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Rare earth catalyst for preparing polyisoprene and preparation method and method for preparing polyisoprene

A rare earth catalyst and a technology for polyisoprene, which are applied to the rare earth catalyst for preparing polyisoprene and the preparation method and the fields of preparing polyisoprene, and can solve the problems of high corrosiveness of chlorine gas, environmental pollution and the like

Inactive Publication Date: 2007-10-03
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

However, chlorine gas is used as the chlorine source of the rare earth catalyst, which is highly corrosive and pollutes the environment.

Method used

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  • Rare earth catalyst for preparing polyisoprene and preparation method and method for preparing polyisoprene

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Under the protection of nitrogen, add 15 mL of 0.1M Nd(vers) to the dry catalyst reactor successively 3 Hexane solution, 15 mL of 1.0M isoprene in hexane, 15 mL of 2.0M Al(i-Bu) 3 Hexane solution, react at 50°C for 5 minutes to obtain a yellow-green solution; then add 15mL 0.2M Al(i-Bu) 2 Cl hexane solution, after reacting at 50°C for 30 minutes, a homogeneous rare earth catalyst for isoprene polymerization was obtained.

[0030] Under nitrogen protection, 2560 mL of hexane solvent and 440 mL of isoprene (300 g) monomer were added to a 5 L dry and oxygen-free autoclave, and the monomer concentration was 10 g / 100 mL at this time. Then add the above-mentioned prepared catalyzer, the molar number of catalyst Nd and the gram number ratio of adding monomer are 5.0 * 10 -6mol / g. After reacting at 40°C for 4 hours, the reaction was terminated with an ethanol solution containing 1.0% 2,6-di-tert-butyl-p-cresol, and then the polymer was precipitated in excess ethanol. °C and...

Embodiment 2

[0033] Under the protection of nitrogen, 24 mL of 0.1M Nd(vers) was sequentially added to the dry catalyst reactor 3 hexane solution, 48mL of 1.0M butadiene in hexane, 36mL of 2.0M Al(i-Bu) 3 hexane solution at 80°C for 1 minute to obtain a dark yellow-green solution; then add 12mL of 0.2M Al(i-Bu) 2 Cl in hexane solution reacted at 40°C for 120 minutes to obtain a homogeneous rare earth catalyst for isoprene polymerization.

[0034] Under nitrogen protection, 2560 mL of heptane solvent and 440 mL of isoprene (300 g) monomer were added to a 5 L dry and oxygen-free autoclave, and the monomer concentration was 10 g / 100 mL at this time. Then add the above-mentioned prepared catalyzer, the molar number of catalyst Nd and the gram number ratio of adding monomer are 8.0 * 10 -6 mol / g. After reacting at 40°C for 5 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...

Embodiment 3

[0037] Under the protection of nitrogen, 6 mL of 0.1M Nd(vers) was sequentially added to the dry catalyst reactor 3 hexane solution, 3mL of 1.0M piperylene in hexane, 6mL of 2.0M Al(i-Bu) 3 Add it into the reactor and react at 40°C for 5 minutes to obtain a yellow-green solution; then add 12mL of 0.2M Al(i-Bu) 2 Cl in hexane solution, react at 80°C for 5 minutes to obtain a homogeneous rare earth catalyst for isoprene polymerization.

[0038] Under nitrogen protection, 2118 mL of cyclohexane solvent and 882 mL of isoprene (600 g) monomer were added to a 5 L dry and oxygen-free autoclave, and the monomer concentration was 20 g / 100 mL at this time. Then add the above-mentioned prepared catalyzer, the molar number of catalyst Nd and the gram number ratio of adding monomer are 1.0 * 10 -6 mol / g. After reacting at 40°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, was...

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Abstract

This invention belongs to rare earth catalyzer for preparing polyisoprene, and its preparation method. This catalyzer is composed by carboxylic acid neodymium, aluminium alkyl, chloride, conjugated diolefine. Mixture ratio of aluminium alkyl, chloride, conjugated diolefine,and carboxylic acid neodymium is 5 - 30:1.0 -4.0:5 - 20:1. This invention could obtain homogeneous phase and stable rare earth catalyzer. This catalyzer possess higher catalytic activity, trigger off isoprene polymerization at higher polymerization temperature, obtain polyisoprene that has high content of syn- 1, 4 structure( not less than 96 percent) and narrow molecular weight distribution ( less than 3.0), and possess tensile crystallinity trait.

Description

technical field [0001] The invention belongs to a rare earth catalyst for preparing polyisoprene, a preparation method and a method for preparing polyisoprene. Background technique [0002] Isoprene rubber can be obtained by polymerizing isoprene with a rare earth catalyst. (Anthology of Rare Earth Catalyst Synthetic Rubber 1980, Science Press, 70-82) mentions catalysts composed of rare earth chloride complexes and alkylaluminum, rare earth carboxylates or phosphorus / phosphonates, alkylaluminum and chloride The catalyst composed of alkylaluminum can synthesize polyisoprene with a cis-1,4 structure content of 93-95%, but its performance is not as good as that of titanium-based isoprene rubber, and far less than that of natural rubber. [0003] Polyisoprene with high cis-1,4 structure content (≥96%) and narrow molecular weight distribution (distribution index <3.0) has excellent performance, which is superior to titanium-based isoprene rubber, close to natural rubber, and ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F136/08C08F4/602
Inventor 董为民李桂连柳希春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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