Butadiene-isoprene copolymer and preparation method thereof

A technology of isoprene and butadiene, which is applied in the field of butadiene-isoprene copolymer and its preparation, can solve the problems of low catalyst activity, large catalyst consumption, and restrictions on large-scale development and use. Achieve the effect of high activity and high cis structure content

Active Publication Date: 2021-02-26
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Although the existing rare earth catalysts have obtained available polybutadiene-isoprene rubber materials, there is a big problem, that is, the activity of the catalyst is low and the consumption of the catalyst is large
This makes the cost of materials high and limits the development and use of large-scale

Method used

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  • Butadiene-isoprene copolymer and preparation method thereof
  • Butadiene-isoprene copolymer and preparation method thereof

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preparation example Construction

[0019] The first aspect of the present invention provides a kind of preparation method of butadiene-isoprene copolymer, the method comprises:

[0020] (1) preparing a homogeneous rare earth catalyst, comprising: in a first organic solvent, mixing the first material and the fifth material for the first time, and then performing static treatment; then introducing the fourth material and the second material for the second mixing , and then introduce the third material for aging treatment; wherein, the time of the standing treatment is more than 1h; wherein, the molar ratio of the first material, the second material and the fifth material is 1:12-30:0.2 -0.4;

[0021] The first material: neodymium phosphonate compound shown in formula (1);

[0022] Formula 1) R a1 , R a2 , R b1 , R b2 , R c1 and R c2 Each independently hydrogen, hydroxyl, C 1 -C 20 Alkyl or C 1 -C 20 alkoxy;

[0023] The second material: an alkylaluminum compound selected from one or more of trialkyl...

preparation example 1

[0073] Add 30mL of hydrochloric acid (concentration: 12mol / L) to 0.05mol of Nd 2 o 3 , then heated to boiling and stirred for 30min, the obtained NdCl 3 The aqueous solution is lavender transparent. Add 0.3 mol of bis(2-ethylhexyl) phosphonate acetone solution (180 mL of acetone) into 450 mL of sodium hydroxide aqueous solution (sodium hydroxide content is 0.3 mol), mix well to obtain a light yellow solution, and then add The above NdCl 3 Aqueous solution, stirred and mixed to obtain a suspension containing fine white granular precipitates, filtered and washed the filter cake with appropriate amount of distilled water and acetone for 3 times, and dried in an oven at 60°C for 72 hours to obtain bis(2-ethylhexyl ) neodymium phosphonate.

[0074] Catalyst preparation example 1

[0075] Under nitrogen protection, mix 250mL of hexane, 6.2mmol of neodymium bis(2-ethylhexyl)phosphonate, and 1.86mmol of bis(2-ethylhexyl)phosphonate at 20°C for 30min and then let it stand for 24h ...

preparation example 2

[0077] 6.2 mmol of neodymium bis(2-ethylhexyl)phosphonate and 1.86 mmol of bis(2-ethylhexyl)phosphonate were mixed at 20° C. for 40 minutes and then left to stand for 5 hours. Then, at 30°C, 105mL of a hexane solution of diethylaluminum hydride with a concentration of 1mol / L and 248mmol of butadiene were added and stirred for 30min, then the temperature was raised to 80°C, and 18.6mL of a concentration of 1mol / L diiso hexane solution of butylaluminum chloride, and aged for 2h to obtain a catalyst in a homogeneous solution state, that is, a homogeneous rare earth catalyst C2, wherein the content of Nd element is 0.0159mmol / mL; two (2-ethylhexyl) The molar ratio of neodymium phosphonate, diethylaluminum hydride, diisobutylaluminum chloride, butadiene and bis(2-ethylhexyl)phosphonate is 1:17:3:40:0.3.

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Abstract

The invention relates to the field of preparation of butadiene isoprene copolymers, in particular to a butadiene isoprene copolymer and a preparation method thereof. The preparation method of the butadiene isoprene copolymer comprises the following steps: (1) preparing a homogeneous rare earth catalyst, namely mixing a first material and a fifth material in a first organic solvent, and performingstanding; introducing a fourth material and a second material for mixing, and then introducing a third material for aging; and (2) performing a polymerization reaction on butadiene and isoprene in a second organic solvent in the presence of a homogeneous rare earth catalyst; wherein A is a neodymium phosphonate compound shown as a formula (1); B: an alkyl aluminum compound; C: a halogenated compound; D: a conjugated diene; and E: a compound represented by formula (2). The homogeneous rare earth catalyst adopted in the preparation method has higher activity, and can still show higher activity under the condition of lower catalyst dosage.

Description

technical field [0001] The invention relates to the field of preparation of butadiene-isoprene copolymers, in particular to butadiene-isoprene copolymers and a preparation method thereof. Background technique [0002] The high cis-butadiene (Bd)-isoprene (Ip) copolymer rubber refers to a Bd-Ip copolymer with a cis-1,4-structure mole fraction greater than 90 wt%. High cis Bd-Ip copolymer rubber has excellent low temperature resistance and wear resistance, better wet skid resistance and lower rolling resistance, and has better processing behavior than butadiene rubber, and its vulcanized rubber comprehensive physical and mechanical properties It has good performance and has been applied in industrial products such as high-performance tires and shock-absorbing materials. The catalysts for preparing Bd-Ip copolymers mainly include lithium, transition metals (cobalt, nickel, titanium, chromium) and rare earth catalyst systems, wherein only rare earth catalyst systems can make th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F236/08C08F236/06C08F4/54
CPCC08F236/08C08F236/06C08F4/545
Inventor 唐正伟赵姜维徐林李建成邵明波孙伟
Owner CHINA PETROLEUM & CHEM CORP
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