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Preparation method of branched polymer

A polymer and branching agent technology, which is applied in the field of preparation of branched polymers, can solve the problem of high price, achieve the effect of strong electron pulling ability, lower solution viscosity, and low price

Active Publication Date: 2015-05-27
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the branching effect of these two branching agents is better, their prices are relatively high

Method used

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  • Preparation method of branched polymer
  • Preparation method of branched polymer

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Experimental program
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Effect test

Embodiment 1

[0038] Under the protection of argon, add 50mL cyclohexane to the dry catalyst preparation bottle, then add 0.03mmol neodymium isooctanoate, 0.75mmol triisobutylaluminum, 0.15mmol diethylaluminum hydride, 0.09mmol diethyl chloride The aluminum was mixed evenly and reacted at room temperature for 1 hour to obtain a rare earth catalyst, which was set aside.

[0039] Under argon protection, add 0.3mol butadiene cyclohexane solution to the dry polymerization reactor, then add the above prepared catalyst solution, the molar ratio of neodymium isooctanoate to butadiene is 1×10 -4 . After polymerization at 50°C for 5 hours, a liquid butadiene-acrylonitrile copolymer was added, wherein the molar ratio of nitrile group to neodymium isooctanoate in the copolymer was 48, and the reaction was continued at 70°C for 0.5h. After the reaction, 1 wt% ethanol solution of 2,6-di-tert-butyl-p-cresol was added to terminate the reaction. After the polymer was washed, it was placed in a vacuum oven...

Embodiment 2

[0045] Under the protection of argon, add 30mL cyclohexane to the dry catalyst preparation bottle, then add 0.04mmol neodymium nonanoate, 0.6mmol triisobutylaluminum, 0.4mmol dibutylaluminum hydride, 0.16mmol diisobutyl chloride The base aluminum was mixed uniformly and reacted at room temperature for 0.5 h to obtain a rare earth catalyst, which was set aside.

[0046] Under the protection of argon, add 0.6mol butadiene and 0.2mol isoprene cyclohexane solution to the dry polymerization reactor, then add the catalyst solution prepared above, the molar ratio of neodymium nonanoate to monomer 5×10 -5 . After 4 hours of polymerization at 55°C, a liquid hydrogenated butadiene-acrylonitrile copolymer was added, wherein the molar ratio of nitrile groups to neodymium nonanoate in the copolymer was 29, and the reaction was continued at 60°C for 0.6h. After the reaction, 1 wt% ethanol solution of 2,6-di-tert-butyl-p-cresol was added to terminate the reaction. After the polymer was was...

Embodiment 3

[0052] Under argon protection, add 95mL hexane to the dry catalyst preparation bottle, then add 0.02mmol neodymium neodecanoate, 0.8mmol diisobutylaluminum hydride, 0.04mmol sesquiethylaluminum chloride and mix well The reaction was carried out for 1 h to obtain a rare earth catalyst, which was set aside.

[0053] Under the protection of argon, add 1mol of butadiene hexane solution to the dry polymerization reactor, then add the catalyst solution prepared above, the molar ratio of neodymium neodecanoate to monomer is 2×10 -5 . After polymerization at 70°C for 5 hours, a liquid butadiene-styrene-acrylonitrile copolymer was added, the molar ratio of nitrile group to neodymium neodecanoate in the copolymer was 8, and the reaction was continued at 80°C for 1 hour. After the reaction, add 1wt% ethanol solution of 2,6-di-tert-butyl-p-methylphenol to terminate the reaction. After the polymer is washed, it is placed in a vacuum oven at 45°C and dried to constant weight. The yield is ...

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Abstract

The invention relates to a preparation method of a branched polymer and particularly relates to the preparation method for branching a conjugated diene polymer with a rare earth catalytic system. The preparation method includes following steps: (1) under the effect of the rare earth catalytic system, performing polymerization to the conjugated diene polymer in an organic inert solvent; (2) adding a branching agent after the polymerization finished, and continuously carrying out a reaction for 0.1-1 h under 50-90 DEG C; (3) adding 1% by weight of an ethanol solution containing 2,6-ditert-butyl p-methylphenol to terminate the reaction to obtain the branched conjugated diene polymer, wherein the branching agent is a liquid polymer containing a nitrile group. The use amount of the branching agent, on the basis of a molar ratio of the nitrile group in the branching agent to rare earth carboxylate, is 5-50 and preferably is 5-30. By means of the method, the conjugated diene polymer, being higher than 98% in the content of a cis-1,4 structure, being adjustable in weight-average molecular weight in the range of 100000-1500000, being 1.5-4.0 in distribution of molecular weight and being 2.0-5.0 dL / g in solution viscosity [eta], can be prepared.

Description

technical field [0001] The invention relates to a preparation method of a branched polymer, in particular to a preparation method of a rare earth catalyst system branched conjugated diene polymer. Background technique [0002] Directional polymerization of conjugated dienes under the action of rare earth catalysts can synthesize polymers with high cis 1,4-structure content (>96%) and high molecular weight (such as rare earth butadiene rubber and rare earth isoprene rubber). A small increase in the cis content can significantly improve the performance of polydiene. For example, when the cis content of rare earth isoprene rubber increases from 95.7% to 96.9%, the tensile strength of the vulcanized rubber increases from 30.6MPa to 32.1MPa, The 300% modulus strength increased from 12.6MPa to 14.1MPa (anthology of rare earth catalyzed synthetic rubber, Science Press, 1980). At the same time, rare earth isoprene rubber is superior to titanium-based isoprene rubber in terms of ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G81/02C08F136/06C08F136/08C08F236/06C08F236/08C08F4/54C08F4/52
Inventor 张华强李艳芹董静何颖魏绪玲徐典宏李广全燕鹏华崔英宋同江崔彦君郑聚成李晶陈建刚梁滔龚光碧
Owner PETROCHINA CO LTD
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