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Block copolymer preparation method and monovinyl aromatic hydrocarbon-isomonoolefin-monovinyl aromatic hydrocarbon block copolymer

A technology of monovinylarene and block copolymer, which is applied in the field of monovinylarene-isomonoolefin-monovinylarene block copolymer, can solve the problem of poor heat resistance, weather resistance and aging resistance, The molecular weight of SIBS triblock copolymer needs to be further improved to achieve the effect of narrow molecular weight distribution

Active Publication Date: 2019-04-30
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The preparation of SBS by active anion technology has been widely used in industry, but the SBS prepared by this technology also has many disadvantages: for example, polybutadiene in the soft segment structure contains double bonds with high unsaturation, which leads to SBS Poor heat resistance, weather resistance and aging resistance
[0005] However, the molecular weight of the SIBS triblock copolymer prepared by this method still needs to be further improved.

Method used

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  • Block copolymer preparation method and monovinyl aromatic hydrocarbon-isomonoolefin-monovinyl aromatic hydrocarbon block copolymer
  • Block copolymer preparation method and monovinyl aromatic hydrocarbon-isomonoolefin-monovinyl aromatic hydrocarbon block copolymer
  • Block copolymer preparation method and monovinyl aromatic hydrocarbon-isomonoolefin-monovinyl aromatic hydrocarbon block copolymer

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preparation example Construction

[0024] The invention provides a method for preparing a block copolymer, the method comprising step (1): under the condition of cationic polymerization reaction, first contacting isomonoolefin and each component in the initiator system in a diluent , to obtain an intermediate solution containing polyisomonoolefin.

[0025] The isomonoolefin is selected from compounds shown in formula I,

[0026]

[0027] In formula I, R 1 and R 2 Each is C 1 -C 5 straight or branched chain alkyl; or R 1 for hydrogen, R 2 for C 3 -C 5 branched chain alkyl.

[0028] In the present invention, C 1 -C 5 straight chain or branched chain alkyl including C 1 -C 5 straight-chain alkyl and C 3 -C 5 branched chain alkyl, specific examples of which may include, but are not limited to: methyl, ethyl, n-propyl, isopropyl, n-butyl, sec-butyl, isobutyl, tert-butyl, n-pentyl, iso Pentyl, tert-pentyl and neopentyl.

[0029] Specifically, the monoolefin may be selected from, but not limited to:...

Embodiment 1

[0092] (1) Preparation of initiator solution

[0093] Weigh 0.115g of p-dicumyl chloride (DCC) and dissolve in 20mL of dichloromethane to obtain a DCC solution, extract 0.2mL of N,N-dimethylacetamide (DMA) and dissolve in 20mL of dichloromethane to obtain a DMA solution, extract 0.2 mL of 2,6-di-tert-butylpyridine (DtBp) was dissolved in 7.5 mL of dichloromethane to obtain a DtBp solution, and the above solution was placed in a cold bath at -80°C for use.

[0094] (2) Preparation of isobutylene solution

[0095] Add 190mL of methylcyclohexane, 126mL of chloromethane and 50mL of isobutene into a 1000mL three-necked flask under nitrogen protection, place the three-necked flask in a cold bath at -80°C, stir for 20 minutes, then add 16mL of DCC solution and 14.4mL of DMA solution and 3.5mL DtBp solution, and continued stirring for 10 minutes to obtain an isobutylene solution.

[0096] Preparation of styrene solution

[0097] 20 mL of styrene, 48 mL of methylcyclohexane, 32 mL o...

Embodiment 2

[0103] Adopt the method identical with embodiment 1 to prepare block copolymer, difference is, in step (3), in the monomer solution, add 1.2mL titanium tetrachloride, and stir reaction at this temperature after 100 minutes (after detecting , the conversion rate of isobutylene is 100%), add the styrene solution prepared by step (2), continue to stir and react for 80 minutes (after testing, the conversion rate of styrene is 100%), then add 5g as terminator in the reaction system methanol, and continued stirring for 5 minutes to obtain poly(styrene-isobutylene-styrene). It was observed that substantially no gel was formed during the polymerization.

[0104] The obtained poly(styrene-isobutylene-styrene) was analyzed by gel permeation chromatography, and its weight average molecular weight was determined to be 103,000, the molecular weight distribution index was 1.74, the weight average molecular weight of the high molecular weight component was 284,000, and the content was 11.0%....

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Abstract

The invention discloses a block copolymer and a preparation method thereof. The preparation method comprises: carrying out first contact on an isomonoolefin and each component of an initiator system in a diluent to obtain a middle solution containing polyisomonoolefin, wherein the initiator system contains a compound capable of providing carbocations, titanium tetrachloride, N,N-dimethylacetamideand 2,6-dialkylpyridine, and the lasting time of the first contact is 40-100 min; and carrying out second contact on the middle solution, a monovinyl aromatic hydrocarbon and optionally supplemented 2,6-dialkylpyridine to obtain a product solution containing the block copolymer, wherein the lasting time of the second contact is 80-110 min. With the application of the method of the present invention to prepare the block copolymer, the content of the high molecular weight component in the prepared copolymer can be significantly increased, the prepared block copolymer has high molecular weight and exhibits narrow molecular weight distribution, and no gelation is generated during the preparation.

Description

technical field [0001] The invention relates to a preparation method of a block copolymer, and also relates to a monovinylarene-isomonoolefin-monovinylarene block copolymer. 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 styrene-based thermoplastic elastomer is styrene-butadiene-styrene triblock copolymer (SBS). The preparation of SBS by active anion technology has been widely used in industry, but the SBS prepared by this technology also has many disadvantages: for example, polybutadiene in the soft segment structure contains double bonds with high unsaturation, which leads to SBS The heat resistance, weather resistance and aging resistance are poor. Although the p...

Claims

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Application Information

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IPC IPC(8): C08F297/00C08F212/08C08F4/16
CPCC08F297/00C08F2500/01C08F2500/03C08F212/08C08F4/16
Inventor 张雷邱迎昕周新钦龚惠勤张月红
Owner CHINA PETROLEUM & CHEM CORP
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