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A kind of method of synthesizing high cis diene polymer

A diene polymer and diene technology, applied in the field of synthesizing high-cis diene polymers, can solve the problems of reaching a certain temperature, increasing volatile content, solvent residue, etc.

Active Publication Date: 2021-07-09
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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Examples

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preparation example Construction

[0025] The present invention has no special limitation on the preparation method of the rare earth composite catalyst, and the technical solution for the preparation of the rare earth composite catalyst well known to those skilled in the art can be adopted. In the present invention, the preparation of the rare earth composite catalyst is preferably referred to Chinese patent CN 101831032 B. In the present invention, the rare earth compound in the rare earth composite catalyst undergoes an alkylation reaction with an aluminum alkyl, undergoes a halogen exchange reaction with a halogen-containing compound, and finally generates a bimetallic dinuclear active complex, or a multinuclear active complex .

[0026] In the present invention, the anhydrous and oxygen-free environment is preferably a vacuum or an inert atmosphere, more preferably a high-purity nitrogen atmosphere. In the present invention, the water-free and oxygen-free airtight container is preferably obtained by vacuu...

Embodiment 1

[0037] 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 n-pentane 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 the prepared catalyst solution, the catalyst molar ratio [Nd] / [Al] / [Cl] / =1 / 20 / 2 , the molar ratio of rare earth compound to monomer in the catalyst [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. .

[0038] The rare earth compound in the catalyst is neodymium neodecanoate, the alkylaluminum is triisobutylaluminum, and the halogen-containing compound is diisobutylaluminum chlorid...

Embodiment 2

[0042] 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 n-pentane 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 / 25 / 2, The molar ratio of rare earth compound to monomer in the catalyst [Nd] / [M]=10.5×10 -4 :1;

[0043] The rare earth compound in the catalyst is neodymium neodecanoate, the alkylaluminum is triisobutylaluminum, and the halogen-containing compound is diisobutylaluminum chloride.

[0044] Put the polymerization bottle in a constant temperature water bath, and react at a constant temperature of 40° C. for 5 hours, then add an anhydrous ethanol solution containing 1% antiaging agent 264 to terminate the reaction.

[0045] The resulting copolymerized product was repeatedly wash...

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Abstract

The invention provides a method for synthesizing high cis-diene polymers, comprising: in an anhydrous and oxygen-free airtight container, polymerizing a reaction solution comprising diene monomers, liquid pentane and a rare earth composite catalyst to obtain High cis diene polymer; the diene monomer is liquid butadiene and / or isoprene; the filling degree of the reaction solution in a closed container is 30-70%. The present invention uses liquid butadiene and / or isoprene as raw materials, and pentane with a low boiling point as a solvent, under anhydrous and oxygen-free airtight conditions, the polymerization reaction is carried out through the catalysis of a rare earth composite catalyst, and after the reaction is completed, the pentane It can be volatilized at room temperature, the solvent residue in the product is reduced, the obtained product is easy to recover and separate, the post-treatment temperature of the product is reduced, and energy is saved.

Description

technical field [0001] The invention relates to the technical field of polymer preparation, in particular to a method for synthesizing high cis-diene polymers. 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...

Claims

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Application Information

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IPC IPC(8): C08F236/08C08F236/06C08F136/06C08F136/08C08F2/06C08F4/54
CPCC08F136/06C08F136/08C08F236/08C08F236/06C08F2/06C08F4/545
Inventor 郎秀瑞姜波
Owner 青岛瑞林材料科技有限公司
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