Catalyzing system for isoprene polymerization and preparation and application method of catalyzing system

A catalytic system and technology of isoprene, applied in the field of catalytic system for isoprene polymerization and its preparation and application, can solve the problem of polymer molecular weight and wide distribution, high dynamic viscosity of polymerization system, lower production capacity and Efficiency and other issues, to achieve high catalytic activity and homogeneous system stability, small temperature fluctuations, easy to react

Active Publication Date: 2013-02-06
CHINA PETROCHEMICAL CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Disclosed as CN1840552A is a kind of rare-earth catalyst system that is used for the polymerization of conjugated dienes, and its third component is chlorinated alkanes, and the fourth component is conjugated dienes and organic acid; In addition, the third component of catalyst disclosed in CN1347923A is chlorine Silane, the fourth component is conjugated diene, this type of rare earth catalyst is mostly a heterogeneous or semi-homogeneous catalytic system, the stability of the catalyst is poor, and there may be multiple active centers, and the catalytic polymerization process is difficult to control , so the molecular weight and distributi...

Method used

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  • Catalyzing system for isoprene polymerization and preparation and application method of catalyzing system
  • Catalyzing system for isoprene polymerization and preparation and application method of catalyzing system
  • Catalyzing system for isoprene polymerization and preparation and application method of catalyzing system

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Under nitrogen protection at 6°C, neodymium isooctanoate (3.5mmol), diisobutylaluminum hydride (35mmol), diethylaluminum chloride (7mmol), ethyl acrylate (5ml, molar weight 42.5mmol) and acetic acid The solution of benzyl ester (8ml, the molar weight is 45.3mmol) was respectively added to clean 250ml horn bottles equipped with hexane, and the concentration of neodymium was prepared to be 0.014mol / L, mixed evenly, and after aging for 3h, a light green transparent homogeneous Prepolymer active center catalytic system solution.

[0043] Under the protection of nitrogen, add 2L of hexane and 300ml of isoprene solution (wherein the monomer mass concentration is 13%) in the polymerization reactor of 2.5 liters at 20 ℃, then add above-mentioned catalytic system solution 25ml, (neodymium / monomer=0.17mmolNd / 100g isoprene) start stirring to carry out polymerization, the initiation time is 3min, after reacting for 3h, add 2,6-di-tert-butyl-p-methylphenol hexane solution containin...

Embodiment 2

[0045] Under nitrogen protection at 45°C, neodymium isooctanoate (3.5mmol), diisobutylaluminum hydride (56mmol), diethylaluminum chloride (10.5mmol), methyl acrylate (10ml, molar weight is 98.8mmol) and A solution of benzyl acetate (15ml, molar weight 85.0mmol) was added to a clean 250ml horn bottle filled with hexane to prepare a neodymium concentration of 0.014mol / L, mixed evenly, and aged for 3 hours to obtain a light yellow-green transparent homogeneous phase of the prepolymer active site catalyst solution.

[0046] Under nitrogen protection, add 1.5L of hexane / cyclohexane mixed solvent and 400ml of isoprene solution (wherein hexane / cyclohexane=1:1, monomer mass concentration 21%), then add 35ml of the above catalyst solution, (neodymium / monomer = 0.18mmolNd / 100g isoprene) start stirring to polymerize, the initiation time is 4min, after 3h of reaction, add the catalyst solution containing 0.5% mass fraction A solution of 2,6-di-tert-butyl-p-methylphenol in hexane terminat...

Embodiment 3

[0054] Under nitrogen protection at 20°C, neodymium isooctanoate (3.5mmol), diisobutylaluminum hydride (40mmol), triisobutylaluminum (12.5ml), diethylaluminum chloride (9.8mmol), methacrylic acid The solutions of methyl ester (10ml, molar weight 88.0mmol) and benzyl formate (27ml, molar weight 174.8mmol) were respectively added to a clean 250ml horn bottle filled with hexane, and the concentration of neodymium was prepared to be 0.014mol / L, and mixed evenly , After aging for 3h, a light green transparent homogeneous prepolymer catalyst solution was obtained.

[0055] Under nitrogen protection, add the hexane solvent of 1.3L and the isoprene of 400ml (wherein the mass concentration of monomer is 23.5%) in the polymerization reactor of 2.5 liters at 60 ℃, then add above-mentioned catalyst solution 30ml (Nd / monomer=0.15mmolNd / 100g isoprene), start stirring to carry out polymerization, the initiation time is 3min, after reacting for 3h, add a hexane solution containing 0.5% by ma...

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Abstract

The invention belongs to a catalyzing system for isoprene polymerization and preparation and an application method of the catalyzing system. The catalyzing system is composed of A) rare earth organic carboxylate compound, B) organic aluminum compound, C) activating agent, D) acrylate compound and E) carboxylic aromatic cyclic ester compound containing total carbon number of C7-C9 according to molar ratios that A:B=1:1-30, A:C=1:1-3, A:D=1:1-60, and A:E=1:5-50. The prepared catalyzing system forms pre-polymerized catalyst activity central body during ageing at 0-80 DEG C. The catalyzing system can be maintained for 180 days at the room temperature, the monomer conversion rate is higher than 98% in polymerization, the molecular weight distribution index of the synthesized poly-isoprene rubber is 1.6-2.8, cis-form 1,4 structural unit content is higher than 96%, and the Mooney viscosity satisfies that ML1+4100 DEG C =40-80.

Description

technical field [0001] The invention relates to a catalytic system for isoprene polymerization and its preparation and application method. Background technique [0002] Polyisoprene with high cis-1,4 structural unit content (cis-1,4 structural content>90%) can be synthesized by directional polymerization of isoprene under the action of titanium series, lithium series and rare earth catalysts. This material is particularly suitable for the manufacture of tires and other elastic materials. [0003] Compared with the polyisoprene rubber obtained by traditional titanium-based catalysis, the polyisoprene rubber obtained by rare earth catalysis has a high monomer conversion rate (conversion rate > 98%), regular molecular chain structure, cis-1 , 4 structure content > 95%, no gel, raw rubber appearance is close to colorless, residual catalyst does not need to be removed. It has better raw rubber strength, tear resistance, self-adhesiveness, abrasion resistance, flex crac...

Claims

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Application Information

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IPC IPC(8): C08F4/54C08F4/52C08F36/08
Inventor 张建国周燎原张红星戴立平陈移娇黄丽芳刘先珍
Owner CHINA PETROCHEMICAL CORP
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