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A kind of preparation method of block copolymer and a kind of monovinylarene-isomonoolefin-monovinylarene block copolymer

A monovinylarene, self-monovinylarene technology, applied in the field of block copolymer preparation, can solve the problem of poor heat resistance, weather resistance and aging resistance, and the molecular weight of SIBS triblock copolymer needs to be further improved. Improve and other problems to achieve the effect of increasing the molecular weight

Active Publication Date: 2021-09-21
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The preparation of SBS by active anion technology has been widely used in industry, but the SBS produced 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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  • A kind of preparation method of block copolymer and a kind of monovinylarene-isomonoolefin-monovinylarene block copolymer
  • A kind of preparation method of block copolymer and a kind of monovinylarene-isomonoolefin-monovinylarene block copolymer
  • A kind of preparation method of block copolymer and a kind of monovinylarene-isomonoolefin-monovinylarene block copolymer

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preparation example Construction

[0023] 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.

[0024] The isomonoolefin is selected from compounds shown in formula I,

[0025]

[0026] 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.

[0027] 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.

[0028] 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 n-hexane, 126mL of monochloromethane and 50mL of isobutylene 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, 14.4mL of DMA solution and 3.5 mL of DtBp solution and continued to stir for 10 minutes to obtain an isobutene solution.

[0096] Preparation of styrene solution

[0097] Mix 20 mL of styrene, 48 mL of n-hexane, 32 mL of dichlorom...

Embodiment 2

[0118] The block copolymer was prepared by the same method as in Example 1, except that the DtBp solution was not used when preparing the styrene solution, thereby obtaining poly(styrene-isobutylene-styrene). After testing, the conversion rates of isobutylene and styrene are both 100%. It was observed that substantially no gel was formed during the polymerization.

[0119] The obtained poly(styrene-isobutylene-styrene) was analyzed by gel permeation chromatography, and its weight average molecular weight was determined to be 228,000, the molecular weight distribution index was 4.2, the weight average molecular weight of the high molecular weight component was 560,000, and the content was 38%.

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Abstract

The invention discloses a block copolymer and a preparation method thereof. The preparation method comprises first contacting isomonoolefin and each component in an initiator system in a diluent to obtain an intermediate solution containing polyisomonoolefin , the initiator system contains compounds that can provide carbocations, titanium tetrachloride, N,N-dimethylacetamide, and 2,6-dialkylpyridine, the duration of the first contact is 30-100 minutes, the intermediate solution is subjected to a second contact with the monovinylarene and optionally supplemented 2,6-dialkylpyridine to obtain a product solution containing the block copolymer, the duration of the second contact being 80-110 minute. By adopting the method of the invention to prepare the block copolymer, not only can the content of high molecular weight components in the prepared copolymer be significantly increased, so that the prepared block copolymer has a higher molecular weight; moreover, no gel phenomenon will occur in the preparation process.

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 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 perf...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F297/00C08F212/08C08F210/10C08F4/16
CPCC08F4/16C08F210/10C08F212/08C08F297/00C08F2500/01
Inventor 张雷邱迎昕周新钦龚惠勤张月红
Owner CHINA PETROLEUM & CHEM CORP
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