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Structure regulator for anionic polymerization and anionic polymerization method

A structure regulator, anionic polymerization technology, applied in the field of anionic polymerization, can solve the problems of increased rolling resistance, increased tire heat generation, affecting the service life of tires, etc., and achieves the effect of low rolling resistance and reduced content

Active Publication Date: 2015-05-20
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the proportion of solution-polymerized styrene-butadiene rubber used in tire tread rubber is increasing day by day, and the content of styrene micro-blocks in solution-polymerized styrene-butadiene rubber will have a greater impact on the rolling resistance of tire treads. High content will lead to a substantial increase in tire heat generation during vehicle driving, increased rolling resistance, and affect the service life of tires
Aiming at the requirement of styrene micro-block content in solution-polymerized styrene-butadiene rubber for tires, the existing methods generally use potassium alkoxide regulators or use a large amount of tetrahydrofuran to reduce the content of styrene micro-blocks, but these two methods make the production The cost is greatly increased, and the synthesis of completely random solution-polymerized styrene-butadiene rubber cannot be realized
[0003] U.S. Patent US20050004333 describes a method for synthesizing butadiene and isoprene copolymers, which uses organophosphates of various rare earth metals, an alkylating agent, and a compound containing alkylaluminum halides Catalytic system, by changing the ratio of each component in the catalytic system, the ratio of reaction monomers, and the control of reaction time, the purpose of synthesizing random butadiene-isoprene copolymer is finally achieved, but the conversion rate of this method is It still needs to be further improved, and the main structure generated is cis structure

Method used

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  • Structure regulator for anionic polymerization and anionic polymerization method
  • Structure regulator for anionic polymerization and anionic polymerization method
  • Structure regulator for anionic polymerization and anionic polymerization method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0090] Before polymerization, the mixed solvent (cyclohexane and n-hexane, weight ratio 88:12) was soaked with 5A molecular sieves (φ3×5, purchased from Dalian Kangyu Chemical Co., Ltd., prebaked at 500°C for 5 hours) for 1 week. Under the protection of high-purity nitrogen, 195Kg of mixed solvent, 7.83Kg of styrene, and regulator Tetrahydrofurfuryl Ethyl Ether (ETE, purchased from Sinopharm Chemical Reagent Beijing Co., Ltd., the same below) 62.7 g and sodium dimethyl butyl siliconate (purchased from Sinopharm Chemical Reagent Beijing Co., Ltd., the same as below) 5.94g, after the polymerization system is deoxygenated by high-purity N2, add 21.17Kg of butadiene, stir for 10 minutes, add 350ml of n-butyllithium solution (the concentration of n-butyllithium is 0.6mol / L) was used for polymerization. The polymerization initiation temperature was 50° C., and the reaction pressure was 0.1 MPa. After 10 minutes of reaction, the peak temperature reached 90° C., and the reaction pre...

Embodiment 2

[0093] Before polymerization, the mixed solvent (cyclohexane and n-hexane, weight ratio 88:12) was soaked with 5A molecular sieves (φ3×5, purchased from Dalian Kangyu Chemical Co., Ltd., prebaked at 500°C for 5 hours) for 1 week. Under the protection of high-purity nitrogen, 195Kg of mixed solvent, 7.83Kg of styrene, 81.22g of regulator tetrahydrofurfuryl ethyl ether, and potassium dimethyl butyl siliconate (purchased from Sinopharm Chemical Reagent Beijing Co., Ltd., the same below) 5.78g, after the polymerization system was deoxidized by high-purity N2, 21.17Kg of butadiene was added, and after stirring for 10 minutes, 350ml of n-butyllithium solution was added (the concentration of n-butyllithium was 0.6 mol / L) for polymerization. The polymerization initiation temperature was 50° C., and the reaction pressure was 0.1 MPa. After 10 minutes of reaction, the peak temperature reached 90° C., and the reaction pressure was 0.28 MPa. After 10 minutes of peak temperature, add 17...

Embodiment 3

[0096] Carry out according to the method for embodiment 1, difference is regulator tetrahydrofurfuryl ethyl ether 50.78g and sodium dimethyl butyl siliconate 7.22g, the number average molecular weight of the obtained styrene-butadiene rubber, molecular weight distribution , The microstructure data are shown in Table 1.

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Abstract

The invention discloses a structure regulator for anionic polymerization and an anionic polymerization method using the structure regulator. The structure regulator contains an alkylsilanol salt compound and alkyl tetrahydrofurfuryl ether. When the structure regulator provided by the invention is applied to solution copolymerization reaction of monovinylarene and conjugated diene, the microstructure of the obtained copolymer can be effectively regulated, and random distribution of various structural units on a macromolecular chain can be realized. Especially when the structure regulator provided by the invention is applied to solution copolymerization reaction of styrene and butadiene, the styrene block content can be significantly reduced.

Description

technical field [0001] The invention relates to a structure regulator for anionic polymerization, and also relates to an anion polymerization method using the structure regulator. Background technique [0002] The synthesis reaction of existing monovinylarene-conjugated diene copolymer rubber mainly adopts anion solution polymerization method. For example, the synthesis of solution-polymerized styrene-butadiene rubber uses cyclohexane as a solvent, alkyllithium or rare earth as a catalyst, and synthesizes solution-polymerized styrene-butadiene rubber by anionic solution polymerization. The most important use of solution-polymerized styrene-butadiene rubber is as a tire product. Tire products have developed from bias tires to radial tires, and then to high-performance radial tires and green radial tires. There are also higher and higher requirements for performance, which require low rolling resistance for energy saving and high requirements. Excellent anti-wet skid perform...

Claims

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Application Information

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IPC IPC(8): C08F236/10C08F2/38C08F2/06C08F8/42
Inventor 徐炜王世朝杨洪友周微频
Owner CHINA PETROLEUM & CHEM CORP
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