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Rare earth catalyst and method for polymerizing conjugated diene by using same

A technology of rare earth catalysts and conjugated olefins, which is applied in the field of rare earth catalysts and their use in the polymerization of conjugated olefins, which can solve the problems of increased energy consumption and high price, and achieve the effect of high orientation and high catalytic activity

Active Publication Date: 2012-07-04
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

), it needs to be carried out at low temperature (such as: -20°C or -78°C) to obtain polyisoprene with cis-1,4 structure content > 98%, thus increasing energy consumption,

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Catalyst preparation and polymerization were carried out under nitrogen protection.

[0041] At 70°C, in a mixed solvent of n-hexane and isohexane (the volume ratio of the two is 6 / 4), mix 0.44mmol neodymium isooctanoate and 1.8mmol triphenylphosphine for 30min; at 50°C, in n-hexane, Mix 3.5mmol triisobutylaluminum, 7.0mmol chloroform and 0.03mmol ethanol for 3h; then mix and react the two for 1.5h to prepare a homogeneous catalyst system.

[0042] Add toluene, isoprene (monomer concentration = 2.7 mol / L) and the above catalyst system into the polymerization reactor, start the polymerization reaction at -40°C, and react under adiabatic conditions for 25 hours. The molar ratio of catalyst component A to monomer is 3.2×10 -3 . Add an ethanol solution containing 1% anti-aging agent 2,6-di-tert-butyl-p-methylphenol to terminate the reaction, wash with water and dry in a vacuum oven at 45°C until constant weight. The cis-1,4 content of the polyisoprene product is 97.2%, a...

Embodiment 2

[0044] Catalyst preparation and polymerization were carried out under nitrogen protection.

[0045] At 40°C, using hexane and cyclohexane (volume ratio: 9 / 1) as solvent, 10.5mmol triisobutylaluminum, 0.5mmol diisobutylaluminum hydride, 3.5mmol trichloromethane, 0.01mmol ethanol, 1.8 mmol of triphenylphosphine was mixed and reacted for 1 hour, and then mixed with 0.44 mmol of neodymium isooctanoate for 2 hours to prepare a homogeneous catalyst system.

[0046] Polymerization method and condition, termination reaction and aftertreatment method are all the same as embodiment 1, but the molar ratio of catalyst component A and total monomer is 2.0 * 10 -3 , Start polymerization at 30°C, and react under adiabatic conditions for 19h. Polyisoprene yield was 40%, M w 2.2×10 5,M w / M n is 3.2, and the cis-1,4 content is 97.3%.

Embodiment 3

[0048] Catalyst preparation and polymerization were carried out under nitrogen protection.

[0049] At 48°C, using hexane as a solvent, mix and react 0.26mol neodymium octanoate and 1.0mol triphenylphosphine for 18 hours, and mix and react 4.2mol triisobutylaluminum, 6.6mol trichloromethane and 0.11mol ethanol for 0.8h; They were mixed and reacted for 1.2h to prepare a homogeneous catalyst system.

[0050] Polymerization method and condition, termination reaction and aftertreatment method are all the same as embodiment 1, but the molar ratio of catalyst component A and total monomer is 2.5 * 10 -3 , Start polymerization at 0°C, and react under adiabatic conditions for 24h. Polyisoprene yield was 92%, M w 2.6×10 5 ,M w / M n is 2.5, and the cis-1,4 content is 97.0%.

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Abstract

The invention relates to a rare earth catalyst, in particular to a homogeneous rare earth catalyst for polymerizing conjugated diene and a method for polymerizing high cis conjugated diene. A homogeneous rare earth carboxylate-based catalysis system is adopted, high catalytic activity and stable catalytic performance are ensured, and high cis isoprene rubber, butadiene rubber, butadiene-isoprene copolymeric rubber or butadiene-styrene copolymer having the cis-1,4 structure content of more than 97 percent (and even more than 98 percent), the Weight-average molecular weight (Mw) range of 6.5*10<4> to 1.3*10<6> and relatively narrow molecular weight distribution (Mw/Mn=1.9-4.3) can be prepared by changing a catalyst preparation method, a component proportion and polymerization process conditions.

Description

Technical field: [0001] The present invention relates to a rare earth catalyst and its method for the polymerization of conjugated olefins, in particular to a rare earth catalyst and its use for the polymerization of butadiene, isoprene or styrene monomers to prepare homopolymers or copolymers way of things. Background technique: [0002] Natural rubber / synthetic rubber is an important strategic resource of the country, and has a wide range of applications in civil, automobile, aircraft manufacturing, aerospace, etc. However, my country's natural rubber resources are limited, and it is of great significance to vigorously develop synthetic rubber, especially high-performance synthetic rubber. [0003] Directional polymerization of conjugated dienes under the action of titanium-based, cobalt-based, nickel-based and rare earth-based catalysts can synthesize high-cis polymers. When the rare earth catalyst system is used for the polymerization of conjugated dienes, it shows sup...

Claims

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Application Information

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IPC IPC(8): C08F36/06C08F36/08C08F36/04C08F12/08C08F4/54C08F4/52C08F2/06C08F2/02
Inventor 吴一弦零萍朱寒
Owner BEIJING UNIV OF CHEM TECH
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