Rare earth catalyst for catalyzing syn form 1,4-selectivity polymerization of isoprene or butadiene

A technology of rare earth catalysts and isoprene, applied in the field of rare earth catalysts, can solve the problems of catalyst activity improvement and achieve the effects of reduced selectivity, high stability and high polymerization activity

Active Publication Date: 2008-05-28
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The problem with the Ziegler-Natta catalytic system currently used in foreign industries is that the cis-1,4- content is lower than 98%, and the catalyst activity needs to be improved

Method used

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  • Rare earth catalyst for catalyzing syn form 1,4-selectivity polymerization of isoprene or butadiene
  • Rare earth catalyst for catalyzing syn form 1,4-selectivity polymerization of isoprene or butadiene
  • Rare earth catalyst for catalyzing syn form 1,4-selectivity polymerization of isoprene or butadiene

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Experimental program
Comparison scheme
Effect test

preparation Embodiment 1

[0041] Preparation Example 1 Preparation of Complex 1

[0042]

[0043] Preparation Example 1

[0044] At 0°C, a 1.5 mol / L hexane solution of butyl lithium (0.8 mL, 1.2 mmol) was added dropwise to the 2,6-(N-2,6-dimethyl)imino group 1 -A suspension of bromobenzene (0.5 g, 1.2 mmol) in hexane (20 mL). The reaction solution was reacted at this temperature for 4 hours and the YCl 3 (THF) 3.5 (0.64g, 1.44mmol) was added to the above reaction solution, the reaction solution naturally rose to room temperature and continued to react for 10 hours, the solvent was removed in vacuo, the residue was extracted with toluene, and the toluene solution was concentrated to obtain a total of 0.57g of bright yellow crystal complex 1 , yield 74%. Elemental analysis, its molecular formula is C 32 h 37 Cl 2 N 2 o 2 Y(%): C, 59.53; H, 5.74; N, 4.31.

preparation Embodiment 2

[0045] Preparation Example 2 Preparation of Complex 2

[0046]

[0047] At 10°C, at 0°C, a 1.5mol / L hexane solution of butyllithium (0.8mL, 1.2mmol) was added dropwise to 2,6-(N-2,6-diethyl 1-bromobenzene imino (0.57 g, 1.2 mmol) in hexane (20 mL). The reaction solution was reacted at this temperature for 6 hours and the YCl 3 (THF) 3.5 (0.64g, 1.44mmol) was added to the above reaction solution, the reaction solution naturally rose to room temperature and continued to react for 8 hours, the solvent was removed in vacuo, the residue was extracted with toluene, and the toluene solution was concentrated to obtain a total of 0.58g of bright yellow crystal complex 2 , yield 70%. Elemental analysis, its molecular formula is C 36 h 45 Cl 2 N 2 o 2 Y: C, 61.92; H, 6.47; N, 4.09.

preparation Embodiment 3

[0048] Preparation Example 3 Preparation of Complex 3

[0049]

[0050] At 0°C, a hexane solution (0.8 mL, 1.2 mmol) of butyllithium with a concentration of 1.5 mol / L was added dropwise to 2,6-(N-2,6.diisopropyl)imino 1-Bromobenzene (0.64 g, 1.2 mmol) was suspended in hexane (20 mL). The reaction solution was reacted at this temperature for 3 hours and the YCl 3 (THF) 3.5 (0.64g, 1.44mmol) was added to the above reaction solution, the reaction solution naturally rose to room temperature and continued to react for 8 hours, the solvent was removed in vacuo, the residue was extracted with toluene, and the toluene solution was concentrated to obtain a total of 0.54g of bright yellow crystal complex 3 , yield 60%. Elemental analysis, its molecular formula is C 40 h 53 Cl 2 N 2 o 2 Y: C, 63.64; H, 6.98; N, 3.63.

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Abstract

The invention relates to a rare-earth catalyst for catalyzing selective polymerization of isoprene or butadiene, while the catalyst system composed of the rare-earth catalyst can catalyze isoprene or butadiene to prepare polyisoprene or butadiene rubber with high cis-1, 4- structure. The rare-earth catalyst is composed of split-core type rare-earth complex, alkyl aluminium and organic boron salt. The solvent of polymerization is toluene or chlorobenzene. When catalyzes the polymerization of isoprene, the alkyl aluminium and split-core type rare-earth complex are rationed at 10-40, the organic boron salt and split-core type rare-earth complex are rationed at 1-3, the polymerization temperature is -20-80DEG C, the polymerization time is 0.5-2h, the monomer conversation ratio can reach 100% most, and the cis-1, 4 content of polymer is 55.0-98.8%, and when catalyzes the polymerization of butadiene, the alkyl aluminium and split-core type rare-earth complex are rationed at 10-40, the organic boron salt and split-core type rare-earth complex are rationed at 1-3, the polymerization temperature is -20-80DEG C, the polymerization time is 0.5-2h, the monomer conversation ratio can reach 100% most, and the cis-1, 4 content of polymer is 90.1-99.99%.

Description

technical field [0001] The invention relates to a rare earth catalyst for catalyzing the cis-1,4-selective polymerization of isoprene or butadiene. Background technique [0002] Natural rubber is an important strategic resource of the country and has a wide range of applications in civil, automobile, aircraft manufacturing, aerospace and other fields. However, my country's natural rubber resources are limited, and vigorously developing synthetic rubber, especially high-performance synthetic rubber, has extremely important practical and strategic significance. On the other hand, with the large-scale expansion of domestic ethylene projects, the C5 fraction increases. How to make full use of limited C5 resources to obtain high-performance and super-valued isoprene rubber is an urgent problem to be solved. Especially when the cis-1,4-content of polyisoprene rubber reaches 99%, its performance can be comparable to that of natural rubber. However, the catalysts for catalyzing t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F36/04C08F4/60
Inventor 崔冬梅高伟
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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