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Preparation method of high cis polydiene

A polydiene and diene technology, applied in the field of polymer preparation, can solve the problems of reaching a certain temperature, increasing the volatile content, and wasting energy.

Inactive Publication Date: 2017-12-29
青岛瑞林材料科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Most of the technical solutions above adopt high boiling point solvents such as hexane, hexanaphthene or heptane as organic solvents, because the boiling point is higher, for example, the boiling point of hexane is 69°C, the boiling point of cyclohexane is 80.7°C, and the boiling point of heptane is 98.42°C, it is easy to cause solvent residue in the product, increase the volatile content, and the post-treatment of the product needs to reach a certain temperature, resulting in energy waste

Method used

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preparation example Construction

[0018] The present invention provides a kind of preparation method of high cis polydiene, comprising:

[0019] In an anhydrous and oxygen-free airtight container, the reaction solution including diolefin monomer, liquid ethane and rare earth composite catalyst is polymerized to obtain high cis polydiene; the diolefin monomer is liquid butadiene and / or isoprene; the filling degree of the reaction solution in the airtight container is 30-70%.

[0020] In the present invention, the diene monomer is liquid butadiene and / or isoprene. In the present invention, when the diene monomer is liquid butadiene, the polydiene is polybutadiene; when the diene monomer is isoprene, the polydiene is Polyisoprene; when the diene monomers are liquid butadiene and isoprene, the polydiene is a butadiene-isoprene copolymer. The present invention has no special limitation on the molar ratio of the liquid butadiene and isoprene, it can be adjusted according to the desired product.

[0021] In the pr...

Embodiment 1

[0036] Under vacuum, add 7mL of isoprene monomer and 6mL of butadiene monomer to a clean and dry 100ml polymerization bottle in sequence, and add 20mL of ethane into the polymerization bottle under liquid nitrogen freezing conditions to form monomer solution, the molar ratio of butadiene to isoprene is 1:1, then add 6mL of the prepared catalyst solution, the catalyst molar ratio [Nd] / [Al] / [Cl] / =1 / 15 / 2, the catalyst The molar ratio of medium rare earth compound to monomer [Nd] / [M]=10.5×10 -4 : 1; the catalyst and the solvent hexane are configured into a solution, the rare earth compound is configured into a 0.1mol / L solution, the alkylaluminum 1.0mol / L solution, and the halogen-containing compound 0.1mol / L solution is configured into a solution for convenient metering and addition.

[0037] The rare earth compound in the catalyst is neodymium neodecanoate, the alkylaluminum is triisobutylaluminum, and the halogen-containing compound is diisobutylaluminum chloride.

[0038] Put...

Embodiment 2

[0041] Under vacuum, add 17.5ml of isoprene monomer and 15mL of butadiene monomer to a clean and dry 100ml polymerization bottle in sequence, and add 25mL of ethane into the polymerization bottle under liquid nitrogen freezing conditions to form a single solid solution, the molar ratio of butadiene to isoprene is 1:1, then add about 6ml of prepared catalyst solution, catalyst molar ratio [Nd] / / [Al] / [Cl] / =1 / 15 / 2. The molar ratio of rare earth compound to monomer in the catalyst [Nd] / [M]=4.2×10 -4 :1;

[0042] The rare earth compound in the catalyst is neodymium neodecanoate, the alkylaluminum is triisobutylaluminum, and the halogen-containing compound is diisobutylaluminum chloride.

[0043] Put the polymerization bottle in a constant temperature water bath, and react at a constant temperature of 30° C. for 5 hours, then add an anhydrous ethanol solution containing 1% antiaging agent 264 to terminate the reaction.

[0044] After repeated washing with absolute ethanol three t...

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Abstract

The invention provides a preparation method of high cis polydiene. The preparation method comprises the following steps: in a water-free and oxygen-free closed container, carrying out a polymerization reaction of a reaction solution containing a diene monomer, liquid ethane and a rare earth composite catalyst to obtain the high cis polydiene, wherein the diene monomer is liquid butadiene and / or isoprene; the filling degree of the reaction solution in the closed container is 30-70%. By the preparation method, the liquid butadiene and / or isoprene is used as a raw material, the ethane with low boiling point is used as a solvent, and under a water-free and oxygen-free closed condition, the polymerization reaction is performed via catalysis of the rare earth composite catalyst; after the reaction, the ethane can be volatilized at room temperature, so that the solvent residue in the product is reduced, the obtained product is easy to recycle and easy to separate, the product post-treatment temperature is lowered, and energy is saved.

Description

technical field [0001] The invention relates to the technical field of polymer preparation, in particular to a preparation method of high cis polydiene. Background technique [0002] With the rapid development of the automobile industry, the demand for rubber with excellent performance is becoming stronger and stronger in the world. Rare earth polybutadiene rubber has the characteristics of high strength, flex resistance, low heat generation, wet skid resistance and low rolling resistance, and is the preferred rubber for the development of high-performance tires and energy-saving tires; rare earth polyisoprene rubber, structural Similar to natural rubber in performance, it is a general-purpose rubber with good comprehensive properties, and its water resistance and insulation are superior to natural rubber; rare earth butadiene-isoprene copolymer rubber (butadiene rubber) has excellent low temperature resistance Performance, wear resistance and low-temperature rolling resist...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F236/08C08F236/06C08F136/08C08F136/06C08F2/06C08F4/54
CPCC08F236/08C08F136/06C08F136/08C08F236/06C08F2/06C08F4/545
Inventor 郎秀瑞姜波
Owner 青岛瑞林材料科技有限公司
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