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Preparation method of polybutadiene

A technology of polybutadiene and polymerization reaction, applied in the field of polymers, can solve the problems of low polybutadiene yield and low catalytic activity, etc.

Active Publication Date: 2012-11-14
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, when the existing cobalt-based catalysts of Schiff base ligands catalyze the polymerization of butadiene, the catalytic activity is still low, so that the yield of polybutadiene is low

Method used

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  • Preparation method of polybutadiene
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  • Preparation method of polybutadiene

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preparation example Construction

[0033] The embodiment of the invention discloses a preparation method of polybutadiene, specifically:

[0034] Polybutadiene is polymerized in an organic solvent under the action of a cocatalyst and a cobalt complex having the structure of formula (I) to obtain polybutadiene;

[0035]

[0036] Among them, R 1 and R 2 each independently selected from hydrogen or C1~C10 alkyl;

[0037] R 3 is hydrogen, halogen or C1~C10 alkyl;

[0038] X is halogen.

[0039] In the above polymerization reaction process, the cobalt complex catalyzes the polymerization of butadiene alone and has catalytic activity, but after adding a cocatalyst, the cobalt complex and the cocatalyst jointly catalyze the polymerization of butadiene, and the catalyst has a higher catalytic activity. active. The cocatalyst is preferably diethylsesquialuminum, triisobutylaluminum, triethylaluminum or methylalkoxyaluminum, more preferably diethylsesquialuminum. The molar ratio of aluminum in the cocatalyst to...

Embodiment 1

[0062] Weigh 5g (30mmol) of pyridine-2,6-dicarboxylic acid into a 50mL round-bottomed flask, add 30mL of thionyl chloride, reflux for 24h to form a homogeneous phase, and drain the excess thionyl chloride under reduced pressure to obtain a pale pink Pyridinedicarboxylic acid chloride was directly used in the next reaction.

[0063] Weigh 8.11g (60mmol) 2,4,6-trimethylaniline and 8.36g (60mmol) triethylamine and dissolve in 50ml CH 2 Cl 2 In, weigh 6.1g (30mmol) pyridinedicarboxylic acid chloride and dissolve in 20mL CH 2 Cl 2 In, pyridine dicarbonyl chloride / CH 2 Cl 2 Solution to substituted aniline / CH 2 Cl 2 Added dropwise in the middle, after reflux for 4 hours, use 100ml water and 100ml1.5M Na respectively 2 CO 3 The solution was washed, and the lower layer of CH was obtained with a separatory funnel 2 Cl 2 solution, adding MgSO 4 Dry overnight, filter and suck dry, then recrystallize with toluene, filter and dry to obtain the product (5b), the yield is 91%. The...

Embodiment 2

[0069] Weigh 5g (30mmol) of picidinedicarboxylic acid into a 50mL round-bottomed flask, add 30mL of thionyl chloride, reflux for 24h to form a homogeneous phase, and drain the excess thionyl chloride under reduced pressure to obtain pale pink pyridinedicarboxylic acid chloride, directly used in the next reaction.

[0070] Weigh 9.3g (60mmol) 4-chloro-2,6-dimethylaniline and 8.36ml (60mmol) triethylamine and dissolve in 50mL CH 2 Cl 2 In, weigh 6.1g (30mmol) pyridinedicarboxylic acid chloride and dissolve in 20mL CH 2 Cl 2 In, pyridine dicarbonyl chloride / CH 2 Cl 2 Solution to substituted aniline / CH 2 Cl 2 Added dropwise in the middle, after reflux for 4 hours, with 100mL water and 100mL1.5M Na 2 CO 3 The solution was washed, and the lower layer of CH was obtained with a separatory funnel 2 Cl 2 solution, adding MgSO 4 Dry overnight, filter and suck dry, then recrystallize with toluene, filter and dry to obtain the product (9b). Yield 83.5%. The product (9b) was an...

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Abstract

The invention provides a preparation method of a polybutadiene, which comprises the following steps: under the actions of a cocatalyst and a cobalt complex disclosed as Formula (I), carrying out polymerization reaction on butadiene in an organic solvent to obtain polybutadiene. In the polybutadiene preparation process, the cobalt complex disclosed as Formula (I) and the cocatalyst are used as the catalyst, the electrophilic chlorine atoms introduced into the ligand structure of the cobalt complex increase the electropositivity of the active center cobalt atom, thereby endowing the butadiene monomer with larger coordination space; and thus, the cobalt complex has higher catalytic activity, so the polybutadiene has higher yield. The experiment proves that the yield of polybutadiene is 72-97% in the butadiene catalytic polymerization process of the cobalt complex.

Description

technical field [0001] The invention relates to the technical field of polymers, in particular to a preparation method of polybutadiene. Background technique [0002] Synthetic rubber is an extremely important synthetic material that is used in a wide range of applications in automotive, construction, medical and other fields. With the development of synthetic rubber industry, polybutadiene rubber has been widely used in the production of rubber products such as tires, tapes, hoses and rubber shoes due to its advantages of good elasticity, strong wear resistance, low heat generation, and small hysteresis loss. Applications. Polybutadiene rubber is a general-purpose synthetic rubber obtained by polymerizing 1,3-butadiene as a monomer. [0003] So far, the catalytic systems commonly used to catalyze the polymerization of butadiene in the prior art include LiR, TiCl 4 / I 2 / Al i Bu 3 , Co (OCOR) 2 / H 2 O / AlEt 2 Cl, Ni (OCOR) 2 / BF 3 ·OEt 2 / AlEt 3 , Nd(OCOR) 3 / Et...

Claims

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Application Information

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IPC IPC(8): C08F136/06C08F4/70C08F2/06C07F15/06
Inventor 张学全刘恒白晨曦张春雨蔡洪光毕吉福代全权那丽华
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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