Star block copolymer and preparation method thereof

A technology of block copolymers and compounds, applied in the field of star-shaped block copolymers, can solve the problems of high cost, poor heat resistance, weather resistance and aging resistance, complicated processes, etc., so as to improve the block efficiency, The effect of reducing the generation of styrene homopolymers and di- or high-copolymers, and the process is simple

Active Publication Date: 2016-10-19
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 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 Poor heat resistance, weather resistance and aging resistance
Although the performance of SBS can be improved and the thermal oxygen stability and service temperature of SBS can be improved by hydrogenation, but hydrogenation often requires noble metals as catalysts, and the process is complicated and costly.
In addition, hydrogenation of polybutadiene chain segments is easy to form polyethylene chain segments, which loses the original elasticity

Method used

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preparation example Construction

[0025] According to the first aspect of the present invention, the present invention provides a kind of preparation method of radial block copolymer, and this method comprises the following steps:

[0026] (1) In the presence of a diluent, the isomonoolefin is contacted with the initiator system to carry out a cationic polymerization reaction to obtain a polymerization system containing a polyisomonoolefin with reactive terminals;

[0027] (2) When the conversion rate of the isomonoolefin reaches more than 60%, the polymerization system is mixed with a solution containing styrene to carry out cationic polymerization;

[0028] Wherein, the initiator system contains at least one compound capable of providing carbocations, titanium tetrachloride and at least one activator,

[0029] The activator is selected from compounds shown in formula I-1 and compounds shown in formula I-2,

[0030]

[0031] In formula I-1 and formula I-2, R 1 ~R 8 each independently -H, -X 1 , -NO 2 ...

Embodiment 1

[0078](1) Configuration of the initiator solution: First, add 0.246 g of tetrachloro-p-benzoquinone, 0.147 g of tricumyl chloride and 5 mL of dichloromethane into a 10 mL volumetric flask, dissolve and place in a cold bath at -80°C for later use.

[0079] Add 175mL of n-hexane, 175mL of dichloromethane and 30mL of isobutylene into a 1000mL three-necked flask under the protection of nitrogen, place the three-necked flask in a cold bath at -80°C, stir for 20 minutes, add the initiator solution prepared above, and continue stirring After 30 minutes, 1.8 mL of titanium tetrachloride was added for polymerization. After 40 minutes of reaction, 20 mL of isobutene was added to continue the reaction for 20 minutes, and a 1.2 g polyisobutene sample was taken to terminate.

[0080] (2) Add 100mL of styrene solution (which contains 12mL styrene, 44mL n-hexane and 44mL methylene chloride) pre-refrigerated at -80°C to the flask of step (1) and continue the reaction for 30 minutes. After the...

Embodiment 2

[0087] (1) Configuration of initiator solution: first add 0.341 grams of 2,3-dichloro-5,6-dicyano-p-benzoquinone, 0.147 grams of tricumyl chloride and 5 mL of dichloromethane into a 10 mL volumetric flask, after dissolving Store in a cold bath at -80°C for later use.

[0088] Add 175mL of n-hexane, 175mL of dichloromethane and 30mL of isobutylene into a 1000mL three-necked flask under the protection of nitrogen, place the three-necked flask in a cold bath at -80°C, stir for 20 minutes, add the initiator solution prepared above, and continue stirring After 20 minutes, 1.8 mL of titanium tetrachloride was added for polymerization. After 40 minutes of reaction, 20 mL of isobutene was added to continue the reaction for 20 minutes, and a 1.2 g polyisobutene sample was taken to terminate.

[0089] (2) Cationic polymerization was carried out in the same manner as in step (2) of Example 1.

[0090] Pour the polymer solution obtained after termination into a beaker and inject an equa...

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Abstract

The present invention discloses a star block copolymer and a preparation method thereof. The method comprises that: (1) in the presence of a diluent, isomonoolefin contacts an initiator system, and a cationic polymerization reaction is performed to obtain the polymerization system of the poly isomonoolefin with the terminal having reaction activity; and (2) when the conversion rate of the isomonoolefin achieves more than 60%, the polymerization system and a styrene-containing solution are mixed, and a cationic polymerization reaction is performed, wherein the initiator system contains at least a compound capable of providing carbenium ion, titanium tetrachloride and at least an activator, and the activator is selected from a compound represented by a formula I-1 and a compound represented by a formula I-2. According to the present invention, with the method, in the case of assurance of the high molecular weights of each block, the generation of the styrene homopolymer and the di or hypercopolymer can be significantly reduced so as to effectively improve the block efficiency. The formulas I-1 and I-2 are defined in the specification.

Description

technical field [0001] The invention relates to a preparation method of a star-shaped block copolymer and a star-shaped block copolymer prepared by the method. 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 SB...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F297/00
Inventor 张雷邱迎昕周新钦龚惠勤张月红
Owner CHINA PETROLEUM & CHEM CORP
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