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Method for catalyzing water phase polymerization by metallocene catalyst

A metallocene catalyst and water-phase polymerization technology, which is applied in the field of metallocene catalyst-catalyzed water-phase polymerization, can solve the problems of limited use of metallocene catalysts, difficult control, harsh reaction conditions, etc.

Inactive Publication Date: 2007-07-11
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In this way, the use of metallocene catalysts is greatly restricted, the reaction conditions are harsh, difficult to control, and the production cost is also increased.

Method used

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  • Method for catalyzing water phase polymerization by metallocene catalyst
  • Method for catalyzing water phase polymerization by metallocene catalyst
  • Method for catalyzing water phase polymerization by metallocene catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] metallocene CpTiCl 3 As a catalyst, it catalyzes the polymerization of MMA in the aqueous phase system

[0029] The entire polymerization operation and reaction process are carried out under the protection of an inert gas, and the metallocene catalyst CpTiCl is sequentially added to the reactor 3 , polymerized monomer MMA 1g, stirred for 1 hour, added the aqueous solution of sodium dodecylsulfonate (5.77 × 10 -3 g SDS / 10ml H 2 0), continue stirring for 1 hour, add MMA 1g. Put it into the set temperature for reaction, after polymerizing for a certain period of time, quench with 20ml of 10% ethanol hydrochloric acid solution to terminate the polymerization, add excess ethanol to precipitate the polymer, and immediately produce white PMMA precipitate. After filtration, PMMA was repeatedly washed with ethanol and distilled water to remove residual catalyst and acid, and dried in vacuum at 60°C to constant weight.

[0030] Reaction conditions and results are shown in Tab...

Embodiment 2

[0039] metallocene CpTiCl 3 As a catalyst, it catalyzes the polymerization of St in the aqueous phase system

[0040] The entire polymerization operation and reaction process are carried out under the protection of an inert gas, and the metallocene catalyst CpTiCl is sequentially added to the reactor 3 , polymerized monomer St 1g, stirred for 1 hour, added an aqueous solution of sodium dodecylsulfonate (5.77×10 -3 g SDS / 10ml H 2 O), continue stirring for 1 hour, add St 1g. Put it into the set temperature for reaction, after polymerization for a certain period of time, quench with 20ml of 10% ethanol hydrochloric acid solution to terminate the polymerization, add excess ethanol to precipitate the polymer, and immediately a white PS precipitate is formed. After filtration, PS was repeatedly washed with ethanol and distilled water to remove residual catalyst and acid, and dried in vacuum at 60 °C to constant weight.

[0041] Reaction conditions and results are shown in Table ...

Embodiment 3

[0047] metallocene CpTiCl 3 As a catalyst, catalyze the copolymerization of MMA and St in the aqueous phase system

[0048] The entire polymerization operation and reaction process are carried out under the protection of an inert gas, and the metallocene catalyst CpTiCl is sequentially added to the reactor 3 , polymerized monomer MMA 0.5g, St 0.5g, stirred for 1 hour, added the aqueous solution of sodium dodecylsulfonate (5.77×10 -3g SDS / 10ml H 2 O), continue stirring for 1 hour, add MMA 0.5g, St 0.5g. Put it into the set temperature for reaction, after polymerizing for a certain period of time, quench with 20ml of 10% ethanol hydrochloric acid solution to terminate the polymerization, add excess ethanol to precipitate the polymer, and immediately a white precipitate is formed. After filtration, the copolymer was repeatedly washed with ethanol and distilled water to remove residual catalyst and acid, extracted with cyclohexane to remove homopolymer PS, and then extracted wi...

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Abstract

The invention discloses a catalyzing method of metallocene catalyst to do water-phase polymerize, which comprises the following steps: adding metallocene catalyst in the reactor; putting 1-2% polar monomer; stirring 0.5-3h; adding emulsifier; stirring continuously for 0.5-3h; supplementing 1-2% polar monomer; polymerizing under 30-85 deg. c in the water phase for 2. 5-25h; adding alcohol solution of alcaine to terminate the reaction; sedimenting the polymer; proceeding after-disposal to obtain the product.

Description

technical field [0001] The invention relates to a metallocene catalyst catalyzed water phase polymerization method, in particular to a method for catalyzing the homopolymerization and copolymerization of polar monomer acrylates and styrene. Background technique [0002] Metallocene catalysts have extremely high catalytic activity, single active center, good uniformity of polymerization products, and relatively narrow molecular weight distribution of polymers. Moreover, it has excellent copolymerization ability, and the obtained polymer has the advantages of controllable microstructure, molecular weight and its distribution. In recent years, the synthesis of binuclear or multinuclear metallocene compounds has become a major research focus in the field of metallocene-catalyzed olefin polymerization. More than one active center can be formed during the polymerization process, so that polymers with broad molecular weight distribution or bimodal distribution can be obtained. [...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F2/16C08F2/26C08F4/76C08F212/08
Inventor 孙俊全严小丽任华程进李洪峰
Owner ZHEJIANG UNIV