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Crystallization-amorphism-crystallization stereo triblock polybutadiene and preparation method thereof

A technology of polybutadiene and polybutadiene block, applied in the field of polymer material synthesis and preparation, to achieve the effect of promoting characterization research work

Active Publication Date: 2008-04-30
大连广盛元实业有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Adopt second main group pure salt-alkyl aluminum-first main group metal catalyst system to synthesize high trans 1,4-structure / high 1,2-structure diblock polybutadiene has been reported (USP 4669518, Tire tread having high trans butadiene based elastomeric blockcopolymers and blends, 1987), but the preparation of triblock high trans 1,4-polybutadiene by difunctional alkyllithium initiator has not been reported

Method used

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  • Crystallization-amorphism-crystallization stereo triblock polybutadiene and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] In a 5-liter stainless steel reactor with stirring, add 3.5 liters of cyclohexane and 350 grams of butadiene, raise the temperature to 60°C, and add the bifunctional alkyllithium initiator 1,1'-(1,3-phenylene )-bis[3-methyl-1-(4-methylphenyl)pentyl]dilithium, start to prepare LCBR block, the amount of alkyllithium is 8×10 according to the polymer number average molecular weight 4 Metering, when the butadiene polymerization conversion rate reaches 50%, add barium thymol (BAT) and triisobutyl aluminum, start to prepare HTBR block, barium thymol (BAT) consumption is 0.5mmolBa / 100gBd ( butadiene), the amount of triisobutylaluminum is measured as (molar ratio) 1.0 / 4.0 / 4.0 according to the Ba / Al / Li ratio, and the reaction is continued until all butadiene is polymerized. After the butadiene polymerization is all finished, add Antiaging agent (1010 and 2.6.4 are mixed with weight ratio 1: 1) 3.5 grams, adopt traditional method to carry out glue solution aftertreatment, obtain H...

Embodiment 2

[0021] When the conversion rate of butadiene polymerization reaction reached 70%, barium thymol (BAT) and triisobutylaluminum were added, and other preparation conditions were exactly the same as in Example 1, and the prepared HTBR-LCBR-HTBR stereoterene The block ratio of segmented polybutadiene is 15 / 70 / 15, and its structure and performance analysis results are as follows: the total content of trans 1,4-structure in stereotriblock polybutadiene is 57.5%, and in HTBR block The trans 1,4-structure content is 77.0%, the molecular weight distribution index is 1.30, the glass transition temperature is -92.1°C, and the crystallization temperature is -65.8°C.

Embodiment 3

[0023] When the conversion rate of butadiene polymerization reaction reached 30%, barium thymol (BAT) and triisobutylaluminum were added, and other preparation conditions were exactly the same as in Example 1, and the prepared HTBR-LCBR-HTBR stereoterene The block ratio of block polybutadiene is 35 / 30 / 35, and its structural and performance analysis results are as follows: the total content of trans 1,4-structure in stereo triblock polybutadiene is 67.5%, and in HTBR block The trans 1,4-structure content is 77.0%, the molecular weight distribution index is 1.38, the glass transition temperature is -91.4°C, and the crystallization temperature is -64.1°C.

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Abstract

The invention relates to crystalline-noncrystalline-crystalline stereotriblock polybutadiene, which belongs to the technical field of the high molecular material synthesis and the preparation. The invention is characterized in that the polymer has the following symmetric structure: HTBR-LCBR-HTBR, wherein, HTBR is high trans-1,4-polybutadiene block, LCBR is low cis-polybutadiene block, the numberaverage molecular weight of stereoblock polymer is 5*10 <4> to 55*10 <4>, the block ratio of HTBR / LCBR is 10 / 90 to 60 / 40 (weight ratio), the general range of 1, 2-structural content in the LCBR block is 5 percent to 55 percent (weight percentage), and the general range of trans-1, 4-structural content in the HTBR block is 50 percent to 95 percent (weight percentage). The invention has the advantages that the preparation method for the crystalline-noncrystalline-crystalline stereotriblock polybutadiene is provided, and important promotion effect to the characterization research work of the crystalline and noncrystalline polymer is realized.

Description

technical field [0001] The invention belongs to the technical field of polymer material synthesis and preparation, and relates to crystalline-amorphous-crystalline three-block polybutadiene and a preparation method thereof. This block polymer has the following symmetrical structure: HTBR-LCBR-HTBR, Among them: HTBR is a high-trans 1,4-polybutadiene block, and LCBR is a low-cis polybutadiene block. The stereo triblock polymer prepared by the invention has better comprehensive properties, and the wet skid resistance, cold flow resistance and wear resistance can achieve a better balance. Background technique [0002] Polybutadiene usually has three structures: cis 1,4-, trans 1,4-, and 1,2-addition. When using alkyllithium as the initiator, butadiene is polymerized in a non-polar solvent, and the prepared polybutadiene is low-cis polybutadiene (LCBR), and its microstructure is: 1,2-addition The number of formed structures is about 8%, the cis-1,4-addition structure is about 4...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F297/00
Inventor 李杨张春庆张雪涛曾凡君李战胜张红霞王玉荣
Owner 大连广盛元实业有限公司
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