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Preparation method and application of catalyst for synthesizing hydroxyl-terminated trans-1, 4-polyisoprene polymer

A technology of polyisoprene and synthesis method, which is applied in the field of synthesizing hydroxyl-terminated trans-1, which can solve problems such as unsuccessful synthesis and achieve good regularity

Active Publication Date: 2021-04-09
青岛竣翔科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] In order to solve the technical problem of highly trans-coordinated hydroxyl-terminated trans-1,4-polyisoprene polymers that cannot be successfully synthesized in the prior art, the present invention provides a method for synthesizing hydroxyl-terminated trans-1,4-polyisoprene polymers. Catalyst preparation method for pentadiene polymer

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  • Preparation method and application of catalyst for synthesizing hydroxyl-terminated trans-1, 4-polyisoprene polymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Example 1 Synthesis of hydroxyl-terminated trans-1, the preparation of 4-polyisoprene polymer catalyst

[0028] 4.1 Under an inert atmosphere, add component C triethylsilyloxypropyllithium into the solution of component D polymer grade butadiene in proportion, the reaction temperature is 10°C, and the reaction time is 10h to obtain a reaction solution;

[0029] 4.2 Keeping in an inert atmosphere, the component A supported titanium-based catalyst TiCl 4 / MgCl 2 , B Tripropylaluminum was added to the solution obtained in 4.1 according to the proportion, and reacted at 0° C. for 480 minutes to obtain a catalyst for synthesizing hydroxyl-terminated trans-1,4-polyisoprene polymer.

[0030] Wherein, the molar ratio of components A, B, C, and D in the reaction process is 1:1:5:1.

Embodiment 2

[0031] Example 2 Synthesis of Terminated Hydroxyl Trans-1, Preparation of 4-polyisoprene Polymer Catalyst

[0032] 4.1 Under an inert atmosphere, add component C tert-butyldiphenylsilyloxypropyllithium into the solution of component D polymer-grade isoprene in proportion, the reaction temperature is 50°C, and the reaction time is 1h to obtain reaction solution;

[0033] 4.2 Keeping in an inert atmosphere, the component A supported titanium-based catalyst TiCl 4 / MgCl 2 , B Triethylaluminum was added to the solution obtained in 4.1 according to the proportion, and reacted at 60° C. for 60 minutes to obtain a catalyst for synthesizing hydroxyl-terminated trans-1,4-polyisoprene polymer.

[0034] Wherein, the molar ratio of components A, B, C, and D in the reaction process is 1:10:10:20.

Embodiment 3

[0035] Example 3 Synthesis of hydroxyl-terminated trans-1,4-polyisoprene polymer catalyst preparation

[0036]4.1 Under an inert atmosphere, add component C tert-butyldimethylsilyloxypropyl lithium in proportion to the solution of component D polymer-grade isoprene, the reaction temperature is 30°C, and the reaction time is 5h, to obtain reaction solution;

[0037] 4.2 Keeping in an inert atmosphere, the component A supported titanium-based catalyst TiCl 4 / MgCl 2 , B Triisobutylaluminum was added to the solution obtained in 4.1 according to the proportion, and reacted at 30° C. for 270 minutes to obtain a catalyst for synthesizing hydroxyl-terminated trans-1,4-polyisoprene polymer.

[0038] Wherein, the molar ratio of components A, B, C, and D in the reaction process is 1:5:8:10.

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Abstract

The invention belongs to the technical field of catalysts for synthesizing hydroxyl-terminated trans-1, 4-polyisoprene polymers, and discloses a preparation method and application of a catalyst for synthesizing hydroxyl-terminated trans-1, 4-polyisoprene polymers. The catalyst comprises the following components: A, a supported titanium catalyst TiCl4 / MgCl2; B, alkyl aluminum of which the general formula is AlR3, wherein R is alkyl of C1C6; C, alkyl lithium with silane protected hydroxyl; and D, polymerization grade butadiene or isoprene; and the preparation method comprises the following steps: in an inert environment, adding the component C into a solution of the component D in proportion, reacting to obtain a reaction solution, adding the component A and the component B into the reaction solution, continuously reacting, terminating the reaction with ethylene oxide, and carrying out acidolysis to obtain the catalyst for synthesizing the hydroxyl-terminated trans-1, 4-polyisoprene polymer. The catalyst provided by the invention can be used for synthesizing hydroxyl-terminated polyisoprene rubber with high trans content.

Description

technical field [0001] The invention belongs to the technical field of catalysts for synthesizing hydroxyl-terminated trans-1,4-polyisoprene polymers, in particular to a preparation method and application of a catalyst for synthesizing hydroxyl-terminated trans-1,4-polyisoprene polymers. Background technique [0002] Synthesis of hydroxyl-terminated trans-1,4-polyisoprene polymers in existing reports is generally through solvent dissolution of the finished product TPI (trans-1,4-polyisoprene polymers) that has been obtained, and then by related The auxiliary agent is reduced to obtain terminal hydroxyl groups; this treatment method requires a treatment process, which increases energy consumption and material consumption, and related solvents and auxiliary agents are toxic and harmful to environmental water bodies. Li Zaifeng and others use hydrogen peroxide as an initiator to synthesize hydroxyl-terminated polyisoprene rubber in a solvent. The content of anti-1,4 structural ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F136/08C08F4/646
CPCC08F136/08C08F4/6465C08F2500/18C08F2500/21
Inventor 王萌王鸿飞李寿张杰郑雷王志晔李迅臧晓燕
Owner 青岛竣翔科技有限公司
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