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Method for preparing phenylethylene copolymer

A kind of technology of styrene copolymer and styrene, applied in the field of preparing styrene copolymer

Inactive Publication Date: 2004-06-30
INST OF CHEM CHINESE ACAD OF SCI +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0012] Shigetaka Shimada et al [Macromolecules, 32, 8234 (1999)] used living free radical polymerization to prepare propylene and styrene copolymer; T.C.Chung [Journal of The American Chemical Society, 123 (21), 4871 (2001)] etc. Preparation of copolymers of propylene and styrene, only copolymers containing random polystyrene segments can be obtained by this method

Method used

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  • Method for preparing phenylethylene copolymer
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Experimental program
Comparison scheme
Effect test

Embodiment l

[0032] 1) All operations are carried out under anhydrous and oxygen-free conditions, and all solvents are dehydrated and deoxidized.

[0033] A, monomer: ethylene, styrene, 4 (1-butenyl) styrene;

[0034] B. Catalyst I: Et(Ind) 2 ZrCl 2 ; Catalyst II: CpTiCl 3 ; Promoter: MAO;

[0035] 2) Replace a 250mL three-neck flask equipped with a stirrer with nitrogen three times, then pass through ethylene, add 100mL of toluene, heat up to 50°C, add 0.1 g of 4(1-butenyl)styrene, and add MAO under stirring [(Al / Zr)=2000:1 (molar ratio)], after stirring for 2 minutes, add 2 mg of catalyst I: Et(Ind) 2 ZrCl 2 After reacting for 30 minutes, the reaction solution was poured into 10% (volume ratio) hydrochloric acid ethanol solution to terminate the reaction, washed with ethanol and water, and vacuum-dried to obtain a copolymer of ethylene and 4 (1-butenyl) styrene;

[0036] 3) Put 10 grams of the polymer obtained in step 2 into a 100 mL two-neck bottle, replace it with nitrogen three ...

Embodiment 2

[0038] 1) All operations are carried out under anhydrous and oxygen-free conditions, and all solvents are dehydrated and deoxidized.

[0039] A, monomer: propylene, styrene, 4 (1-butenyl) styrene;

[0040] B. Catalyst I: Me 2 Si(Ind) 2 ZrCl 2 ; Catalyst II: CpTiCl 3 ; Promoter: MAO;

[0041] 2) Replace a 250mL three-neck flask equipped with a stirrer with nitrogen three times, then pass through propylene, add 100mL toluene, heat up to 50°C, add 0.1 g of 4(1-butenyl)styrene, and add MAO under stirring [(Al / Zr)=2000:1 (molar ratio)], after stirring for 2 minutes, add 2 mg catalyst I: Me 2 Si(Ind) 2 ZrCl 2 After reacting for 30 minutes, the reaction solution was poured into 10% (volume ratio) hydrochloric acid ethanol solution to terminate the reaction, washed with ethanol and water, and vacuum-dried to obtain a copolymer of propylene and 4 (1-butenyl) styrene;

[0042] 3) Put 5 grams of the polymer obtained in step 2 into a 100 mL two-neck bottle, replace it with nitroge...

Embodiment 3

[0044] 1) All operations are carried out under anhydrous and oxygen-free conditions, and all solvents are dehydrated and deoxidized.

[0045] A. Monomer: 1-butene, 4(1-butenyl)styrene, styrene, 4(1-butenyl)styrene

[0046] B. Catalyst I: Cp * Ti(OBz) 3 ; Catalyst II: CpTiCl 3 ; Promoter: MAO;

[0047] 2) A 250mL three-neck flask equipped with a stirrer was replaced with nitrogen three times, then 1-butene was introduced, 100mL toluene was added, the temperature was raised to 50°C, 0.3 g of 4(1-butenyl)styrene was added, and stirred Add MAO[(Al / Ti)=2000:1 (molar ratio)], after stirring for 2 minutes, add 2mg catalyst I:Cp * Ti(OBz) 3 , after reacting for 30 minutes, the reaction solution was washed into 10% (volume ratio) hydrochloric acid ethanol solution to terminate the reaction, washed with ethanol and water, and dried in vacuum to obtain 1-butene and 4(1-butenyl)styrene copolymerization thing;

[0048] 3) Put 8 grams of the polymer obtained in step 2 into a 100 mL t...

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Abstract

The method for preparing styrene copolymker uses 4(1-alkenyl) styrene as important raw material and adopts the following steps: making said raw material and alpha-olefines, such as ethane, propene and 1-butylene, etc. or conjugated diolefines, such as 1,3-butadiene and isoprene, etc. implement copolymerization to obtain the copolymer which has the main chains of poly-alpha-olefines, such as polyethylene, polypropylene and poly-1-butylene, etc. or polyconjugated diolefines, such as poly-1,3-butadiene and polyisoprene, etc. and whose side group or end group contains styrene group; then making the obtained copolymer and styrene implement copolymerization so as to conveniently obtain the graft copolymer or block copolymer of alpha-olefines, such as ethane, propene and 1-butylene, etc. or conjugated diolefines, such as 1,3-butadiene and isoprene, etc. and styrene.

Description

technical field [0001] The present invention relates to a method for preparing styrene copolymers. Background technique [0002] Due to chemical structural reasons, it is difficult to achieve copolymerization of styrene and other olefins, and there are very few related reports. Even if copolymers of styrene and other olefins can be prepared, the content of styrene segments in the copolymer is very small. The stereo configuration of the styrene segment and other olefin segments cannot be changed conveniently, or only copolymers composed of random polystyrene and other olefin segments can be prepared. [0003] In literature reports, there are several methods for synthesizing styrene copolymers: [0004] The first method is to directly copolymerize two monomers with a metallocene catalyst or a Ziegler-Natta catalyst. Styrene and ethylene copolymerization, once reported catalytic system such as: [0005] TiCl 3 / MAO [Macromolecules, 24, 5476 (1991)]; CpTiCl 3 / MAO,Ti(OR) 4...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F212/08
Inventor 李泽胡友良洪瀚马志柯毓才丁瑞东科尔文・霍华德
Owner INST OF CHEM CHINESE ACAD OF SCI