Method for synthesis of solution-polymerized styrene butadiene rubber through two-component regulator

A solution-polymerized styrene-butadiene rubber and regulator technology, applied in the field of rubber, can solve problems such as uneven distribution of styrene, and achieve the effect of completely uniform and random distribution, mature technology and simple process

Active Publication Date: 2012-02-08
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The addition of polar additives can simultaneously make the two monomers random copolymerize and increase the 1,2-structure content in polybutadiene, but such polar additives

Method used

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  • Method for synthesis of solution-polymerized styrene butadiene rubber through two-component regulator

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Under the protection of nitrogen, add 100ml of cyclohexane, 7.6g of butadiene, 2.4g of styrene, 0.40ml of tetrahydrofuran, 0.0056g of potassium tert-butyl oxide into a purified 250ml polymerization bottle with electromagnetic stirring, and use n-butyllithium Residual impurities in the system were removed, and 0.10 mmol of n-butyllithium was added to carry out polymerization reaction at 50°C. Samples were taken at different reaction times, and the reaction was stopped and samples were taken after 3 hours. All samples were flocculated with ethanol, and then placed in a vacuum oven for extraction and drying. Determination of conversion rate by mass method, test by nuclear magnetic resonance spectrometer 1 H-NMR spectrum. Calculate the styrene content in the polymer and the 1,2-structure content in the copolymer at different reaction times.

[0035] Copolymer composition and 1,2-structure content under different conversion ratios of Table 1 Comparative Example 1 and Examp...

Embodiment 2

[0039] Under the protection of nitrogen, add 100ml of cyclohexane, 7.6g of butadiene, 2.4g of styrene, 0.24ml of tetrahydrofuran, 0.0051g of potassium tert-butyl oxide into a purified 250ml polymerization bottle with electromagnetic stirring, and use n-butyl Lithium was used to remove residual impurities in the system, and 0.10 mmol of n-butyllithium was added to carry out polymerization reaction at 50°C. Samples were taken at different reaction times, and the reaction was stopped and samples were taken after 3 hours. All samples were flocculated with ethanol, and then placed in a vacuum oven for extraction and drying. Determination of conversion rate by mass method, test by nuclear magnetic resonance spectrometer 1 H-NMR spectrum. Calculate the styrene content in the polymer and the 1,2-structure content in the copolymer at different reaction times.

[0040] Copolymer composition and 1,2-structure content under different conversion ratios of Table 2 Example 2

[0041] ...

Embodiment 3

[0044] Under nitrogen protection, add 70ml of cyclohexane, 30ml of hexane, 8.0g of butadiene, 2.0g of styrene, 0.40ml of tetrahydrofuran, 1,1-dimethylpropyl Oxypotassium 0.0057g, use n-butyllithium to remove residual impurities in the system, add n-butyllithium 0.10mmol to carry out polymerization reaction at 50°C, take samples at different reaction times, stop the reaction and take samples after 3 hours. All samples were flocculated with ethanol, and then placed in a vacuum oven for extraction and drying. Determination of conversion rate by mass method, test by nuclear magnetic resonance spectrometer 1 H-NMR spectrum. Calculate the styrene content in the polymer and the 1,2-structure content in the copolymer at different reaction times.

[0045] Copolymer composition and 1,2-structure content under different conversion ratios of Table 3 Example 3

[0046] Conversion rates(%)

[0047] As can be seen from Table 3, adding THF and potassium tert-butyl oxide into the...

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Abstract

The present invention discloses a method for synthesis of solution-polymerized styrene butadiene rubber through a two-component regulator, and belongs to the technical field of rubber. The method comprises the following steps: in the protection of nitrogen and in a hydrocarbon solvent, adopting organic lithium as an initiator, adopting butadiene and styrene as monomers, adopting tetrahydrofuran as a structure regulator, adopting tetrahydrofuran and potassium alkoxide as randomizing agents, carrying out an anionic random copolymerization reaction for the butadiene and the styrene; after completing the polymerization, carrying out flocculation and drying to obtain the solution-polymerized styrene butadiene rubber. The method provided by the present invention has characteristics of simple process and mature technology; with precise control of the use amounts of the regulator and the initiator, the 1,2- structure content can be controlled in the medium vinyl range, complete and uniform random distribution of the styrene units on the macromolecular chain can be realized.

Description

technical field [0001] The invention belongs to the technical field of rubber and relates to a method for synthesizing solution-polymerized styrene-butadiene rubber with a two-component regulator. Using anionic polymerization technology, organic lithium initiator is used to synthesize solution-polymerized styrene-butadiene rubber. By adding a two-component regulator during the polymerization process, the microstructure of the polymer can be controlled to have a medium vinyl content, and the styrene can be achieved. The purpose of uniform and random distribution of units on the macromolecular chain. Background technique [0002] Tires are an important part of a car's driving system. At present, the most prominent performances in tire performance are wear resistance, rolling resistance and wet skid resistance. Among them, the wear resistance directly affects the service life of the tire, and it is directly related to the economy of the tire. The performance of rolling resis...

Claims

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Application Information

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IPC IPC(8): C08F236/10C08F2/38C08F4/48
Inventor 张兴英刘涛唐清泉慕春雨
Owner BEIJING UNIV OF CHEM TECH
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