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Preparation method of low-cis and high-vinyl hydroxyl-terminated polybutadiene rubber

A technology of hydroxyl-terminated polybutadiene and hydroxyl-terminated polybutadiene, which is applied in the field of polymer synthesis

Pending Publication Date: 2021-10-01
广东众和高新科技股份公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

CN106749775A discloses that the hydroxyl-terminated polybutadiene is used to carry out epoxidation reaction to prepare epoxy-terminated polybutadiene, which does not involve the preparation process of the hydroxyl-terminated polybutadiene base glue

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] In this example, low-cis, high vinyl-terminated hydroxyl polybutadiene rubber was prepared by the following preparation method:

[0054] Use a 500mL open glass bottle, put it in a nitrogen-sealed box, first weigh 30g of 20% n-butyllithium solution and 54g of cyclohexane, and pour them into the glass bottle, then add 0.01g of tetrahydrofuran, shake well, Then weigh 12g of divinylbenzene, and drop it into 7% n-butyllithium cyclohexane solution by means of dropwise addition. Put the thermometer in a glass bottle and insert it into the reaction solution. After the thermometer scale no longer rises, seal it and cool it for storage until use.

[0055] Then replace a 10L reactor with high-purity nitrogen, add 4500g of cyclohexane / n-hexane mixed solvent, add 1.35g of THF (tetrahydrofuran) / DMF (dimethylformamide) (prepared solution at a mass ratio of 1:1), and start Stir (150r / min) and stir well. After the temperature reaches 40-45°C, first add 32g of the bis / multifunctional ch...

Embodiment 2

[0057] In this example, low-cis, high vinyl-terminated hydroxyl polybutadiene rubber was prepared by the following preparation method:

[0058] The preparation of the initiator is the same as in Example 1. To the 10L reactor, add 4500g cyclohexane / n-hexane mixed solvent, add 1.35gTHF (tetrahydrofuran) and TMEDA (tetramethylethylenediamine) preparation solution (prepared by mass ratio 2:1 ), start stirring (150r / min) and stir well, after the temperature reaches 40-45°C, first add 32g of the above-mentioned bi / multifunctional chain extension initiator prepared above, after stirring well, then add 200g butadiene, Control the temperature peak at 95-105°C until the temperature does not rise for about 3 minutes, then add 1.5g of ethylene oxide to react for 15 minutes, add 1g of water for hydrolysis reaction for 10 minutes, and then pour into the liquid hydroxyl-terminated polybutadiene glue for 20 minutes Carbon dioxide, followed by the addition of tetrakis[β-(3,5-di-tert-butyl-4-hy...

Embodiment 3

[0060] In this example, low-cis, high vinyl-terminated hydroxyl polybutadiene rubber was prepared by the following preparation method:

[0061] The preparation of the initiator is the same as in Example 1. To the 10L reactor, add 4500g cyclohexane / n-hexane mixed solvent, add 1.35gTHF (tetrahydrofuran) and TMEDA (tetramethylethylenediamine) preparation solution (prepared by mass ratio 2:1 ), start stirring (150r / min) and stir well. After the temperature reaches 40-45°C, first add 32g of the bis / multifunctional chain extension initiator prepared above. After stirring well, add 312.5g of butadiene , control the temperature peak at 95-105°C until the temperature no longer rises for about 3 minutes, add 1.5g of ethylene oxide to react for 15 minutes, add 1g of water for hydrolysis reaction for 10 minutes, and then pass into the liquid hydroxyl-terminated polybutadiene glue 20min carbon dioxide, then add the combination of tetrakis[β-(3,5-di-tert-butyl-4-hydroxyphenyl) propionate] p...

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PUM

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Abstract

The invention provides a preparation method of low-cis and high-vinyl hydroxyl-terminated polybutadiene rubber. The preparation method comprises the following steps: (1) preparation of a bifunctional initiator: reacting bifunctional conjugated olefin with an alkali metal alkyl compound to obtain the bifunctional initiator; (2) preparing active polybutadiene; (3) carrying out ring-opening reaction to terminate polymerization; (4) hydrolyzing to obtain an alkaline hydroxyl-terminated polybutadiene glue solution; and (5) introducing carbon dioxide for alkaline neutralization to obtain hydroxyl-terminated polybutadiene, then adding an anti-aging agent, and removing the solvent to obtain the low-cis and high-vinyl hydroxyl-terminated polybutadiene glue solution. The number-average molecular weight of the hydroxyl-terminated polybutadiene rubber obtained by the preparation method disclosed by the invention is 5000-10000 g / mol, the cis content is 10-25%, the trans content is 40-60%, the content of a 1, 2 structure is 30-45%, and the content of a 1, 4-structure is 60-75%.

Description

technical field [0001] The invention belongs to the technical field of polymer synthesis, and relates to a preparation method of polybutadiene rubber with low cis type and high vinyl-terminated hydroxyl group. Background technique [0002] Hydroxyl-terminated polybutadiene can be divided into high-trans-terminated hydroxyl, high-cis-terminated polybutadiene, and high-vinyl-terminated hydroxyl polybutadiene in the field of product microscopic composition. At present, hydroxyl-terminated polybutadiene has been widely used in military fields, such as high-energy fuel coating agents in solid rocket propellants, etc. The industry uses more free radical processes, mainly anti-1,4 polymerization (over 60%), However, the molecular weight distribution is relatively wide. Japan Nippon Soda Co., Ltd. has developed high-vinyl-terminated hydroxyl polybutadiene, with a 1,2-polymer content of over 80%. Stable, usually used more in the electronic field, especially in the field of bonding a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08C19/00C08F136/06C08F2/38
CPCC08C19/00C08F136/06C08F2/38
Inventor 黎广贞王平杨寿盛郑岩张海涛廖伟超舒畅谢宝东刘君刘敏张先汉袁兴有柏木兰李林峰
Owner 广东众和高新科技股份公司
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