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Preparation methods of polyisoprene low polymer, branched modifier and branched rare earth isoprene rubber

A technology of polyisoprene and isoprene is applied in the field of polyisoprene branching agent to achieve the effects of reducing dynamic viscosity, facilitating post-processing and simple preparation process

Active Publication Date: 2019-10-08
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to solve the existing problems in the preparation process of branching agents for isoprene rubber, and to provide a preparation method for polyisoprene oligomers, branching modifiers and branched rare earth isoprene rubber , the polyisoprene oligomer is used as a branching agent for rare earth isoprene rubber, the preparation process is simpler and does not bring impurities such as water and ethanol into the polymerization of isoprene rubber, and the branched rare earth isoprene rubber obtained has better viscosity reduction

Method used

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  • Preparation methods of polyisoprene low polymer, branched modifier and branched rare earth isoprene rubber
  • Preparation methods of polyisoprene low polymer, branched modifier and branched rare earth isoprene rubber
  • Preparation methods of polyisoprene low polymer, branched modifier and branched rare earth isoprene rubber

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preparation example Construction

[0044] The present invention can also provide a preparation method of the polyisoprene oligomer of the present invention, comprising: under the presence of an inert atmosphere and an alkyllithium initiator, the isoprene in the oligomerization solvent is oligomerized reaction. The conditions therein are as described above.

[0045] The third aspect of the present invention provides a method for preparing branched rare earth isoprene rubber, comprising:

[0046] In the presence of an inert atmosphere and a rare earth polymerization catalyst, the isoprene monomer in the polymerization solvent and the branched modifier of the present invention are subjected to polymerization reaction.

[0047] In the present invention, preferably, the concentration of the isoprene monomer in the polymerization solvent may be 8-20% by weight.

[0048] In the present invention, preferably, the branched modifier contains the aforementioned polyisoprene oligomer of the present invention, and the pol...

Embodiment A1-A3

[0078] Mark the 4 polymerization bottles as A0, A1, A2, A3, vacuumize them and bake them at high temperature, then fill them with high-purity nitrogen, and repeat this three times;

[0079] Add the same amount of hexane and isoprene into each polymerization bottle (the content of isoprene is 0.10 g isoprene / mL hexane, referred to as Ip). Take the polymerization bottle A0 as the trash-killing bottle, add 4-vinylpyridine as the indicator, and use nBuLi to calibrate the amount of impurities in the solution to obtain the amount of trash-killing.

[0080] Initiator nBuLi (abbreviated as Li) was added to polymerization bottles A1, A2 and A3 after deducting the amount of impurities. The metering of initiator nBuLi was according to the data of Li / Ip in Table 1. According to the oligomerization conditions in Table 1, the isoprene in the polymerization bottles A1, A2, and A3 is subjected to an oligomerization reaction, and after the reaction is completed, metered triisobutylaluminum (Al...

preparation example 1

[0091] Preparation of rare earth polymerization catalysts.

[0092] Add a certain amount of neodymium neodecanoate (abbreviation: Nd) and triisobutylaluminum (abbreviation: Al) to the catalyst preparation device under the protection of nitrogen, Al / Nd (mol) = 30:1; After 0.5h, add a certain amount of diethylaluminum chloride (abbreviation: Cl), Cl / Nd (mol) = 2.5:1, and continue to age at 30°C for 1h.

[0093] The obtained catalyst aging solution is designated as Cat-1.

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Abstract

The invention relates to the field of polyisoprene branching agents, and discloses preparation method of a polyisoprene low polymer, a branched modifier and branched rare earth isoprene rubber. According to the polyisoprene low polymer, the number-average molecular weight of the low polymer is 3000-30000, the content of a cis-1, 4 structure unit is 65-75wt%, the content of a trans-1, 4 structure unit is 18-28wt%, and the content of a 3, 4 structure unit is 6-12wt% in a structure of the low polymer. The polyisoprene low polymer can be prepared into the branched modifier by the method, a preparation process is simple, water or ethyl alcohol serving as a terminating agent is omitted, the polyisoprene low polymer is further used for preparing the rare earth isoprene rubber, the dynamic viscosity of the polymer can be effectively reduced, and post-processing of the polymer is facilitated.

Description

technical field [0001] The invention relates to the field of polyisoprene branching agents, in particular to a preparation method of polyisoprene oligomers, branching modifiers and branched rare earth isoprene rubber. Background technique [0002] The structure and properties of isoprene rubber are similar to those of natural rubber. It is a general-purpose synthetic rubber with excellent comprehensive properties and is mainly used in the production of tires. In recent years, due to the good wet skid resistance and low rolling resistance of rare earth isoprene rubber, while the wear resistance can still maintain a good level, it has attracted much attention from tire companies in the world. [0003] However, the isoprene rubber prepared by rare earth-catalyzed isoprene polymerization has high molecular weight, high linearity, narrow molecular weight distribution, high solution viscosity during the polymerization process, and poor processability, which limit its industrializa...

Claims

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Application Information

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IPC IPC(8): C08F236/08C08F4/48
CPCC08F236/08C08F4/461
Inventor 孙伟赵姜维徐林李建成邵明波唐正伟
Owner CHINA PETROLEUM & CHEM CORP
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