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Comb-like polyfarnesene rubber and preparation method thereof

A technology of polyfarnesene and farnesene, which is applied in the field of polyfarnesene rubber with comb-like structure and its preparation, can solve the problems of harsh process condition control, low catalytic efficiency, easy deactivation and the like, and achieves flexural resistance. Excellent fatigue performance, high catalytic efficiency, good grip

Inactive Publication Date: 2020-06-26
青岛竣翔科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The object of the present invention is to provide a kind of polyfarnesene rubber of comb structure and preparation method thereof, solves the problem that existing farnesene polymerization adopts anion method to prepare usually, adopts alkyllithium catalyst in the anion method, to oxygen, moisture And other impurities are sensitive and easy to deactivate, and have the disadvantages of harsh control of process conditions in industrial production, and the problem of low catalytic efficiency

Method used

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  • Comb-like polyfarnesene rubber and preparation method thereof
  • Comb-like polyfarnesene rubber and preparation method thereof
  • Comb-like polyfarnesene rubber and preparation method thereof

Examples

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Embodiment 1

[0032] This embodiment provides a polyfarnesene rubber, which is prepared by the following method: under nitrogen protection, 750 mL of farnesene monomer is added to the reactor, followed by adding 1.2 mL of triisobutyl Aluminum and 0.4 g anhydrous magnesium chloride loaded with 2% TiCl 4 The Ziegler-Natta catalyst is used, and the reaction pressure in the reactor is adjusted to be 0.2MPa. The polymerization reaction temperature was 60°C, and the polymerization reaction was 6 hours. After the polymerization was completed, acidified ethanol was added to terminate the polymerization reaction, and vacuum-dried at 90°C to obtain about 168 grams of colorless to light yellow transparent polyfarnesene rubber material.

[0033] In this reaction, the catalytic efficiency of the product is 3500 / g.Ti.h, and the obtained polyfarnesene rubber homopolymer has a weight-average molecular weight Mw of about 115861, and the sample is named PFR1.

Embodiment 2

[0035] This embodiment provides a polyfarnesene rubber, which is prepared by the following method: under nitrogen protection, 750 mL of farnesene monomer is added to the reactor, followed by adding 1.2 mL of triisobutyl Aluminum and 0.4 g anhydrous magnesium chloride loaded with 2% TiCl 4The Ziegler-Natta catalyst is used, and the reaction pressure in the reactor is adjusted to be 0.2MPa. The polymerization reaction temperature is 60°C, and the polymerization reaction is 6 hours. During the polymerization reaction, hydrogen gas is added once every two hours. The partial pressure of hydrogen gas is 0.005, and a total of three times are added at 0h, 2h, and 4h respectively. First, nitrogen is used to adjust the reaction The reaction pressure of the reactor was 0.02 and then 0.005 partial pressure was supplemented with hydrogen. After the polymerization was completed, acidified ethanol was added to terminate the polymerization reaction, and vacuum-dried at 90° C. to obtain about...

Embodiment 3

[0038] This embodiment provides a polyfarnesene rubber, which is prepared by the following method: under nitrogen protection, 750 mL of farnesene monomer is added to the reactor, followed by adding 1.2 mL of triisobutyl Aluminum and 0.4 g anhydrous magnesium chloride loaded with 2% TiCl 4 The Ziegler-Natta catalyst is used, and the reaction pressure in the reactor is adjusted to be 0.2MPa. The polymerization reaction temperature is 60°C, and the polymerization reaction is 6 hours. During the polymerization reaction, hydrogen is added every 1 hour, and the partial pressure of hydrogen is 0.005. A total of three times are added at 0h, 1h, 2h, 3h, 4h, and 5h. , first use nitrogen to adjust the reaction pressure of the reactor to 0.02 and then use hydrogen to supplement 0.005 partial pressure. After the polymerization was completed, acidified ethanol was added to terminate the polymerization reaction, and vacuum-dried at 90° C. to obtain about 208 grams of colorless to light yell...

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Abstract

The invention discloses comb-like polyfarnesene liquid rubber and a preparation method thereof. The comb-like polyfarnesene liquid rubber and the method are characterized in that: a certain amount offarnesene, organic aluminum and an MgCl2 supported titanium catalyst are added into a polymerization device for bulk or solution polymerization; the molar ratio of the Ti element in the MgCl2 loaded titanium catalyst to the farnesene monomer is 1: (100-1000000); the molar ratio of the Al element in the organic aluminum to the Ti element in the MgCl2 loaded titanium catalyst is (10-200): 1, the polymerization reaction temperature is 0-120 DEG C, the hydrogen partial pressure is 0-1 MPa, the polymerization time is 1-72 hours, then unreacted monomers or solvents are removed and drying is performed to obtain the polyfarnesene liquid rubber. The polyfarnesene liquid rubber has the excellent characteristics of low viscosity, good fluidity, excellent low-temperature performance, low heat generation, good wear resistance, good road holding performance, excellent flexural fatigue resistance and the like, and is suitable for dynamic rubber products, and the preparation method adopts a titanium catalytic system, so that the catalytic efficiency is high and the method is more suitable for industrial production.

Description

technical field [0001] The invention relates to the field of rubber preparation, in particular to a comb-shaped polyfarnesene rubber and a preparation method thereof. Background technique [0002] Liquid rubber is a kind of relative molecular mass between about 2000-10000, which is a viscous fluid liquid at room temperature. After proper chemical reaction, it can form a three-dimensional network structure, so as to obtain physical and mechanical properties similar to ordinary vulcanized rubber. Oligomers and liquid rubber can be directly added with fillers and reinforcing agents to prepare rubber products, and can also be added to thermosetting resins and other polymers for modification. In addition, the active functional groups of liquid rubber can react with many other groups to form New materials of various structures; the characteristics of liquid rubber are: first, the molecular weight should be appropriately small to maintain a fluid state; second, it must be able to p...

Claims

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Application Information

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IPC IPC(8): C08F136/22C08F2/38C08F4/64C08F4/02C08L7/00C08L19/00C08L91/06C08L57/02C08K13/04C08K3/02C08K3/22C08K3/06C08K5/09
CPCC08F136/22C08K2003/2241C08K2003/2296C08K2201/011C08L7/00C08L2205/035C08F2/38C08F4/6421C08F4/022C08L19/00C08L91/06C08L57/02C08K13/02C08K3/04C08K3/22C08K3/06C08K5/09
Inventor 曹兰臧晓燕郑雷荣先超王萌
Owner 青岛竣翔科技有限公司
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