Polyisoprene preparation method and prepared polyisoprene

A technology of polyisoprene and isoprene, applied in the field of polyisoprene, can solve problems such as poor effect

Active Publication Date: 2013-08-21
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, in actual use, the effect of removing titanium metal in polymers is not good.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0033] The improvement of the preparation method of polyisoprene provided by the present invention lies in that the catalyst in the obtained polyisoprene solution is deactivated and the polyisoprene solution is stabilized, that is, the polyisoprene solution is mixed with Oleic acid contact, therefore, the present invention has no method for obtaining polyisoprene solution by polymerizing isoprene monomer in a mixture containing isoprene monomer, catalyst and organic solvent under solution polymerization conditions In particular, methods known to those skilled in the art can be used.

[0034] For example, in the present invention, the isoprene monomer undergoes a solution polymerization reaction under the action of a catalyst. Thus, the isoprene monomer is generally polymer grade, which is commercially available.

[0035] In the present invention, the catalyst can be any suitable catalyst commonly used in the art for catalyzing the polymerization of isoprene monomers, for exam...

Embodiment 1

[0052] This example is used to illustrate the preparation of polyisoprene provided by the present invention.

[0053] Under the protection of nitrogen, add 1700g hexane, 350gIP to the 5L reactor, add TiCl 4 / triisobutylaluminum / diphenyl ether (the molar ratio of the three is 1:1:0.5) the hexane solution of catalyst, and catalyst consumption is 1.0×10 -3 mol Ti / mol IP, polyisoprene monomer concentration 17% by weight. React at 20° C. for 2 hours to obtain a polymer solution containing an active catalyst with a polymer weight percentage of 15%.

[0054] At 60°C, add 14.5 g of oleic acid hexane solution containing 40% by weight of oleic acid to the above polymer solution, and add 8.75 g of stabilizer 4-methyl-2,6-di-tert-butylphenol at the same time A 20% hexane solution was stirred and mixed for 30 minutes.

[0055] At 50°C, wash the polymer solution after the above treatment with 3.5L deionized aqueous solution containing 7.7g sodium hydroxide twice until the gel has no colo...

Embodiment 2

[0058] This example is used to illustrate the preparation of polyisoprene provided by the present invention.

[0059] Under the protection of nitrogen, add 2340g hexane, 350gIP into the 5L reactor, add TiCl 4 / triisobutylaluminum / diphenyl ether (the molar ratio of the three is 1:1:0.5) the hexane solution of catalyst, and catalyst consumption is 1.0×10 -3mol Ti / mol IP, polyisoprene monomer concentration 13% by weight. React at 20° C. for 2 hours to obtain a polymer solution containing an active catalyst with a polymer weight percentage of 10%.

[0060] At 60°C, add 14.5 g of oleic acid hexane solution containing 30% by weight of oleic acid to the above polymer solution, and simultaneously add 9.8 g of stabilizer N-phenyl-N'-isopropyl-p-phenylenediamine A hexane solution with a concentration of 20% by mass was stirred and mixed for 30 minutes.

[0061] At 40°C, the polymer solution after the above treatment was washed twice with 4L of deionized aqueous solution containing 5g...

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PUM

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Abstract

The invention relates to a polyisoprene preparation method and polyisoprene prepared with the method. According to the method, under the condition of solution polymerization, isoprene monomers in a mixture comprising isoprene monomers, a catalyst and an organic solvent are polymerized, such that a polyisoprene solution is obtained, wherein the catalyst comprises titanium halide and an organic aluminum compound. The method also comprises the steps that the obtained polyisoprene solution contacts oleic acid; a water solution of alkali metal hydroxide and / or a water solution of alkaline earth metal hydroxide is mixed with the solution obtained by the contact of the polyisoprene solution and oleic acid; and oil-water separation is carried out. With the method provided by the invention, the obtained polymer solution is stable; metal titanium content in separated polymer polyisoprene can be effectively reduced, such that polymer physical and mechanical performances can be ensured; and the method is simple and is easy to operate. Also, oleic acid is used for replacing a catalyst deactivator such as methanol, such that environment pollution can be effectively reduced.

Description

technical field [0001] The invention relates to a method for preparing polyisoprene and polyisoprene prepared by the method of the invention. Background technique [0002] According to its microstructure, polyisoprene can be divided into cis-1,4-polyisoprene, trans-1,4-polyisoprene, 3,4-polyisoprene and 1 , 2-polyisoprene. Among them, cis-1,4-polyisoprene is commonly known as isoprene rubber, and its microstructure is similar to natural rubber (such as Hevea, guayule). Isoprene rubber is widely used in the manufacture of tires and other rubber products, and is the main substitute of natural rubber. [0003] Many titanium-based Ziegler-Natta catalysts are available for the synthesis of cis-1,4-polyisoprene. In industrial production, only TiCl is usually used 4 -AlR 3 and TiCl 4 - Two types of catalysts, polyiminoalanes. Typically, the coordination polymerization of isoprene monomer is carried out as a solution polymerization. [0004] The physical and mechanical prope...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F36/08C08F2/06C08F6/02
Inventor 王超刘慧玲李传清吕鹏飞于国柱
Owner CHINA PETROLEUM & CHEM CORP
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