Rare-earth catalyst and conjugated diene polymerization process

A rare earth catalyst and catalyst technology, which is applied in the field of polymerization of conjugated dienes, can solve the problems of reduced molecular weight and failure to meet the molecular weight requirements, and achieve the effects of small temperature fluctuations, easy control of the reaction, and stable catalytic performance

Active Publication Date: 2009-01-07
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Flat 3-185008 using R 1 -CO-N(OH)-C 6 h 2 (R) 3 As a ligand of rare earth elements, it can improve the phase state of the catalyst and produce polybutadiene rubber with a narrow molecular weight distribution (distribution index of 1.5 to 1.8), but at the same time cause a decrease in molecular weight (Mooney viscosity value is lower than 35), which cannot reach Requirements for molecular weight when used as a tire material (Mooney viscosity value is usually around 45)

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] at 50°C and N 2 Under protection, neodymium octanoate (0.05mmol), triisobutylaluminum (Al(i-Bu) 3 ) (0.78mmol), chloroform (1.7mmol), dichlorobutane (0.05mmol) and styrene (0.049mmol) were added to the dry catalyst preparation bottle, mixed evenly, and after aging for 26h, a light green transparent homogeneous catalyst solution.

[0024] in N 2 Under protection, add 30ml of butadiene / cyclohexane solution (wherein the monomer mass concentration is 12%) and the above-mentioned catalyst solution (catalyst / monomer=1.0mmol / mol) to start polymerization in the polymerization reactor at 10°C After reacting for 4 hours, an ethanol solution containing 0.1% by mass of 2,6-di-tert-butyl-p-cresol and hydrochloric acid was added to terminate the polymerization. After removing the solvent and unreacted monomers, the polymer product was obtained after repeated washing with ethanol / water and drying to constant weight. The weight average molecular weight of the product is 1.05×10 6 ...

Embodiment 2

[0026] at 50°C and N 2 Under protection, neodymium octanoate (0.09mmol), triisobutylaluminum Al(i-Bu) 3 (1.44mmol), chloroform (3.15mmol) and ethyl dichloroacetate (0.002mmol) were added to a dry catalyst preparation bottle, mixed uniformly, and after aging for 2h, a light gray blue transparent homogeneous catalyst solution was obtained.

[0027] in N 2 Under protection, add 40ml of butadiene and cyclohexane / raffinate (i.e. C 6 ~C 8 alkane mixed solution) (wherein the monomer mass concentration is 20%, cyclohexane / raffinate=1 / 1) and the above-mentioned catalyst solution (catalyst / monomer=0.9mmol / mol) start polymerization, after adiabatic reaction 4h, An ethanol solution containing 0.1% by mass of 2,6-di-tert-butyl-p-cresol and hydrochloric acid was added to terminate the polymerization. After removing the solvent and unreacted monomers, the polymer product was obtained after repeated washing with ethanol / water and drying to constant weight. The monomer conversion rate is 10...

Embodiment 3

[0029] at 40°C and N 2 Under protection, add neodymium octoate (0.08mmol), triisobutylaluminum (1.2mmol), trichloroethane (0.38mmol) into the dry catalyst preparation bottle, mix uniformly and age for 1.5h, a light gray blue color is obtained Transparent homogeneous catalyst solution.

[0030] in N 2 Under protection, add 30ml of butadiene and cyclohexane / raffin oil solution (wherein the monomer mass concentration is 20%, cyclohexane / raffin oil=1 / 1) and The above catalyst solution (catalyst / monomer = 1.0 mmol / mol) started the polymerization, and after 3.7 hours of reaction, an ethanol solution containing 0.1% by mass of 2,6-di-tert-butyl-p-cresol and hydrochloric acid was added to terminate the polymerization. After removing the solvent and unreacted monomers, the polymer product was obtained after repeated washing with ethanol / water and drying to constant weight. The weight average molecular weight of the product is 3.36×10 5 . The cis-1,4 structure content in polybutadi...

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Abstract

The related rare earth catalyst for conjugated diene has high catalytic activity even on low temperature, and benefit to obtain the product with high conversion ratio and yield. This product is convenient to apply and can control the polyreaction even there is 30% butadiene in system.

Description

Technical field: [0001] The invention relates to a rare-earth catalyst, especially a rare-earth catalyst for the polymerization of conjugated dienes and a polymerization method for conjugated dienes. Background technique: [0002] Polybutadiene or Polyisoprene, a material especially suited for making tires and other elastic materials. [0003] The polybutadiene rubber prepared by rare earth catalysis has better green rubber strength and vulcanized rubber properties, such as green rubber strength, Tear resistance, self-adhesiveness, hysteresis loss, wear resistance, flex crack resistance, hot air aging resistance and fatigue resistance. Therefore, polybutadiene rubber prepared by rare earth catalysis can adapt to the high-speed driving performance of automobiles and can be used to manufacture high-performance tires. [0004] In the liquid phase polymerization of conjugated diolefins in the presence of rare earth catalysts, the catalyst is usually composed of a rare earth s...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F36/04C08F4/602
Inventor 吴一弦朱寒王静郭青磊武冠英
Owner CHINA PETROLEUM & CHEM CORP
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