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Rare-earth catalyst for diolefin polymerization and its prepn.

A rare earth catalyst and diolefin technology, applied in the field of rare earth catalyst and preparation, can solve the problems of difficult control and the like

Active Publication Date: 2006-09-20
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] The catalyst composed of rare earth halide electron donor complex and alkylaluminum catalyzes the polymerization of diolefins, and has high polymerization activity (Chinese Science, 1980, (2): 127-135; Macromolecules, 1982, 15: 230-233 ), but because the catalyst system is heterogeneous and has the properties of multiple active centers, the molecular weight distribution of the resulting polymer is quite wide (M w / M n >3.0), difficult to control

Method used

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  • Rare-earth catalyst for diolefin polymerization and its prepn.

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Under the protection of nitrogen, add 3.0×10 -4 mol of NdCl 3 3 (i-PrOH), 6 mL of 1.0 mol / L isoprene hexane solution, 4.5 mL of 2.0 mol / L MMAO toluene solution, and 9.5 mL of hexane was added. React at 20°C for 0.5 hour to obtain a rare earth catalyst for diolefin polymerization.

[0025] Under the protection of nitrogen, 2560 mL of hexane, 440 mL of isoprene (300 g) and the catalyst prepared above were added to a 5 L dry and deoxygenated autoclave. At this time, the monomer concentration is 10g / 100mL, and the Nd / isoprene ratio is 1.0×10 -6 mol / g. After reacting at 50°C for 4 hours, terminate the polymerization with an ethanol solution containing 1.0% 2,6-di-tert-butyl-p-cresol, then precipitate the polymer in excess ethanol, wash and extrude it with ethanol, and place it at 40°C Drying under reduced pressure for 24 hours yielded 285 g of isoprene polymerization product with a conversion rate of 95%. The cis-1,4 structure content measured by infrared spectrum is 96...

Embodiment 2

[0027] As in the catalyst preparation method and polymerization conditions in Example 1, only with NdCl 3 3EtOH instead of NdCl 3 • 3(i-PrOH).

[0028] The results of the obtained polyisoprene are as follows: the polymerization product is 240g, the conversion rate is 80%, the cis-1 and 4 structure content is 95.6% as measured by infrared spectroscopy, and the number average molecular weight is 146200 as measured by GPC. is 1.85.

Embodiment 3

[0030] As in the catalyst preparation method and polymerization conditions in Example 1, only with NdCl 3 ·3CH 3 (CH 2 ) 5 OH instead of NdCl 3 • 3(i-PrOH).

[0031] At this time, the result of using the polyisoprene obtained therefrom is as follows: 270 g of the polymerized product, the conversion rate is 90%, the cis-1, 4 structure content is 96.0% as measured by infrared spectroscopy, and the number average molecular weight as measured by GPC is 189,500. The molecular weight distribution was 1.83.

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Abstract

This invention is attributed to the rare earth catalyst for diene polymerization and its preparation method. The catalyst is composed of neodymium chloride electron donor complex and organic methylaluminoxane with a molar ratio of 1:20~200. Monomers can be also added, with a neodymium chloride electron donor complex / monomer molar ratio of 1:5~40. The preparation method is simple and the obtained rare earth catalyst has high catalytic activity. With this catalyst, polybutadiene with a cis-1, 4-butadiene content of over 95%, polyisopentadiene and butadiene / isopentadiene copolymer can be obtained and the polymers uniquely have narrow molecular weight distributions, i.e., the ratio of weight-average molecular weight to number-average molecular weight is not larger than 2.0.

Description

technical field [0001] The invention belongs to a rare earth catalyst and a preparation method for diolefin polymerization. Background technique [0002] The catalyst composed of rare earth halide electron donor complex and alkylaluminum catalyzes the polymerization of diolefins, and has high polymerization activity (Chinese Science, 1980, (2): 127-135; Macromolecules, 1982, 15: 230-233 ), but because the catalyst system is heterogeneous and has the properties of multiple active centers, the molecular weight distribution of the resulting polymer is quite wide (M w / M n >3.0), difficult to control. [0003] Catalyst system composed of organoaluminoxane as cocatalyst and rare earth compound, such as tri(isopropoxy) neodymium / methylaluminoxane (polymer science, Journal of Polymer Science: Part A: Polymer Chemistry 2002, 40, 1838 -1844) or tri(isopropoxy) neodymium / modified methylaluminoxane (high polymer, Polymer 2003, 44:1561-1567) catalyst, can prepare narrow molecular ...

Claims

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Application Information

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IPC IPC(8): C08F36/02C08F4/52
Inventor 董为民李桂连任长友姜连升张学全王佛松
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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