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Preparation method of high-cis-content butadiene-isoprene copolymer

A technology of isoprene and butadiene is applied in the field of preparation of butadiene-isoprene copolymers with high cis content, and can solve the problems of wide molecular weight distribution and low cis content, etc.

Inactive Publication Date: 2014-08-13
华宇橡胶有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The present invention provides the preparation method of high cis-content butadiene-isoprene copolymer, in order to solve the problem of low cis content and wide molecular weight distribution of butadiene and isoprene copolymer in the prior art question

Method used

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  • Preparation method of high-cis-content butadiene-isoprene copolymer

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Under nitrogen protection, add diisobutylaluminum hydride (HAl), isoprene (IP) and tris(2-ethylhexylphosphonic acid 2-ethylhexyl ester) neodymium in sequence to the dry catalyst reaction flask (Nd), after reacting at 30°C for 15 minutes, add diisobutyl aluminum chloride (Cl), and react at 60°C for 40 minutes to obtain a catalyst for the polymerization of butadiene and isoprene . In this catalyst, the molar ratio of [Nd] / [IP] / [HAl] / [Cl] is 1 / 30 / 5 / 2.5.

[0030] Under nitrogen protection, add 40 mL of the hexane solution of the reaction monomers butadiene and isoprene to a dry 100 mL ampoule, the molar ratio of butadiene to isoprene is 4:1, and then add the above-mentioned preparation Good catalyst, the mol ratio of reaction monomer and catalyst is 4000: 1;

[0031] The polymerization reaction was carried out at 30°C, and the polymerization reaction was terminated with ethanol solution after 4 hours, and coagulated with ethanol to obtain a random copolymer of butadiene a...

Embodiment 2

[0033] Under nitrogen protection, add diisobutylaluminum hydride (HAl), isoprene (IP) and tris(2-ethylhexylphosphonic acid 2-ethylhexyl ester) neodymium in sequence to the dry catalyst reaction flask (Nd), after reacting at 30°C for 10 minutes, add diisobutylaluminum chloride (Cl), and react at 60°C for 40 minutes to obtain a catalyst for the polymerization of butadiene and isoprene . In this catalyst, the molar ratio of [Nd] / [IP] / [HAl] / [Cl] is 1 / 30 / 5 / 2.5.

[0034] Under the protection of nitrogen, add 40 mL of the hexane solution of the reaction monomers butadiene and isoprene to a dry 100 mL ampoule, the molar ratio of butadiene and isoprene is 4:1, at -10 ° Freeze 1 hour under ℃, then add above-mentioned prepared catalyzer, the mol ratio of reaction monomer and catalyzer is 3000: 1;

[0035] The polymerization reaction was carried out at -10°C. After 48 hours, the polymerization reaction was terminated with ethanol solution, and the random copolymer of butadiene and isopr...

Embodiment 3

[0037] Under the protection of nitrogen, in the dry catalyst reaction bottle, add triisobutylaluminum (Al), isoprene (IP) and tris (2-ethylhexyl phosphonic acid 2-ethylhexyl ester) neodymium ( Nd), reacted at 30°C for 15 minutes, then added diisobutylaluminum chloride (Cl), and reacted at 60°C for 40 minutes to obtain a catalyst for the polymerization of butadiene and isoprene. In this catalyst, the molar ratio of [Nd] / [IP] / [Al] / [Cl] is 1 / 30 / 5 / 2.5.

[0038] Under the protection of nitrogen, add 40 mL of the hexane solution of the reaction monomers butadiene and isoprene to a dry 100 mL ampoule, the molar ratio of butadiene and isoprene is 4:1, at -10 ° Freeze 1 hour under ℃, then add above-mentioned prepared catalyzer, the mol ratio of reaction monomer and catalyzer is 3000: 1;

[0039]The polymerization reaction was carried out at -10°C. After 48 hours, the polymerization reaction was terminated with ethanol solution, and the random copolymer of butadiene and isoprene with h...

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Abstract

The invention belongs to the field of high-polymer synthesis. The invention discloses a preparation method of a high-cis-content butadiene-isoprene random copolymer, and aims to solve the problems of low cis-content and wide molecular weight distribution in the butadiene-isoprene copolymer in the prior art. The method comprises the following steps: preparing a homogeneous-phase stable organic rare-earth phosphonate catalytic system, wherein the system is mainly composed of a solution-type organic rare-earth phosphonate compound, alkyl aluminum disclosed as general formula AlR3 or AlHR2 or mixture thereof, a halogen-containing compound and conjugated diene; carrying out butadiene-isoprene random copolymerization at proper temperature by using the prepared organic rare-earth phosphonate catalytic system to prepare the high-cis-content butadiene-isoprene copolymer. In the butadiene-isoprene copolymer synthesized by the method, the cis-1,4 bond content of the butadiene chain segment is higher than 97%, and the cis-1,4 bond content of the isoprene chain segment is higher than 98%.

Description

technical field [0001] The invention relates to the technical field of polymer synthesis, in particular to a preparation method of a high-cis-content 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. The development of the rubber industry has always been inseparable from the development of its corresponding catalysts. Cis 1,4 content is an important parameter for butadiene and isoprene copolymers, high cis content has high elasticity and low hysteresis, high tensile strength and abrasion resistance. Molecular weight is also an important parameter for butadiene and isoprene copolymers, includi...

Claims

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Application Information

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IPC IPC(8): C08F236/06C08F236/08C08F4/52
Inventor 侯红霞王胜伟陈双喜王玉强陈晓丽苏忠魁胡尊燕刘海燕
Owner 华宇橡胶有限责任公司
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