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Preparation method of wide molecular weight distribution powder syndiotactic polystyrene polymer

A wide molecular weight distribution, polystyrene technology, applied in the field of wide molecular weight distribution powder syndiotactic polystyrene polymer preparation, can solve the problems of poor processability and narrow molecular weight distribution

Active Publication Date: 2016-09-07
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The technical problem to be solved by the present invention is that the syndiotactic polystyrene polymer synthesized by previous literature reports has a narrow molecular weight distribution, which leads to the problem of poor processability, and provides a new preparation method for a syndiotactic polystyrene polymer with a wide molecular weight distribution

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  • Preparation method of wide molecular weight distribution powder syndiotactic polystyrene polymer
  • Preparation method of wide molecular weight distribution powder syndiotactic polystyrene polymer

Examples

Experimental program
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Effect test

Embodiment 1

[0021] In a dry 100ml three-necked bottle, N 2 Evacuate 3 times, add 0.1 mmol, A) IndTiCl 2 (OR 1 ) indenyl metal titanium compound, 0.1 mmol B) Cp*Ti(OPhOR 2 ) 3 50 ml of toluene was added, and the compound was dissolved by electromagnetic stirring at room temperature to obtain the metallocene titanium composition 1 with dual active centers.

[0022] On a 5-liter mechanically stirred tank, first bake at 90°C for 8 hours, then cool down, N 2 Evacuate 3 times, add 1188 grams of styrene monomer, at this time the temperature in the system is 35 ° C, inject triisobutylaluminum and methylalumoxane with a syringe, and add the double active center metallocene titanium prepared in Example 1 Composition 1, wherein the titanium molar concentration was 0.06 mmol titanium / L, and the alkylaluminoxane to titanium molar ratio (aluminum / titanium) was 600. After the catalyst is added, heat the jacket step by step, bring the temperature in the system to the polymerization temperature of 60...

Embodiment 2

[0024] In a dry 100ml three-necked bottle, N 2 Evacuate 3 times, add 0.16 mmol A=CpTi(OC 6 h 4 OCH 3 ) 3 and 0.04 mmol B=Cp*Ti(OC 6 h 4 OCH 3 ) 3 , mixing molar ratio A:B=4:1, adding 50 ml of n-hexane, electromagnetic stirring at room temperature to dissolve the compound, to obtain the double active center metallocene titanium composition 2.

[0025] On a 5-liter mechanically stirred tank, first bake at 90°C for 8 hours, then cool down, N 2 Evacuate 3 times, add 1188 grams of styrene monomer, at this time the temperature in the system is 35 ° C, inject triisobutylaluminum and methylalumoxane with a syringe, and add the double active center metallocene titanium prepared in Example 2 Composition 2, wherein the titanium molar concentration was 0.1 mmol titanium / L, and the alkylaluminoxane to titanium molar ratio (aluminum / titanium) was 400. After the catalyst is added, heat the jacket step by step, bring the temperature in the system to the polymerization temperature of ...

Embodiment 3

[0028] On a 5-liter mechanically stirred tank, first bake at 90°C for 8 hours, then cool down, N 2 Evacuate 3 times, add 1188 grams of styrene monomer, at this time the temperature in the system is 35 ° C, inject triisobutylaluminum and methylalumoxane with a syringe, and add the double active center metallocene titanium prepared in Example 2 Composition 2, wherein the titanium molar concentration was 0.05 mmol titanium / L, and the alkylaluminoxane to titanium molar ratio (aluminum / titanium) was 600. After the catalyst is added, heat the jacket step by step, make the temperature in the system reach the polymerization temperature of 55°C in about 40 minutes, stir and react at 300 rpm for 4 hours, stop the reaction with ethanol-hydrochloric acid solution, wash, and dry to obtain a powder solid , catalyst efficiency 129 kg polymer / (gram titanium), product syndiotactic polystyrene polymer syndiotacticity 98%, Mw=51×10 4 , molecular weight distribution Mw / Mn=48.

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Abstract

The invention relates to a preparation method of a syndiotactic polystyrene polymer with a wide molecular weight distribution, and aims to solve the problem that the syndiotactic polystyrene polymer synthesized by conventional methods has a narrow molecular weight distribution causing the bad processing ability of the polystyrene polymer. The preparation method comprises the following steps: adding metallocene titanium compositions with different active centers namely (a) an indenyl titanium compound IndTiCl2(OR1) and (b) a metallocene titanium compound Cp*Ti(OPhOR2)3, alkyl aluminoxane, and styrene into a reactor according to a certain ratio, evenly mixing, and carrying out reactions under stirring at a constant temperature of 50 to 80 DEG C for 3 to 10 hours in the protection of a gas which is inert to the reactants. The preparation method well solves the problem mentioned above, and is capable of being applied to the industrial production of syndiotactic polystyrene polymer with a wide molecular weight distribution.

Description

technical field [0001] The invention relates to a preparation method of a wide molecular weight distribution powder syndiotactic polystyrene polymer. Background technique [0002] The homogeneous catalytic system composed of titanocene compound and cocatalyst methylaluminoxane (MAO) or borofluorine compound can be used for syndiotactic polymerization of styrene to obtain syndiotactic polymer with a syndiotactic degree of more than 96%. The melting point of the polymer is as high as 270°C, the crystallization speed is fast, the chemical resistance is good, the heat resistance is good, the molecular weight distribution is narrow, the dimensional stability is good, and it has excellent electrical properties. Its comprehensive properties can be compared with engineering plastics. The advent of syndiotactic polystyrene (SPS) has aroused people's research on its catalytic system, especially the metallocene compound as the main catalyst. Documents US5252693 and EP210615 report the...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F112/08C08F4/6592
Inventor 沈志刚赵微微
Owner CHINA PETROLEUM & CHEM CORP