A kind of styrene-isomonoolefin-styrene triblock copolymer and preparation method thereof

A technology of isomonoolefin and styrene, which is applied in the field of styrene-isomonoolefin-styrene triblock copolymer and its preparation, can solve the problems of high block efficiency, low content, and decreased block copolymerization efficiency, etc. To achieve the effect of improving efficiency

Active Publication Date: 2018-11-02
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The purpose of the present invention is to overcome the preparation method of styrene-isomonoolefin-styrene triblock copolymerization in the prior art, which easily leads to homopolymerization of styrene monomers and electrophilic aromatic substitution reactions between styrene molecules The defect of generating double or high-linked interpolymers, which leads to a decrease in the efficiency of block copolymerization, provides a benzene with low styrene homopolymer content and low styrene biphenyl copolymer content. Ethylene-isomonoolefin-styrene triblock copolymer and preparation method thereof

Method used

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  • A kind of styrene-isomonoolefin-styrene triblock copolymer and preparation method thereof
  • A kind of styrene-isomonoolefin-styrene triblock copolymer and preparation method thereof
  • A kind of styrene-isomonoolefin-styrene triblock copolymer and preparation method thereof

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preparation example Construction

[0022] The invention provides a kind of preparation method of styrene-isomonoolefin-styrene triblock copolymer, the method comprises:

[0023] (1) In the presence of an organic solvent and titanium tetrachloride, the isomonoolefin is subjected to the first cationic polymerization reaction to obtain a polymerization system containing polyisomonoolefin with reactive terminals;

[0024] (2) contacting the polymerization system with a solution containing styrene to carry out the second cationic polymerization reaction;

[0025] Wherein, the first cationic polymerization described in step (1) also includes introducing an initiator system, which contains at least one compound capable of providing carbocations and at least one activator,

[0026] The activator is selected from compounds shown in formula I-1 and compounds shown in formula I-2,

[0027]

[0028] In formula I-1 and formula I-2, R 1 -R 8 each independently -H, -X 1 , -NO 2 , and-CN,X 1 and x 2 each independen...

Embodiment 1

[0087] This example is used to illustrate the triblock copolymer of the present invention and its preparation method.

[0088] (1) Configuration of initiator solution: the concentration of tetrachloro-p-benzoquinone and p-dicumyl methyl ether configured in methylene chloride to obtain the concentration of 0.008mol / L and p-dicumyl methyl ether It is a 0.01mol / L solution and placed in a cold bath at -80°C for later use.

[0089]Under the protection of nitrogen, put the solution of isobutene (175mL n-hexane + 175mL dichloromethane + 0.58mol isobutene) in a cold bath at -80°C, add 50mL of the initiator solution prepared above, continue stirring for 20 minutes, and then add After 0.02 mol of titanium tetrachloride was polymerized at -80°C for 60 minutes, the measured conversion rate of isobutene is shown in Table 1.

[0090] (2) Add 100 mL of styrene solution (containing 20 mL of styrene (about 0.17 mol) + 44 mL of n-hexane + 44 mL of dichloromethane) pre-refrigerated at -80 ° C t...

Embodiment 2

[0100] This example is used to illustrate the triblock copolymer of the present invention and its preparation method.

[0101] (1) Configuration of initiator solution: configure 2,3-dichloro-5,6-dicyano-p-benzoquinone and p-dicumyl methyl ether in dichloromethane to obtain 2,3-dichloro-5,6 - a solution in which the concentration of dicyano-p-benzoquinone is 0.02mol / L and the concentration of p-dicumyl ether is 0.01mol / L, and placed in a cold bath at -50°C for subsequent use.

[0102] Under the protection of nitrogen, put the solution of isobutene (150mL n-hexane + 180mL dichloromethane + 0.58mol isobutene) in a cold bath at -50°C, add 50mL of the initiator solution prepared above, continue stirring for 20 minutes, and then add After 0.02 mol of titanium tetrachloride was polymerized at -50°C for 70 minutes, the measured conversion rate of isobutene is shown in Table 1.

[0103] (2) Add 100 mL of styrene solution (containing 20 mL of styrene (about 0.17 mol) + 40 mL of n-hexan...

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Abstract

The invention relates to a styrene-isomonoolefin-styrene triblock copolymer and a preparation method thereof. The method comprises the following steps: (1) in the presence of an organic solvent and titanium tetrachloride, carrying out first cationic polymerization reaction on isomonoolefin to obtain a polymeric system containing polyisomonoolefin with reaction activities at the tail end; and (2) contacting the polymeric system with a styrene-containing solution, and carrying out second cationic polymerization reaction, wherein the first cationic polymerization reaction in the step (1) also comprises the step of introducing an initiator system, and the initiator system contains at least one compound capable of providing carbonium ions and at least one activator. The method can effectively lower the generation of the styrene homopolymer and styrene bi or high copolymer, thereby effectively enhancing the block polymerization efficiency.

Description

technical field [0001] The invention relates to a styrene-isomonoolefin-styrene triblock copolymer and a preparation method thereof. Background technique [0002] The synthesis of thermoplastic elastomers generally involves the preparation of triblock copolymers with rubbery soft segments and plastic hard segments. The plastic hard segment is usually a vinyl aromatic compound (such as polystyrene), while the rubbery soft segment is usually polybutadiene or polyisoprene. The most important styrenic thermoplastic elastomer is polystyrene-butadiene-styrene triblock copolymer (SBS). The preparation of SBS by active anion technology has been widely used in industry, but the SBS produced by this technology also has many shortcomings: for example, polybutadiene in the soft segment structure contains double bonds with high unsaturation, resulting in SBS The heat resistance, weather resistance and aging resistance are poor. Although the performance of SBS can be improved and the t...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F293/00
Inventor 张雷邱迎昕周新钦龚惠勤张月红
Owner CHINA PETROLEUM & CHEM CORP
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