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A kind of chain transfer agent and its preparation method and application

A technology of chain transfer agent and reaction, applied in the field of applied chemistry, which can solve the problems of high risk factor of operation, high price of thiourea, poor stability, etc., and achieve the effect of reducing production cost, good technical effect, and good slump performance

Active Publication Date: 2020-07-03
CHINA UNIV OF MINING & TECH (BEIJING)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the most commonly used chain transfer agent in industry at home and abroad is β-mercaptopropionic acid. Patent CN1185432A introduces a kind of synthesis of β-mercaptopropionic acid through the addition reaction of hydrogen sulfide and acrylic acid in the presence of a solid carrier containing basic functional groups. , because the reaction needs to be carried out under high pressure conditions, the requirements for equipment are high, and at the same time, due to the need to feed highly toxic hydrogen sulfide gas for a long time, the operation risk factor is large, and it is difficult to realize industrialization
[0004] Patent CN100491346C introduces a method for synthesizing β-mercaptopropionic acid with sodium hydroxide, sodium hydrosulfide, sodium polysulfide, acrylonitrile, hydrochloric acid, and zinc powder as raw materials. The catalyst sodium polysulfide used in this invention has poor stability. It needs to be used and prepared immediately, and due to the unstable factors of sodium polysulfide, a large amount of by-product sulfide will be generated during the production process, and the solid waste pollution is relatively serious
[0005] Patent CN102229550A introduces a method for synthesizing β-mercaptopropionic acid with thiourea and acrylic acid as the main raw materials. In this method, the price of thiourea is relatively high, and there are various by-products such as sodium chloride, ammonia gas, barium sulfate, etc. in the reaction process. The high cost of recycling makes it difficult to market the product

Method used

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  • A kind of chain transfer agent and its preparation method and application
  • A kind of chain transfer agent and its preparation method and application
  • A kind of chain transfer agent and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] At room temperature, add 7.2g of sodium hydrosulfide and 20g of water into a 100ml beaker and mix evenly. Stir on a magnetic stirrer at 120r / min to dissolve sodium hydrogensulfide, and then add 9.14g of acrylic acid hydroxyl into the beaker dropwise through a peristaltic pump. Addition reaction of ethyl ester, the dropwise addition time is 10min. After the dropwise addition was completed, the stirring was continued on a magnetic stirrer for 2 h, and the chain transfer agent A was obtained by filtering.

Embodiment 2

[0043] At room temperature, add 7.2g of sodium hydrosulfide and 18.57g of water into a 100ml beaker and mix evenly, stir on a magnetic stirrer at 120r / min to dissolve the sodium hydrogensulfide, then add 12.19g of acrylic acid dropwise to the beaker through a peristaltic pump The addition reaction of hydroxyethyl ester was carried out, and the dropping time was 10 minutes. After the dropwise addition was completed, stir on a magnetic stirrer for 2 h, and filter to obtain chain transfer agent B.

Embodiment 3

[0045] At room temperature, add 7.2g of sodium hydrosulfide and 23.33g of water into a 100ml beaker and mix evenly, stir on a magnetic stirrer at 120r / min to dissolve the sodium hydrosulfide, then add 12.19g of acrylic acid dropwise to the beaker through a peristaltic pump The addition reaction of hydroxyethyl ester was carried out, and the dropping time was 10 minutes. After the dropwise addition was completed, stir on a magnetic stirrer for 2 h, and filter to obtain chain transfer agent C.

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PUM

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Abstract

The invention discloses a chain transfer agent. The chain transfer agent comprises a compound represented by the following general formula A HS-(CH2)2-R1-COO-R2-X; and in the formula A, R1 is absent or is selected from a C1-C10 alkylene group and a C6-C10 arylene group, R2 is selected from a C1-C10 alkylene group and a C6-C10 arylene group, and X is selected from an oxygen-containing group, wherein the C1-C10 alkylene group and the C6-C10 arylene group are optionally substituted with one or more substituent groups selected from a C1-C6 alkyl group, halogen, a cyano group and an amino group. The chain transfer agent provided by the invention has a good chain transfer property. The invention also provides a preparation method and an application of the chain transfer agent. The selected raw materials are cheap and are easy to obtain, so the production cost is reduced; the reaction is carried out under normal temperature conditions, so the method is simple to operate, and has a small danger coefficient; and the method meets modern industrial production requirements of green chemistry and green production.

Description

technical field [0001] The invention belongs to the field of applied chemistry, and in particular relates to a chain transfer agent and its preparation method and application. Background technique [0002] Free radical polymerization has the advantages of wide source of monomers, simple production process, various preparation methods, and low industrialization cost. It has become one of the most important reactions in the synthesis of polymers. However, the traditional free radical polymerization is a random process conforming to probability and statistics, and it is difficult to control the composition and structure of the synthesized polymer. Therefore, synthesizing a chain transfer agent that can adjust the relative molecular mass of the polymer and control the relative molecular mass distribution of the polymer has good application prospects and practical value. [0003] At present, the most commonly used chain transfer agent in industry at home and abroad is β-mercapto...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F2/38C08F283/06C08F220/06C07C323/52C07C319/04
Inventor 王栋民杨国武石佳佳黄自励
Owner CHINA UNIV OF MINING & TECH (BEIJING)