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Titanium system catalyst composition as well as preparation method and application thereof, and application of alkyl tetrahydrofurfuryl ether compound in titanium system catalyst

A composition and compound technology, applied in the titanium-based heterogeneous catalyst composition and its preparation, in the field of high-cis polyisoprene rubber, can solve the problems of high molecular weight, narrow molecular weight distribution, poor overall rubber performance, etc., To achieve the effect of high activity, simple synthesis method and easy control

Active Publication Date: 2014-07-02
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Lithium-based isoprene rubber (Li-IR) is a stereoregular elastomer formed by anionic solution polymerization of isoprene monomer under the action of an alkyllithium initiator; compared with titanium-based isoprene rubber, lithium The isoprene rubber has high molecular weight, narrow molecular weight distribution, and almost no gel, but the cis content of the isoprene rubber of the lithium isoprene is low (91%-92%), and the comprehensive performance of the rubber is not as good as that of the isoprene of the titanium.
In addition, lithium-based catalysts are very sensitive to impurities, especially compounds containing oxygen, sulfur, and nitrogen, and have very strict requirements on raw materials

Method used

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  • Titanium system catalyst composition as well as preparation method and application thereof, and application of alkyl tetrahydrofurfuryl ether compound in titanium system catalyst
  • Titanium system catalyst composition as well as preparation method and application thereof, and application of alkyl tetrahydrofurfuryl ether compound in titanium system catalyst

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0056] Triisobutylaluminum (Yanshan Petrochemical Rubber Factory) and ethyl tetrahydrofurfuryl ether (Yanshan Petrochemical Rubber Factory) were prepared into 0.05 mol / L and 0.005 mol / L hexane solutions for use. Titanium tetrachloride (Tianjin Guangfu Chemical Reagent Co., Ltd.) was prepared into a 0.05 mol / L hexane solution for use. Mix 5.2ml of triisobutylaluminum and 0.5ml of ethyl tetrahydrofurfuryl ether solution and place them in contact at -60°C for 30 minutes; place 5.2ml of titanium tetrachloride solution at -60°C. After 10 minutes, the aluminum ether mixture was added into the titanium tetrachloride solution and aged at -30°C for 1 hour.

[0057] Under nitrogen protection, in 5L reactor, add 1700g hexane, 350g IP, add above-mentioned catalyst mixed solution, catalyst consumption is 0.5 * 10 -4 mol Ti / mol IP, the single concentration is 17wt%. After reacting for 4 hours at 30°C, the methanol solution of 2,6-di-tert-butylhydroquinone (Shanghai Nuotai Chemical Co., Lt...

Embodiment 2

[0060] Triisobutylaluminum (Yanshan Petrochemical Rubber Factory) and ethyl tetrahydrofurfuryl ether (Yanshan Petrochemical Rubber Factory) were prepared into 0.05 mol / L and 0.005 mol / L hexane solutions for use. Titanium tetrachloride (Tianjin Guangfu Chemical Reagent Co., Ltd.) was made into a 0.05 mol / L hexane solution for use. Mix 2.5ml of triisobutylaluminum and 0.75ml of ethyl tetrahydrofurfuryl ether solution and place them in contact at -20°C for 30 minutes; place 2.1ml of titanium tetrachloride solution at -20°C. After 30 minutes, the aluminum ether mixture was added into the titanium tetrachloride solution and aged at 30° C. for 30 minutes.

[0061] Under nitrogen protection, in 5L reactor, add 1700g hexane, 350g IP, add above-mentioned catalyst mixed solution, catalyst consumption is 0.2 * 10 -4 mol Ti / mol IP, the single concentration is 17wt%. After reacting at 60°C for 3 hours, the reaction was terminated with a methanol solution of 2,6-di-tert-butylhydroquinone ...

Embodiment 3

[0064] Triisobutylaluminum (Yanshan Petrochemical Rubber Factory) and ethyl tetrahydrofurfuryl ether (Yanshan Petrochemical Rubber Factory) were prepared into 0.05 mol / L and 0.005 mol / L hexane solutions for use. Titanium tetrachloride (Tianjin Guangfu Chemical Reagent Co., Ltd.) was prepared into a 0.05 mol / L hexane solution for use. Mix 9.3ml of triisobutylaluminum and 4.7ml of ethyl tetrahydrofurfuryl ether solution and place them in contact at -40°C for 30 minutes; place 10.3ml of titanium tetrachloride solution at -40°C. After 30 minutes, the aluminum ether mixture was added into the titanium tetrachloride solution and aged at 10° C. for 20 minutes.

[0065] Under nitrogen protection, in 5L reactor, add 1700g hexane, 350g IP, add above-mentioned catalyst mixed solution, catalyst consumption is 1 * 10 -4 mol Ti / mol IP, the single concentration is 17wt%. After reacting at 20°C for 2 hours, the reaction was terminated with a methanol solution of 2,6-di-tert-butylhydroquinon...

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Abstract

The invention relates to a novel tetrahydrofurfuryl ether compound modified titanium system heterogeneous catalyst composition. The synthesis method of the catalyst composition is simple and easy to control. According to the invention, the amount of the tetrahydrofurfuryl ether compound in the catalyst composition disclosed by the invention is lower as compared with the traditional symmetrical ether, and the activity of the modified catalyst is higher as compared with the traditional symmetrical ether; and simultaneously, the catalyst composition disclosed by the invention can be used for synthesizing polyisoprene rubber with excellent physical and mechanical properties, wherein the cis-1,4-structure content of the synthesized polyisoprene rubber is higher and more than 99%, the Mooney viscosity ML(1+4) at 100 DEG C of the rubber is adjustable in a range from 60 to 90, the tensile strength of the rubber is more than 35MPa, and 300% stretching stress of the rubber is more than 14MPa. The synthesized polymer can partially replace natural rubber to be used for tyre products.

Description

technical field [0001] The invention relates to a titanium-based catalyst composition, in particular to a titanium-based heterogeneous catalyst composition and a preparation method thereof. The titanium-based heterogeneous catalyst composition of the present invention is especially suitable as a catalyst for isoprene polymerization to synthesize high-cis polyisoprene rubber with higher tensile strength. 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 a major substitute for natural rubber. In the 1970s, the highest consumption of synthetic isoprene rubber used to account for 15% of all synthetic isopren...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F36/08C08F4/649C08F4/642
Inventor 王超张杰李传清徐林于国柱梁爱民吕鹏飞刘慧玲
Owner CHINA PETROLEUM & CHEM CORP
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