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A kind of termination method in the still of active polymer that prevents the generation of gel in the still

An active polymer and active technology, which is used in the field of termination in active polymer kettles, can solve problems such as poor thermal processing performance, product defects, and indissolubility

Active Publication Date: 2016-03-02
CHINA PETROLEUM & CHEM CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Gel is difficult to dissolve in commonly used solvents, and has poor thermal processing performance. It will still exist in the form of small solid particles in the general thermal processing process, resulting in poor surface finish of the processed product and defects inside the product.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025]In a clean polymerization kettle with magnetic stirring, cyclohexane is used as a polymerization solvent to synthesize styrene-isoprene-styrene active polymer by a step-by-step feeding method (the step-by-step feeding method is a common technology in the field of anionic polymerization) well-known to personnel), observe that the active polymer solution is yellow, and immediately add a terminator to terminate the active chain after the polymerization reaction is completed. Stir at 10-80°C for 0.1-20 minutes, and observe that the polymer solution is colorless and transparent after termination, indicating that the termination has been completed. The number average molecular weight of the polymer measured by sampling is 109,000, which is very close to the designed molecular weight of 107,000. Release the glue solution from the polymerization kettle, add an antioxidant and stir evenly, remove the solvent and dehydrate to obtain the final product. Put in the next batch of sol...

Embodiment 2~4

[0027] Change the terminator into isooctyl alcohol, 2-methyl-2-propanol, 3,7-dimethyl-3-octanol respectively, and repeat the steps of Example 1 to synthesize styrene-butadiene-styrene active polymer. The number average molecular weight of the polymer is about 110,000, which is very close to the design molecular weight of 107,000. After 100 tests, no gel was detected. The polymerization kettle was opened to observe the kettle wall, stirring shaft and stirring blades, and no gel was found.

Embodiment 5

[0029] The terminator is a combination of methanol and 3,7-dimethyl-3-octanol, where methanol: 3,7-dimethyl-3-octanol = 1:1, and the amount added is the hydroxyl group in methanol and 3,7 -Total hydroxyl groups of the sum of hydroxyl groups in dimethyl-3-octanol:active chain end=1.1:1 (molar ratio) Repeat the steps of Example 1. The number average molecular weight of the polymer is 110,000, which is very close to the design molecular weight of 107,000. After 100 tests, no gel was detected. The polymerization kettle was opened to observe the kettle wall, stirring shaft and stirring blades, and no gel was found.

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PUM

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Abstract

The invention discloses a reactive polymer in-kettle termination method capable of preventing generation of gel in a kettle. According to the method, one or more selected from the group consisting of alcohols, phenols and carboxylic acids are used as a terminator and added into a reaction vessel in which polymerization of active anions is completed, and a reaction is terminated for 0.1 to 20 min at 10 to 80 DEG C. The method has the advantages of a fast termination speed, a substantial termination effect, capacity of accurately controlling molecular weight, easy availability of raw materials and capability of preventing generation of gel in the kettle.

Description

technical field [0001] The invention discloses a method for terminating an active polymer in a kettle to prevent gel generation in the kettle, and belongs to the field of polymer synthesis. Background technique [0002] The polymerization or copolymerization of conjugated dienes or vinyl aromatics mostly belongs to anionic polymerization using organic alkali metals as initiators. The characteristics of anionic polymerization are: once the monomer is initiated, the chain growth reaction starts immediately to form ion pairs, and the monomer is continuously inserted into the ion pair. If there is no terminator to terminate it, as long as there are monomers, the chain growth reaction will continue. Continue until all monomers are consumed. In order to control the appropriate molecular weight, a terminator must be used to terminate the chain extension reaction. There are two types of termination: internal termination and external termination. Termination outside the reactor doe...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F2/42C08F297/04
Inventor 周燎原彭小寒李望明佘振银姚琼胡朝阳
Owner CHINA PETROLEUM & CHEM CORP
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