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Method for preparing high-molecular polymer through anionic polymerization of alkyl acrylate polar monomers

A technology of alkyl acrylate and high molecular polymers, applied in the field of high molecular polymers, can solve the problems of difficult acquisition of side reaction inhibitors, insufficient industrial application value, increase of preparation steps, etc., to achieve the benefits of industrial production operations, The effect of overcoming potential difficulties and simple reaction system

Pending Publication Date: 2021-03-12
SHENYANG RES INST OF CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing related technologies are relatively complicated and cumbersome to operate, and the value of industrial application is still insufficient. The side reaction inhibitors are relatively difficult to obtain or need to increase the corresponding preparation steps, high cost, and / or have specific risks.

Method used

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  • Method for preparing high-molecular polymer through anionic polymerization of alkyl acrylate polar monomers

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Example 1: Methyl methacrylate homopolymer.

[0035] Under the temperature condition of 25°C, 1241g of toluene and 2.0g of 1,1-stilbene were added to the reactor. Add 1.85 mL of n-butyllithium hexane solution to initiate reaction for 1 h. Cool down to 12°C, add 7.8g tetrahydrofuran (46eq), and react for 1h. Add 13.9g of methyl methacrylate and react for 1h. After the reaction was completed, isopropanol was added to terminate the reaction. The product was precipitated with ethanol and washed, and dried under vacuum at 40°C for 12h. Analyze product with gel permeation chromatography (GPC), its number average molecular weight M n =5.8×10 3 , Molecular weight distribution width (polydispersity coefficient) d=1.44.

Embodiment 2

[0036] Embodiment 2: methyl methacrylate-n-butyl acrylate copolymer.

[0037] Under the temperature condition of 21°C, 1089g of toluene and 1.8g of 1,1-stilbene were added to the reactor. Add 1.76 mL of n-butyllithium hexane solution to initiate reaction for 1 h. Cool down to 8°C, add 7.2g tetrahydrofuran (43eq), and react for 1h. Add 9.0 g of methyl methacrylate and 5.4 g of n-butyl acrylate, and react for 1 h. After the reaction was completed, isopropanol was added to terminate the reaction. The product was precipitated with ethanol and washed, and dried under vacuum at 40°C for 12h. The product was analyzed by GPC, its M n =6.2×10 3 , d=1.41.

Embodiment 3

[0038] Example 3: Styrene-methyl methacrylate copolymer.

[0039] Under the temperature condition of 24°C, 1003g of toluene and 66.3g of styrene were added to the reactor. Add 1.70 mL of n-butyllithium hexane solution to initiate reaction for 1 h. Add 1.7g 1,1-stilbene and react for 0.5h. Cool down to 6°C, add 6.8g tetrahydrofuran (40eq), and react for 1h. Add 19.7g of methyl methacrylate and react for 1h. After the reaction was completed, isopropanol was added to terminate the reaction. The product was precipitated with ethanol and washed, and dried under vacuum at 40°C for 12h. The product was analyzed by GPC, its M n =3.7×10 4 , d=1.27.

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Abstract

The invention belongs to the field of high-molecular polymers, and particularly relates to a method for preparing a high-molecular polymer through anionic polymerization of alkyl acrylate polar monomers and application of the high-molecular polymer. In a system in which tetrahydrofuran is not used as a solvent or a main component of the solvent, the polymerization reaction temperature is close toor higher than 0 DEG C, under the assistance of a cap monomer, a certain amount of tetrahydrofuran is introduced to play a role in inhibiting carbonyl side reaction of alkyl acrylate polar monomers, and the molecular weight of the obtained product is in unimodal distribution. The side reaction inhibitor used in the method is easier to obtain, lower in cost, simpler and more convenient to operate and lower in risk. The product prepared by the method provided by the invention is used as a plastic and / or rubber blending modification compatibilizer, and the obtained blend (polymer alloy) has improved mechanical properties.

Description

technical field [0001] The invention belongs to the field of high-molecular polymers, in particular, the invention relates to a method and application for preparing high-molecular polymers by anion polymerization of alkyl acrylate polar monomers. Background technique [0002] Anionic polymerization is a kind of polymer preparation technology with great development prospects. The reaction mechanism is simple, and it has the characteristics of no termination and no chain transfer. Advantage. In the anionic polymerization system, the commonly used monomers are olefins and alkyl acrylates. The polymerization of olefins is relatively easy and industrial production has been achieved; while the polymerization of alkyl acrylates is a difficult point. Because the polar groups of such polar monomers are prone to carbonyl side reactions in the anionic polymerization system, resulting in broadening of the molecular weight distribution of the product, or premature termination of the act...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F120/14C08F220/14C08F220/18C08F212/08C08F236/10C08F8/04C08F2/38C08L53/02C08L69/00C08L25/14
CPCC08F120/14C08F220/14C08F212/08C08F8/04C08F2/38C08L53/025C08L2205/03C08L2205/08C08F220/1804C08F220/1802C08F236/10C08F220/1806C08L69/00C08L25/14C08F2500/03
Inventor 于胜楠朱思琪卢俊典刘晓杰李嵬刘歌陈二中燕晓宇鄂彦鹏张娇
Owner SHENYANG RES INST OF CHEM IND
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