3-mercaptopropionate compounds. There are many defects in industrial waste water, catalysts and excessive raw materials cannot be ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C319/12C07C323/52C07C319/28
Inventor 刘秀君吴林茂孙培霞
Owner SHANXI QIYOU BUILDING MATERIALS TECH CO LTD
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