A kind of liquid polyconjugated diene rubber and preparation method thereof

A technology of polyconjugated diene and conjugated diene, which is applied in the field of liquid polyconjugated diene rubber and its preparation, can solve the problems of poor molecular chain linearity, fast anionic polymerization rate, and reduced reaction rate, and achieve saving Desolvent removal link, good industrial application value, and the effect of improving production efficiency

Active Publication Date: 2020-06-09
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, free radical polymerization is mainly used in China to produce liquid rubber. Its advantage is low cost, and its disadvantages are poor linearity of molecular chains, easy branching, wide molecular weight distribution, and difficulty in microstructure adjustment.
[0004] The liquid polybutadiene rubber obtained by anionic polymerization has a narrow molecular weight distribution, the microstructure and molecular weight distribution can be adjusted freely, and the quality is uniform, but there are also significant shortcomings: the anionic polymerization rate is extremely fast, and the polymerization heat is difficult to withdraw in time; low molecular weight and At high monomer concentration, the conversion of the monomer is completed in a short time, the temperature of the polymerization system is as high as 300-400°C, the side reaction is very serious, and the product performance deteriorates
Due to the use of retarded anionic polymerization technology, the concentration of polymerized monomers has been greatly increased and the production efficiency has been improved, but there are disadvantages that the viscosity of the system increases sharply in the later stage and the reaction rate decreases sharply.

Method used

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Examples

Experimental program
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preparation example Construction

[0016] The invention provides a preparation method of liquid polyconjugated diene rubber, the method comprising:

[0017] (1) in the presence of an organolithium compound and a non-polar solvent, the conjugated diene is subjected to an initiation reaction, and the initiation reaction time is 1-8min;

[0018] (2) In the presence of a retarder, the first polymerization reaction of the product initiated by the reaction is carried out until the conversion rate of the conjugated diene is more than 70% by weight; wherein, the retarder is selected from a metal alkyl compound. one or more;

[0019] (3) In the presence of an accelerator, the product of the first polymerization reaction is subjected to a second polymerization reaction; wherein, the accelerator is one or more of saturated ether compounds.

[0020] According to the present invention, the conjugated diene can be a variety of conjugated dienes known in the art that can prepare liquid polyconjugated diene rubber, preferably...

Embodiment 1

[0057] This example is used to illustrate the liquid polybutadiene rubber of the present invention and its preparation method.

[0058] Under nitrogen protection, 1650 g of n-heptane and 720 g of butadiene were added to the reaction vessel, and 130 mL of a hexane solution (1 mol.L of n-butyllithium) was added under stirring at 150 rpm at 40 °C -1 , the same below) react for 2min; then add 120mL triisobutylaluminum hexane solution (1mol.L -1 , the same below), heated to 70°C for polymerization for 100min (conversion rate of butadiene was 84% ​​by weight, and the highest temperature of the polymerization system was 131°C); then 85mL of THF (about 1mol) was added, and the reaction was carried out at 80°C for 1.5h; In the reaction system, continue to feed carbon dioxide gas at 70 ° C, the pressure is 0.5MPa, and the time is 20min; stop feeding carbon dioxide gas, after 10min, add 1520 antioxidant (purchased from Ciba Chemistry, Switzerland) with a weight ratio of 1:1. (China) Co....

Embodiment 2

[0060] This example is used to illustrate the liquid polybutadiene rubber of the present invention and its preparation method.

[0061] Under nitrogen protection, 1200 g of isooctane and 1200 g of butadiene were added to the reaction vessel, and under stirring at 150 rpm and at 30 °C, 120 mL of a hexane solution of sec-butyllithium (1 mol.L -1, the same below) react for 4min; then add the hexane solution of 108mL triisobutylaluminum, be heated to 60 ℃ to carry out polymerization reaction 120min (the conversion rate of butadiene is 88% by weight, and the maximum temperature of the polymerization system is 129 ℃); then add 50mL THF (about 0.6mol), react at 70°C for 1.5h; continue to feed carbon dioxide gas into the reaction system at 70°C, the pressure is 0.6MPa, and the time is 15min; stop feeding carbon dioxide gas, and add weight after 10min After mixing 2.4g of 1520 antioxidant and 1076 antioxidant in a ratio of 1:1 and stirring for 10min; obtain liquid polybutadiene rubber ...

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Abstract

The present invention relates to the field of liquid poly conjugated diene rubbers, and discloses a liquid poly conjugated diene rubber preparation method, which comprises: (1) in the presence of an organic lithium compound and a non-polar solvent, carrying out an initiation reaction on conjugated diene for 1-8 min; (2) in the presence of a blocking agent, carrying out a first polymerization reaction on the product of the initiation reaction until the conversion rate of the conjugated diene is more than 70 wt%; and (3) in the presence of an accelerating agent, carrying out a second polymerization reaction on the product of the first polymerization reaction. The invention further provides the liquid poly conjugated diene rubber prepared through the preparation method. According to the present invention, with the preparation method, the performing of the polymerization reaction can be well controlled, such that the liquid poly conjugated diene rubber with characteristics of narrow molecular weight distribution and highly-controlled molecular weight can be prepared through the high monomer conversion rate; and especially the method can be performed in the high monomer concentration, and has the good industrial application value.

Description

technical field [0001] The present invention relates to liquid polyconjugated diene rubber, in particular, to a liquid polyconjugated diene rubber and a preparation method thereof. Background technique [0002] Liquid rubber is generally a viscous flowable rubber with an index average molecular weight of 500-60000. It has the advantages of simple processing equipment and easy operation. It can be used to prepare various rubber products such as tapes, hoses, and shock pads. Liquid rubber is also an excellent processing aid and has a wide range of uses in the plastics and electronics industries. According to different polymerized monomers, common liquid rubbers are polybutadiene rubber, polyisoprene rubber, styrene-butadiene copolymer, nitrile rubber and neoprene rubber. [0003] Liquid rubber polymerization methods mainly include free radical polymerization and anionic polymerization. At present, the free radical polymerization method is mainly used to produce liquid rubber...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F136/06C08F2/40C08F2/38
Inventor 李建成刘天鹤毕海鹏赵姜维
Owner CHINA PETROLEUM & CHEM CORP
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