Liquid poly conjugated 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: 2018-01-09
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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Experimental program
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Effect test

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 time of the initiation reaction is 1-8 minutes;

[0018] (2) In the presence of a retarder, the product of the initiating reaction is subjected to the first polymerization reaction to a conversion rate of more than 70% by weight of the conjugated diene; wherein, the retarder is selected from one of the metal alkyl compounds one or more kinds;

[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 capable of producing liquid polyconjugated...

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 of n-butyllithium (1mol.L -1 , the same below) to react for 2min; then add 120mL of triisobutylaluminum in hexane (1mol.L -1 , the same below), heated to 70°C for 100 minutes of polymerization reaction (the conversion rate of butadiene was 84% ​​by weight, and the highest temperature of the polymerization system was 131°C); then 85mL THF (about 1mol) was added, and the reaction was carried out at 80°C for 1.5h; Continuously feed carbon dioxide gas into the reaction system at 70° C., the pressure is 0.5 MPa, and the time is 20 min; stop feeding carbon dioxide gas, and add 1520 antioxidant (purchased from Ciba Chemicals, Switzerland) with a weight ratio of 1:1 after 10 min. (China) Co., Ltd., hereinafter the s...

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, 1200g of isooctane and 1200g of butadiene were added to the reaction vessel, and 120mL of a hexane solution of sec-butyllithium (1mol.L -1, the same below) to react for 4min; then add 108mL triisobutylaluminum hexane solution, heat to 60°C to carry out polymerization reaction for 120min (butadiene conversion rate is 88% by weight, and the highest temperature of the polymerization system is 129°C); then add 50mL THF (about 0.6mol), react at 70°C for 1.5h; continuously 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 2.4g of the mixture of 1520 antioxidant and 1076 antioxidant at a ratio of 1:1 and stirred for 10 minutes, a liquid polybutadiene rubber LCBR-2 was obtained with a number average molecu...

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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 invention relates to a 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 500-60,000. 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 shockproof pads. Liquid rubber is also an excellent processing aid and is widely used in the plastics industry and the electronics industry. According to different polymerized monomers, common liquid rubbers include 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, free radical polymerization is mainly used in China to produce liquid rubb...

Claims

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Application Information

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Patent Type & Authority Applications(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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