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A kind of 2,3-dimethyl-1,3-butadienyl block copolymer and its preparation method

A technology of block copolymer and butadiene, applied in the field of 2,3-dimethyl-1,3-butadiene-based block copolymer and its preparation

Active Publication Date: 2019-06-04
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But so far, there is no research report on block copolymerization of high-cis 1,4-poly(DMB) with other polyconjugated dienes

Method used

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  • A kind of 2,3-dimethyl-1,3-butadienyl block copolymer and its preparation method
  • A kind of 2,3-dimethyl-1,3-butadienyl block copolymer and its preparation method
  • A kind of 2,3-dimethyl-1,3-butadienyl block copolymer and its preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0139] Example 1: Under anhydrous and oxygen-free conditions, the rare earth compound 1 (4.9 mg, 10 μmol), [Ph 3 C][B(C 6 f 5 ) 4 ] (9.2mg, 10μmol) and Ai i Bu 3 (0.2mL × 0.25M) of toluene solution 2mL, at 25 ° C, was added to the toluene solution containing DMB and butadiene (BD) (the total amount of monomer is 10mmol, wherein DMB content is 50mol%) monomer (6mL). After stirring and reacting at room temperature for 2 hours, a small amount of ethanol solution was added to terminate the polymerization reaction. Then the reaction solution was poured into a small amount of 100 mL ethanol containing hydrochloric acid and stabilizer (BHT) for sedimentation. The obtained polymer was dried in a vacuum oven at 40° C. for 48 hours to obtain a polymer with a net weight of 0.74 g (yield 100%).

Embodiment 2~34

[0140] Examples 2-34: The experimental procedures of this series of examples are basically the same as those of Example 1, and the polymerization reaction conditions and the change conditions of the catalyst composition are described in Table 1 in detail.

[0141]

[0142]

[0143] Note: A is [Ph 3 C][B(C 6 f 5 ) 4 ], B is [PhNMe 2 H][B(C 6 f 5 ) 4 ], C is [NEt 3 H][B(C 6 f 5 ) 4 ].

Embodiment 12

[0144] Example 12: According to the sequential feeding method, the toluene solution of butadiene was first added to the toluene solution of the catalyst, and reacted for 0.5 hours, and then DMB was added to the reaction solution, and the reaction was continued for 1.5 hours.

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Abstract

The invention relates to a 2,3-dimethyl-1,3-butadiene-based block copolymer and a preparation method thereof, and belongs to the technical field of synthesis of polymers. The 2,3-dimethyl-1,3-butadiene-based block copolymer is formed by 2,3-dimethyl-1,3-butadiene and other conjugate dienes, and the cis-1,4 tacticity of a poly(2,3-dimethyl-1,3-butadiene) structure unit in the block copolymer is not less than 95%. The preparation method of the 2,3-dimethyl-1,3-butadiene-based block copolymer allows the 2,3-dimethyl-1,3-butadiene-based block copolymer with high cis-1,4 tacticity to be successfully prepared through polymerizing a 2,3-dimethyl-1,3-butadiene monomer and a 2-substituted-1,3-butadiene monomer by using a catalyst composition including a rare earth compound, an organic born salt, an organic aluminum compound and / or organic lithium.

Description

technical field [0001] The invention relates to the technical field of polymer synthesis, in particular to a 2,3-dimethyl-1,3-butadiene block copolymer and a preparation method thereof. Background technique [0002] In the field of tire manufacturing, especially in the formulation of tire tread rubber, in order to achieve the best rolling resistance, dry and wet adhesion and wear resistance of the tire, various fillers need to be added to the tire formulation. It has been found that thermoplastic resin particles can optimize the above properties of the tire. The glass transition temperature or melting temperature of this thermoplastic resin is 80-300° C., and the particle size is less than or equal to 200 microns. In addition, in the field of medical and edible rubber, especially in the field of medical rubber that is in direct contact with pharmaceuticals, it is often necessary to replace carbon black with hard plastic particles with a higher melting temperature or glass tr...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F230/06C08F236/04C08F236/08C08F4/54
CPCC08F4/545C08F230/06C08F236/045C08F236/08
Inventor 崔冬梅李世辉刘博
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI