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Olefines unsaturated bond-containing polymer hydrogenation reaction method

A hydrogenation reaction and unsaturated technology, which is applied in the field of polymer hydrogenation reaction containing olefinic unsaturated bonds, can solve the problems of large amount of hydrogenation catalyst, high reaction temperature, and large heat release, etc., to improve the hydrogenation reaction Efficiency, good heat transfer effect

Active Publication Date: 2014-05-14
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the inventive method has a fast hydrogenation rate, it has the following disadvantages: the amount of hydrogenation catalyst is large and the reaction temperature is high; the liquid holdup of the trickle bed reactor is small and the utilization rate of the unit volume reactor is low; The heat transfer effect of the reactor is not good. In the initial stage of the reaction, when the concentration of double bonds in the polymer solution is high and the heat of reaction is large, it is difficult to withdraw the heat of reaction. The amplitude increases, which in turn will deactivate the hydrogenation catalyst, prolong the hydrogenation cycle or reduce the degree of hydrogenation of the final product
The disadvantage of this invention is that the reactor structure is complicated, the manufacturing cost is high and the hydrogenation degree of the final product is low
[0007] US 4,501,875, US 4,673,714 and GB 2,159,819A all use stirred tanks for intermittent hydrogenation. Due to the high concentration of double bonds in the reaction solution in the early stage of the reaction and the fast hydrogenation rate, the heat release is large, making it difficult to control the reaction temperature. Catalyst deactivation affects hydrogenation efficiency
In addition, the batch reaction is not conducive to industrial scale-up

Method used

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  • Olefines unsaturated bond-containing polymer hydrogenation reaction method
  • Olefines unsaturated bond-containing polymer hydrogenation reaction method

Examples

Experimental program
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Effect test

Embodiment 1

[0034] This example is used to illustrate the hydrogenation method of polymers containing olefinic unsaturated bonds.

[0035] The 500L jacketed stirred reactor was fully replaced with purified nitrogen, and after the replacement, 250L of cyclohexane and hexane mixed solvent (the weight percentage of cyclohexane in the mixed solvent was 87% by weight) and 3.5L of refined styrene were added, and 1.15 L tetrahydrofuran, then add 0.71L of 0.5M n-butyllithium initiator solution (the molar ratio of tetrahydrofuran to n-butyllithium is 40:1), react at 50-60°C for 30 minutes, continue to add 24L refined butadiene for 30 minutes Minutes, then add 3.5L refined styrene to react for 30 minutes, add 27ml isopropanol after the completion of the reaction to terminate the reaction. Here, the concentration of the styrene-butadiene block polymer (S-B-S) is about 10% by weight based on the entire polymerization system, the molecular weight of the block polymer is 60,000, and the weight of styre...

Embodiment 2

[0043] Except that the ratio of the recycle flow in the first loop reactor to the flow out of said loop reactor was 100, the ratio of the recycle flow in the second loop reactor to the flow out of said loop reactor was 40 Except, carry out the hydrogenation reaction of the polymkeric substance containing olefinic unsaturated bond with the same method among the embodiment 1, the result is shown in Table 1.

Embodiment 3

[0045] In addition to the ratio of the recycle flow in the first loop reactor to the flow out of said loop reactor being 150, the ratio of recycle flow in the second loop reactor to the flow out of said loop reactor was 40 Besides, the same method as in Example 1 was used to carry out the hydrogenation reaction of the polymer solution containing olefinic unsaturated double bonds, and the results of the hydrogenation reaction are shown in Table 1.

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Abstract

The invention discloses an olefines unsaturated bond-containing polymer hydrogenation reaction method. The method comprises the following steps: under a hydrogenation reaction condition and existence of a hydrogenation catalyst, an olefines unsaturated bond-containing polymer solution and hydrogen are contacted in a reactor, wherein the reactors are two or more loop reactors connected in series, the cycle ratio of the loop reactors can be controlled so that the material in the reactor is close to a complete mixing flow state, wherein the cycle ratio of a first reactor is 10-200, and the cycle ratio of a second reactor and other reactor is 10-100. The method can better control the reaction temperature, the catalyst activity can be kept in a long operation period, hydrogenation efficiency is increased, and ideal hydrogenation degree can reached.

Description

technical field [0001] The invention relates to a method for hydrogenation reaction of polymers containing olefinic unsaturated bonds. More specifically, two or more loop reactors connected in series are used to continuously hydrogenate polymers containing unsaturated bonds in the presence of hydrogenation catalysts and hydrogen. Background technique [0002] Polymers containing unsaturated bonds have poor thermal and oxygen stability and aging resistance, so the unsaturated bonds of polymers are often saturated by hydrogenation to increase their stability. It is generally required that the degree of unsaturation of the polymer after hydrogenation is less than 2% (that is, the degree of hydrogenation is greater than 98%) in order to achieve significant improvement in polymer properties. Polymer hydrogenation is usually carried out in the presence of metal catalysts, which can be organic compounds of Group VIIIB metals of the periodic table such as Fe, Co, Ni and / or Pb, or m...

Claims

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Application Information

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IPC IPC(8): C08F297/04C08F136/08C08F136/06C08F236/10C08F8/04
Inventor 贺小进李传清张国娟赵英健李伟陈建军王爱东胡保利常学工陈淑明石建文
Owner CHINA PETROLEUM & CHEM CORP
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