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Method for preparing polyvinyl ether through cationic polymerization by adopting continuous flow method

A cationic polymerization and polyvinyl ether technology, applied in the field of polymer material synthesis, can solve problems such as difficult stereoselective control, catalyst deactivation, and restrictions on large-scale applications

Active Publication Date: 2022-05-27
UNIV OF SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, these metallocene catalysts are usually easily poisoned by polar groups on the monomers, leading to catalyst deactivation.
Subsequently, late transition metal catalysts appeared for the polymerization of polar vinyl ether monomers, but these methods are difficult to achieve good control of stereoselectivity
At this stage, many researchers use free radical polymerization or cationic polymerization to polymerize vinyl ether monomers, which have great advantages in controlling polymer composition, molecular weight and molecular weight distribution. However, in terms of stereoselectivity still face great challenges
[0003] In the prior art, some catalysts are used to carry out cationic polymerization of vinyl ether at low temperature, but the obtained polymer is only about 70% isotactic
Although the isotacticity of the polymers prepared by some polymerization systems can reach about 90%, there is also the problem of the reverse correlation between the stereoselectivity of the polymer and the concentration of the monomer.
Based on these problems, the large-scale application of cationic polymerization of vinyl ethers is limited.

Method used

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  • Method for preparing polyvinyl ether through cationic polymerization by adopting continuous flow method
  • Method for preparing polyvinyl ether through cationic polymerization by adopting continuous flow method
  • Method for preparing polyvinyl ether through cationic polymerization by adopting continuous flow method

Examples

Experimental program
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Embodiment 1

[0075] In this embodiment, n-hexane is used as the solvent, the flow rate of the solution in the syringe pump is 10mL / h, and the cationic polymerization reaction is carried out at -78°C. The specific process is as follows:

[0076] In the glove box, prepare 20mL of 0.02M TiCl 2 (OAr) 2 (Ar is 2,6-diisopropylphenyl) catalyst in n-hexane solution and draw it into a 20mL syringe A, and then prepare 20mL isobutyl vinyl ether monomer concentration of 0.72M, initiator concentration of 0.01 M. The n-hexane mixed solution with the additive concentration of 0.004M is drawn into another 20mL syringe B. Take the syringes A and B out of the glove box, connect them to a pipeline with an inner diameter of 2 mm, and fix them on the syringe pump respectively. Set the program of the syringe pump so that the liquid flow rate is 10 mL / h, and then put the pipeline on the tube that has been cooled to a temperature of 10 mL / h. In a low temperature ethanol bath at -78°C, the solutions in syringes ...

Embodiment 2

[0083] Adopt the same preparation method as in Example 1, the only difference is that the monomer in Example 2 is n-butyl vinyl ether, and the relevant test results are shown in Table 1.

Embodiment 3

[0085] The same preparation method as in Example 1 was adopted, except that the vinyl ether monomer in Example 3 was cyclohexyl vinyl ether. The relevant test results are shown in Table 1.

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Abstract

The invention provides a method for preparing polyvinyl ether through cationic polymerization by adopting a continuous flow method, which comprises the following steps: providing an injector A and an injector B, filling a cationic polymerization catalyst solution in the injector A, filling a vinyl ether monomer and an initiator solution in the injector B, and optionally comprising an additive; the method comprises the following steps: respectively connecting an injector A and an injector B to two injection pumps, controlling the flow rate of liquid through the injection pumps, injecting solutions in the injector A and the injector B into a mixer, mixing the solutions in the mixer, enabling the mixed solutions to flow into a tubular reactor, and carrying out cationic polymerization reaction while continuously flowing in the tubular reactor to obtain the product polyvinyl ether.

Description

technical field [0001] The present disclosure belongs to the field of polymer material synthesis, and in particular relates to a method for preparing polyvinyl ether by cationic polymerization using a continuous flow method. Background technique [0002] The stereoregularity of polymers has a very significant impact on the properties of polymeric materials, therefore, the stereoselective polymerization of various types of monomers has been extensively explored over the past few decades, for example, using chirality Metallocene catalysts perform coordination-insertion polymerization of alpha-olefins. However, these metallocene catalysts are usually easily poisoned by the polar groups on the monomers, resulting in catalyst deactivation. Subsequently, late transition metal catalysts have appeared for the polymerization of polar vinyl ether monomers, but these methods are difficult to achieve good stereoselectivity control. At this stage, many researchers use free radical poly...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F116/18C08F116/14C08F130/08C08F2/06C08F4/76
CPCC08F116/18C08F116/14C08F130/08C08F2/06C08F4/76C08F2500/15
Inventor 陈昶乐巴舍尔廖道鸿
Owner UNIV OF SCI & TECH OF CHINA
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