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Atom transfer radical polymerization method

A technology of atom transfer and free radical, which is applied in the field of organic synthesis, can solve the problem of low conversion rate and achieve the effect of mild polymerization reaction conditions

Active Publication Date: 2014-05-14
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The experimental results show that the number average molecular weight of polyacrylonitrile is 41342, and the molecular weight distribution is 1.13, but the conversion rate of monomeric acrylonitrile is only 9.56%, which is relatively low.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0055] 0.21g CuBr 2 , 0.14g of o-dipyridine, 0.14mL of ethyl α-bromoisobutyrate, 20mL of ethanol and 100mL of methyl methacrylate were placed in a 500mL four-neck round bottom flask, three of which were respectively inserted with a working electrode and an auxiliary electrode and the reference electrode, the fourth port is used to add the above materials; the air in the flask is purged with nitrogen gas and then sealed, and the four-necked round bottom flask is placed in an oil bath, heated to 60 ° C, and a voltage of 1.0V is applied. Polymerization was carried out for 6h to obtain polymethyl methacrylate.

[0056] The present invention uses the 1H-NMR method to identify the obtained polymer, indicating that the product obtained by the polymerization reaction is the target product.

[0057] The present invention calculates the conversion rate of the monomer and tests the number-average molecular weight and molecular weight distribution of the polymer according to the test met...

Embodiment 2

[0060] The atom transfer radical polymerization method of the present invention according to the technical solution described in Example 1, the difference lies in that the voltage of this example is 0.5V.

[0061] The present invention uses 1H-NMR to identify the obtained polymer, and the result shows that the polymer in the product is polymethyl methacrylate.

[0062] The present invention calculates the conversion rate of the monomer and tests the molecular weight and molecular weight distribution of the polymer according to the test method described in the above technical solution. The results are shown in Table 1. Table 1 is the experimental results of the polymerization reactions of Examples 1 to 13 of the present invention. .

[0063] It can be seen from Table 1 that the conversion rate of the monomer in Example 2 of the present invention is 4%, the number average molecular weight of the polymer is 8,000, and the molecular weight distribution is 1.13.

Embodiment 3

[0065] The atom transfer radical polymerization method of the present invention according to the technical solution described in Example 1, the difference lies in that the voltage of this example is 1.5V.

[0066] The present invention uses 1H-NMR to identify the obtained polymer, and the result shows that the polymer in the product is polymethyl methacrylate.

[0067] The present invention calculates the conversion rate of the monomer and tests the molecular weight and molecular weight distribution of the polymer according to the test method described in the above technical solution. The results are shown in Table 1. Table 1 is the experimental results of the polymerization reactions of Examples 1 to 13 of the present invention. .

[0068] It can be seen from Table 1 that the conversion rate of the monomer in Example 3 of the present invention is 29%, the number average molecular weight of the polymer is 11,600, and the molecular weight distribution is 1.16.

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Abstract

The invention provides an atom transfer radical polymerization method which comprises the following steps: mixing a monomer, an initiator, a ligand and a catalyst under an electrochemical initiation condition, and producing an atom transfer radical polymerization reaction to obtain a polymer, wherein the electrochemical initiation voltage is 0.5V-36V. According to the method, an oxidation-reduction process in a polymerization reaction system is controlled through an electrochemical method, and the polymerization reaction is initiated through controlling the electrochemical initiation voltage, so that the dynamics of the polymerization reaction and the molecular weight of the polymer are controlled and the monomer conversion rate in the polymerization reaction process is relatively high; and in the polymerization reaction, the usage amount of the catalyst is very low and the polymerization reaction condition is mild. Therefore, the method has a very good industrialization prospect.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, in particular to a method for atom transfer radical polymerization. Background technique [0002] Since Xerox discovered the nitroxide living radical polymerization method in 1993, the living radical polymerization method has entered a period of rapid development. In the following two decades, a variety of living radical polymerization methods were discovered one after another, and quickly became a common method for preparing polymers with structures such as block, graft, star, gradient, hyperbranched, and inorganic hybrids. At present, the more mature living radical polymerization methods mainly include iniferter living radical polymerization method, stable free radical polymerization method, reversible addition-fragmentation chain transfer living radical polymerization method and atom transfer radical polymerization method. Atom transfer radical polymerization (ATRP) has become a res...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F120/14C08F4/54C08F4/50C08F2/58C08F4/80C08F112/08C08F112/12C08F4/78C08F120/16
Inventor 张贺新白晨曦张学全张春雨张梦辉于琦周代全权毕吉福那丽华董博
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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