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Synthetic method of high-cis-alkadiene polymer

A technology of a diene polymer and a synthesis method, which is applied in the field of synthesis of high cis diene polymers, can solve the problems of increasing volatile content, solvent residue, and needing to reach a certain temperature, etc.

Inactive Publication Date: 2017-12-22
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

[0018] The invention provides a kind of synthetic method of high cis-diene polymer, comprising:

[0019] In an anhydrous and oxygen-free airtight container, the reaction solution including diene monomer, liquid methane and rare earth composite catalyst is polymerized to obtain a high cis diene polymer; the diene 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 diene polymer is polybutadiene; when the diene monomer is isoprene, the diene polymer The compound is polyisoprene; when the diene monomer is liquid butadiene and isoprene, the diene polymer 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. ...

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 methane into the polymerization bottle under liquid nitrogen freezing conditions to form a monomer 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 / 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. ...

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 methane into the polymerization bottle under liquid nitrogen freezing conditions to form a monomer 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, catalyst The molar ratio of medium rare earth compound to monomer [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] The resulting copolymerized product was repeatedly washed w...

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Abstract

The invention provides a synthetic method of a high-cis-alkadiene polymer. The synthetic method comprises the step of carrying out polymerization reaction on a reaction solution containing alkadiene monomers, liquid methane and a rare earth composite catalyst in an anhydrous and oxygen-free closed container so as to obtain high-cis-alkadiene polymer, wherein the alkadiene monomers are liquid butadiene and / or isoprene, and the filling degree of the reaction solution in the closed container is 30%-70%. According to the synthetic method, liquid butadiene and / or isoprene are taken as the raw materials, low-boiling-point methane is taken as a solvent, the polymerization reaction is carried out under anhydrous and oxygen-free closed conditions by virtue of the catalysis of the rare earth composite catalyst, and after the reaction is finished, methane can be volatilized at room temperature, so that the residual solvent in a product is reduced, the obtained product is easy to recycle and separate, the post-treatment temperature of the product is decreased, and the energy source is saved.

Description

technical field [0001] The invention relates to the technical field of polymer synthesis, 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 r...

Claims

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Application Information

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