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Selective hydrogenation method of styrene/conjugated diene polymers

A technology for selective hydrogenation of conjugated dienes, applied in the field of selective hydrogenation of styrene/conjugated dienes polymers, can solve the problems of increased process complexity and increased consumption of synthetic products, and achieve improved hydrogenation reaction efficiency, Gentle hydrogenation reaction and improved hydrogenation efficiency

Active Publication Date: 2009-05-06
CHINA PETROCHEMICAL CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Improving the efficiency of the hydrogenation reaction by adding co-catalysts not only increases the complexity of the process, but also increases the consumption of synthetic products

Method used

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  • Selective hydrogenation method of styrene/conjugated diene polymers
  • Selective hydrogenation method of styrene/conjugated diene polymers
  • Selective hydrogenation method of styrene/conjugated diene polymers

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Example 1: Add 3000 milliliters of pure cyclohexane, 5.5 milliliters of tetrahydrofuran, and 4 mmol of n-butyllithium into a 10-liter polymerization kettle replaced with pure nitrogen, and heat up to 60° C. under stirring, then add 45 g of styrene to the The polymerization kettle carries out one-stage polymerization reaction; after one-stage reaction for 30 minutes, add 210g of butadiene to carry out two-stage reaction. Carry out three-stage polymerization, the three-stage polymerization temperature is 50° C. to 80° C., and the polymerization time is 30 minutes to 45 minutes; the styrene / butadiene polymer glue is obtained. Then introduce the styrene / butadiene polymer glue containing active lithium into the hydrogenation tank purified by nitrogen, and add butyllithium to the hydrogenation tank at a ratio of 20 molar ratio of active lithium to the main catalyst Stir for 3 minutes to 5 minutes. At this time, the temperature of the glue in the hydrogenation tank is 60°C to ...

Embodiment 2

[0016] Embodiment 2: The experiment process is the same as in Example 1, and the molar ratio of the procatalyst and the main catalyst is changed during the experiment. The experimental results are shown in Table 1.

[0017] Table 1 Effect of the molar ratio of co-catalyst to main catalyst on the hydrogenation degree of polymer

[0018]

Embodiment 3

[0019] Example 3: The experiment process is the same as that in Example 1. The cocatalyst is dicyclohexyldimethoxysilane, and the hydrogenation temperature of the styrene / conjugated diene polymer is changed during the experiment. The experimental results are shown in Table 2.

[0020] Table 2 Effect of hydrogenation start temperature on polymer hydrogenation degree

[0021]

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PUM

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Abstract

The invention provides a selective hydrogenation method for styrene / conjugated dienes polymer. The method takes dicyclopentadiene titanium dioxide as a main catalyst, and takes diphenyl dimethoxy silane or dicyclohexyldimethoxysilane as an auxiliary catalyst. The hydrogenation reaction lasts for one hour so that the double-bond hydrogenation degree in the styrene / conjugated dienes polymer is more than 98 percent. The hydrogenation reaction can be performed at lower temperature. The hydrogenation efficiency is high, and the reaction is slow, thereby contributing to the transfer of reaction heat.

Description

technical field [0001] The invention relates to a method for selective hydrogenation of styrene / conjugated diene polymer. Background technique [0002] In the prior art, there have been many patent reports on the selection of titanocene procatalysts for the selective hydrogenation saturation process of conjugated diene polymers, such as US patents 4,501,857; 4,980,421; Chinese patents 1067898; 1,070,412, etc. Patent No. 4,501857 emphasizes that titanocene compounds are used as the main catalyst, but at the same time it is necessary to add hydrocarbyl lithium as a reducing agent, wherein the atomic ratio of Ti:Li is at least 1:1. U.S. Patent No. 4,980,421 uses titanocene compounds as the main catalyst, and emphasizes the need to add alkoxide lithium (RO-Li) and organometallic compounds (such as organoaluminum, organomagnesium, organozinc) as reducing agents, wherein Ti: The Li atomic ratio ranges from 1:2 to 1:20, and the molar ratio of Ti to organic magnesium (or aluminum o...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F8/04C08F236/10
Inventor 邬智勇梁红文张志斌李望明张君花彭小寒何雪松
Owner CHINA PETROCHEMICAL CORP