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Method for preparing butadiene-isoprene copolymer

A technology of isoprene and butadiene, applied in the field of preparation of butadiene-isoprene copolymers, can solve the problems of low molecular weight, wide molecular weight distribution, and no preparation mentioned

Active Publication Date: 2012-05-02
CHANGZHOU INST OF ENERGY STORAGE MATERIALS &DEVICES
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Problems solved by technology

[0004] The preparation method of multiple butadiene-isoprene copolymers has been reported in the prior art, for example, "Rare Earth Catalyzed Synthetic Rubber Anthology" (Science Press, 1980) summarizes rare earth catalysts to prepare butadiene-isoprene copolymerization method of production, but does not mention the preparation of low molecular weight butadiene isoprene copolymers
Both free radical polymerization and cationic polymerization methods and sulfonic acid rare earth catalyst system can prepare low molecular weight butadiene isoprene copolymers, but the molecular weight distribution of the prepared butadiene isoprene copolymers is relatively wide
In the prior art, the Chinese patent with the publication number CN1599762A reports a method for preparing a butadiene-isoprene copolymer, which uses conjugated diene monomers, organic phosphates of rare earth metals, alkanes Butadiene and isoprene are reacted under the action of the catalyst system using a base-based reagent and a halogen donor containing an alkylaluminum halide as a catalyst system, but the molecular weight of the prepared butadiene-isoprene copolymer is relatively low High, wide molecular weight distribution

Method used

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  • Method for preparing butadiene-isoprene copolymer

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preparation example Construction

[0031] A preparation method of butadiene-isoprene copolymer, comprising:

[0032] a) reacting the reaction monomer and the solvent under the action of a catalyst to obtain a solution A;

[0033] b) adding ethanol solution to the solution A to coagulate butadiene and isoprene copolymer;

[0034] The reactive monomers are butadiene and isoprene,

[0035] The molar ratio of the reaction monomer to the catalyst is 100~4000:1,

[0036] The preparation method of described catalyst is:

[0037] Mixing and reacting the rare earth compound, butadiene, isoprene and alkylaluminum to obtain solution B;

[0038] Chloride was added to solution B for reaction to obtain a catalyst.

[0039] In addition, the present invention also includes:

[0040] Add 2,6-di-tert-butyl-p-cresol with a mass concentration of 0.005g / ml to 0.02g / ml into the solution A, and the 2,6-di-tert-butyl-p-cresol is an anti-aging agent , the trade name is anti-aging agent 264.

[0041] The present invention also in...

Embodiment 1

[0058] Under the protection of nitrogen, add neodymium neodecanoate (Nd), butadiene (BD) or isoprene (IP) and diisobutylaluminum hydride (Al) successively to the dry catalyst reaction flask, at 50 After reacting at °C for 5 minutes, dimethyldichlorosilane (Cl) was added and reacted at 25°C for 30 minutes to obtain a catalyst for the polymerization of butadiene and isoprene. In this catalyst, the molar ratio of [Nd] / [BD / IP] / [Al] / [Cl] is 1 / 10 / 30 / 2 / 0.

[0059] Under the protection of nitrogen, add 20 mL of the hexane solution of the reaction monomers butadiene and isoprene to a dry 50 mL reaction flask, the molar ratio of butadiene and isoprene is 4:1, and then add the above-mentioned For a good catalyst, the molar ratio of reaction monomer to catalyst is 400:1;

[0060] The polymerization reaction is carried out at 50°C, and after 4 hours of the polymerization reaction, the ethanol solution of anti-aging agent 264 with a mass concentration of 0.01 g / ml is terminated, and a low ...

Embodiment 2

[0062] Under the protection of nitrogen, add neodymium neodecanoate (Nd), butadiene (BD) or isoprene (IP) and diisobutylaluminum hydride (Al) successively to the dry catalyst reaction flask, at 50 After reacting at ℃ for 5 minutes, chlorobutylaluminum (Cl) was added and reacted at 25℃ for 30 minutes to obtain a catalyst for the polymerization of butadiene and isoprene. In this catalyst, the molar ratio of [Nd] / [BD / IP] / [Al] / [Cl] is 1 / 10 / 20 / 2.0.

[0063] Under the protection of nitrogen, add 20 mL of the hexane solution of the reaction monomers butadiene and isoprene to a dry 50 mL reaction flask, the molar ratio of butadiene and isoprene is 4:1, and then add the above-mentioned For a good catalyst, the molar ratio of reaction monomer to catalyst is 400:1;

[0064] The polymerization reaction is carried out at 50°C, and after 4 hours of the polymerization reaction, the ethanol solution of anti-aging agent 264 with a mass concentration of 0.01 g / ml is terminated, and a low molec...

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Abstract

The embodiment of the invention discloses a method for preparing butadiene-isoprene copolymer, which comprises the steps of: reacting a reaction monomer under the action of a catalyst so as to obtain a solution A; and adding an ethanol solution to the solution A so as to condense butadiene and isoprene copolymer, wherein the mol ratio of the reaction monomer to the catalyst is 100 to 4000:1. In the invention, the molecular weight and the molecular weight distributions of the butadiene-isoprene copolymer are controlled by controlling the mol ratio of the reaction monomer to the catalyst, and apolymerization reaction is terminated through hydroxyl in ethanol. The experimental result proves that the butadiene-isoprene copolymer prepared by the invention has the advantages of low molecular weight and narrow molecular weight distributions, wherein the molecular weight of the butadiene-isoprene copolymer is 1,000 to 120,000, and Mw / Mn is 1.1 to 2.0.

Description

technical field [0001] The invention relates to the technical field of rubber, in particular to a method for preparing a butadiene-isoprene copolymer. Background technique [0002] With the continuous improvement of the requirements for the variety and performance of rubber materials, the butadiene-isoprene copolymer rubber synthesized by the copolymerization of butadiene and isoprene has excellent low temperature resistance, wear resistance and low temperature resistance. Low rolling resistance and other properties have attracted widespread attention. [0003] Molecular weight is an important parameter for butadiene and isoprene copolymers, including number average molecular weight (M n ) and weight average molecular weight (M w ), wherein the number average molecular weight of the low molecular weight butadiene isoprene copolymer is generally 1,000 to 120,000. At the same time, the molecular weight distribution is also an important factor affecting the performance of th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F236/06C08F236/08C08F4/54
Inventor 张学全范长亮王佛松蔡洪光代全权毕吉福张春雨那丽华姜连升
Owner CHANGZHOU INST OF ENERGY STORAGE MATERIALS &DEVICES
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