Conjugated diene polymer, preparation method thereof, polybutadiene and polyisoprene

A technology of conjugated diene and polymer, which is applied in the field of conjugated diene polymer and its preparation and polybutadiene and polyisoprene, which can solve the problems of increasing the residence time of the amount of initiator added, and achieve a single The effects of fast body conversion rate, short polymerization time and wide molecular weight distribution

Active Publication Date: 2017-11-10
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0010] The purpose of the present invention is to overcome the high temperature continuous polymerization process in the prior art to synthesize conjugated diene polymers. In order to obtain a wide molecular weight distribution, it is necessary to compensate for the monomer conversion rate by increasing the amount of initiator added or by prolonging the residence time of the material. Insufficient shortcoming, provide a kind of conjugated diene polymer and preparation method thereof and polybutadiene and polyisoprene

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  • Conjugated diene polymer, preparation method thereof, polybutadiene and polyisoprene

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preparation example Construction

[0020] The invention provides a method for preparing a conjugated diene polymer. The method is to carry out continuous conjugated diene polymerization reaction in a continuous polymerization reaction device comprising a plurality of series reactors, comprising: under anionic polymerization conditions, The reaction material containing the first part of conjugated diene monomer, solvent, gel inhibitor, polarity regulator and monoorganolithium initiator is continuously introduced into the continuous polymerization from the first tank of the continuous polymerization reaction device The reaction device carries out a continuous polymerization reaction; the second part of the conjugated diene monomer is introduced into the final kettle of the continuous polymerization reaction device, and the second continuous polymerization reaction is carried out in the final kettle, and the maximum temperature of the second continuous polymerization reaction is 110 ~160°C, preferably 115-120°C.

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Embodiment 1

[0059] This example illustrates the preparation of the polybutadiene of the present invention.

[0060] Three 5-liter polymerization reactors connected in series are continuous polymerization reaction devices.

[0061] In the continuous polymerization reaction device, under the protective atmosphere of high-purity nitrogen, the residence time of the reaction materials in the three single tanks is 15 minutes respectively, and the reaction pressure of the conjugated diene polymerization is controlled at 0.6±0.05MPa:

[0062] (1) Control the temperature in the first kettle, the second kettle and the last kettle to 80±1°C, and add the reaction material from the bottom of the first kettle: mixed solvent (a mixture of cyclohexane and n-hexane in a weight ratio of 88:12) 11340g / h, 1,3-butadiene 3024g / h, n-butyllithium 37.8mmol / h, ethyl tetrahydrofurfuryl ether 2.27g / h and 1,2-butadiene 1.134g / h, once Continuous polymerization reaction, the maximum temperature of one continuous polym...

Embodiment 2

[0074] This example illustrates the preparation of the polybutadiene of the present invention.

[0075] Three 5-liter polymerization reactors connected in series are continuous polymerization reaction devices.

[0076] In the continuous polymerization reaction device, under the protective atmosphere of high-purity nitrogen, the residence time of the reaction materials in the three single tanks is 20 minutes respectively, and the reaction pressure of the conjugated diene polymerization is controlled at 0.7±0.05MPa.

[0077] (1) Control the temperature in the first kettle, the second kettle and the last kettle to 90±1°C, add the reaction materials from the bottom of the first kettle: 1,3-butadiene 1701g / h, cyclohexane 9072g / h, normal Butyllithium 9.07mmol / h, ethyl tetrahydrofurfuryl ether 2.72g / h and 1,2-butadiene 0.45g / h, conduct a continuous polymerization reaction, the maximum temperature of a continuous polymerization reaction is 90°C;

[0078] (2) When the maximum temperat...

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Abstract

The invention relates to the field of conjugated diene polymer preparation, and provides a conjugated diene polymer, a preparation method thereof, polybutadiene and polyisoprene. The preparation method is a continuous polymerization reaction of conjugated diene in a continuous polymerization reaction device comprising a plurality of reaction kettles which are connected in series, and comprises the following steps: introducing reaction materials containing a first-part conjugated diene monomer, a solvent, a gel inhibitor, a polarity modifier and a single organic lithium initiator from a first kettle of the continuous polymerization reaction device under anionic polymerization conditions to the continuous polymerization reaction device and performing first continuous polymerization reaction; and introducing a second-part conjugated diene monomer to a last kettle of the continuous polymerization reaction device, and performing secondary continuous polymerization reaction in the last kettle, wherein the highest temperature of the secondary continuous polymerization reaction is 110-160 DEG C. According to the invention, the conjugated diene polymer with a relatively-wide molecular weight distribution can be obtained by using the method provided in the invention.

Description

technical field [0001] The present invention relates to the field of preparation of conjugated diene polymers, in particular, to a method for preparing conjugated diene polymers by continuous polymerization, and the conjugated diene polymers prepared by the method, and specifically, the application Polybutadiene obtained by polymerizing 1,3-butadiene by the method, and polyisoprene obtained by polymerizing isoprene by applying the method. Background technique [0002] Generally speaking, when the content of the high molecular weight fraction of the polymer is high, the strength of the rubber is high, but the processing performance is poor; when the content of the low molecular weight fraction is high, although the content of the low molecular weight fraction is high, the strength of the rubber becomes low, which will affect its performance. . In addition, during the vulcanization process, the extremely low molecular weight part is generally difficult to vulcanize, which mak...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F136/08C08F136/06C08F2/06C08F2/38
CPCC08F136/06C08F136/08C08F2/06C08F2/38
Inventor 吕万树徐林王雪胡保利邰峰董新民赵晓冬
Owner CHINA PETROLEUM & CHEM CORP
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