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Cationic polymerization method for vinyl monomer

A technology of cationic polymerization of vinyl monomers, applied in the field of cationic polymerization of vinyl monomers, can solve the problems of low polymerization degree of polymerization products, achieve the effect of increasing molecular weight, low price, and low dosage

Active Publication Date: 2012-12-12
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] In order to solve the problem in the prior art that it is necessary to use a complex co-initiator to initiate the cationic polymerization of vinyl monomers in an organic solvent containing a certain amount of water or in a complete aqueous phase, and the resulting polymerization product has a low degree of polymerization, the present invention proposes A method for initiating cationic polymerization of vinyl monomers in a mixed reaction medium containing an organic solvent and water or in a reaction medium entirely of water

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] At -50°C, add 40 mL of isobutylene (IB) / dichloromethane solution and 2 mL of an aqueous solution containing 20% ​​LiCl and 1% NaCl to the polymerization reactor, so that the water content in the reaction medium is 7%, and the concentration of IB in the reaction system It is 2.8mol / L. After mixing evenly, use water, o-cresol, dichloroisobutylaluminum and AlCl 3 Composition of the initiator system to initiate polymerization, the molar ratio of o-cresol to IB is 1.3×10 -2 : 1, the molar ratio of dichloroisobutylaluminum to IB is 1.0×10 -3 : 1, AlCl 3 The molar ratio to IB is 1.3×10 -2 : 1. After reacting for 10 min, NaOH / ethanol solution was added to terminate the reaction, and the mass fraction of NaOH was 5%.

[0047] The solvent, the initiator system and unreacted monomers are removed firstly, and the product is washed with lye and water several times in sequence, and finally dried in vacuum at 40°C until constant weight. Polymerization product yield is 69%, M w 5...

Embodiment 2

[0048] Example 2: (090317A7)

[0049] At -80°C, add 7 mL of IB and methyl chloride solution to the polymerization reactor, 30 mL of an aqueous solution containing 23% LiCl and 1.2% NaCl, so that the water content in the reaction medium is 85%, and the concentration of IB in the polymerization system is 0.6mol / L, after mixing evenly, use water, 1,1-dimethylbenzyl alcohol (abbreviation: cumyl alcohol), anisole and AlCl 3 The initiation system of composition initiates polymerization, makes cumyl alcohol and IB molar ratio be 5 * 10 -4 : 1, the molar ratio of anisole to IB is 3.1×10 -2 : 1, AlCl 3 The molar ratio to IB is 2.1×10 -2 : 1. Polymerization reaction 10min. Termination and post-processing methods are the same as in Example 1. Polymer yield was 66%, M w 1.4×10 5 ,M w / M n is 3.9.

Embodiment 3

[0050] Example 3: (090304A5)

[0051] At -80°C, add 30mL of a mixed solution of IB, ethyl chloride and methylene chloride (ethylene chloride / methylene chloride=0.1) to the polymerization reactor, and 15mL of an aqueous solution containing 23% of LiCl and 1.2% of NaCl, so that H in the reaction medium 2 The O content is 40%, and the IB concentration in the polymerization system is 2.0mol / L. 3 The initiation system of composition initiates polymerization, makes di-tert-butyl p-cumyl peroxide and IB molar ratio be 1 * 10 -4 : 1, the molar ratio of N,N-dimethylacetamide to IB is 6×10 -3 : 1, AlCl 3 The molar ratio to IB is 1.0×10 -2 : 1. Polymerization reaction 10min. Termination and post-processing methods are the same as in Example 1. Polymer yield was 31%, M w 4.7×10 4 .

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Abstract

The invention discloses a cationic polymerization method for vinyl monomer. In the method, a reaction medium, the vinyl monomer, an initiator, lewis acid and an additive are used, wherein the reaction medium is a mixed reaction medium comprising an organic solvent and water or completely water; the organic solvent is at least one selected from alkane, naphthenic hydrocarbon and halogenated hydrocarbon; the lewis acid is one or a mixture of substances which accord with a general formula of MXn or YRn-mXm; the additive is an oxygen atom and nitrogen atom-containing organic compound; the molar ratio of the lewis acid to the additive to the monomer is 1.0*10<-3> to 3.2*10<-2>:1.0*10<-3> to 3.0*10<-1>:1; and the materials are reacted at the temperature of between -100 and 50 DE C for 0.5 minute to 2 hours to form a polymerization product, namely polymer with molecular weight of 10<5>. The method can simplifies the process flow, saves the production cost, and has great significance and considerable market application value.

Description

technical field [0001] The invention relates to a method for preparing vinyl monomer homopolymer or copolymer through homopolymerization or copolymerization of vinyl monomer through carbocation process. In particular, a method for initiating cationic homopolymerization or copolymerization of vinyl monomers by using an initiating system in a reaction medium containing water mixed with an organic solvent or even in a reaction medium completely composed of water. Background technique [0002] As one of the main methods in ionic polymerization, cationic polymerization has been widely used in various polymerization fields, such as: synthetic rubber, oil additives, plastic modifiers, etc. In the cationic polymerization of vinyl monomers, the polymerized monomers are usually vinyl compounds or conjugated dienes with alkyl substitution, aryl substitution or electron-donating group substitution, such as: vinyl ether, isobutylene, benzene Ethylene and its derivatives, isoprene, and r...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F2/00C08F2/38
Inventor 吴一弦黄强
Owner BEIJING UNIV OF CHEM TECH
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