Method for preparing halogenated polymer

A compound and copolymer technology, which is applied in the field of preparation of halogenated polymers, can solve the problems of high technical requirements for the preparation of aluminoxane, unsatisfactory, difficult preparation of initiator system, etc., to achieve high polymer yield and reduce energy Consumption, the effect of raising efficiency

Active Publication Date: 2016-11-23
CHINA PETROLEUM & CHEM CORP +1
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Problems solved by technology

Although the initiation efficiency and polymerization rate of the initiator system disclosed in US6403747 have been improved to a certain extent, it is still unsatisfacto

Method used

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  • Method for preparing halogenated polymer
  • Method for preparing halogenated polymer

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preparation example Construction

[0034] The invention provides a kind of preparation method of halogenated monoolefin-conjugated diene copolymer, the method comprises the following steps:

[0035] (1) Under cationic polymerization conditions, at least one monoolefin and at least one conjugated diene are contacted with each component in the initiator system in a polymerization solvent to obtain monoolefin-conjugated diene copolymer a solution, the polymerization solvent is composed of at least one first polymerization solvent and at least one second polymerization solvent, the first polymerization solvent is selected from halogenated alkanes, and the second polymerization solvent is selected from alkanes;

[0036] (2) Replace the halogenated alkane in the solution containing the monoolefin-conjugated diene copolymer with at least one replacement solvent and remove unreacted monomers to obtain a replacement solvent containing the monoolefin-conjugated diene copolymer After the solution, the replacement solvent ...

experiment example 1

[0110] (1) 0.133g of chloro-p-benzoquinone was dissolved in 66.5g of dichloromethane solution to obtain a solution of chloro-p-benzoquinone. By weight, in this solution, the concentration of chloro-p-benzoquinone is 2000ppm.

[0111]At -80°C, 20mL of dichloromethane solution containing HCl (concentration: 0.0044mol / L), 1.5mL containing dichloroethylaluminum (concentration: 0.9mol / L) and L) n-hexane solution and 1 mL of the above-mentioned tetrachloro-p-benzoquinone solution were mixed uniformly and then aged at -80° C. for 15 minutes to obtain an initiator solution. By weight, in the initiator solution, the concentration of chloro-p-benzoquinone is 100ppm.

[0112] (2) Add 100 mL of methylene chloride pre-cooled to -60 °C, 80 mL of n-hexane pre-cooled to -60 °C, and 32 mL of isobutylene pre-cooled to -60 °C in a 500 mL glass reactor equipped with strong constant-speed stirring and 1 mL of isoprene pre-cooled to -20°C, and mix well. Add the initiator solution prepared in ste...

experiment example 2

[0117] Adopt the method identical with Experimental Example 1 to carry out polymerization, difference is, in the initiator solution that step (1) obtains, by weight, the concentration of tetrachloro-p-benzoquinone is 400ppm; In step (2), the initiator solution The addition amount was 20 mL, the temperature in the reactor was kept in the range of -60° C. to -65° C. during the dripping of the initiator solution and the polymerization reaction, and the polymerization reaction time was 15 minutes. The experimental results are listed in Table 1.

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Abstract

The invention discloses a method for preparing a halogenated monoolefine-conjugated diene copolymer. The method comprises the steps that under the condition of cationic polymerization, monoolefine shown as the formula I, conjugated diene shown as the formula III and all components in an initiator system are in contact in a mixed solvent of alkane and haloalkane, alkane is used for displacement and polymerization to obtain haloalkane in the solution, meanwhile, unreacted monomers are separated out and then are in contact with a halogen containing compound for a halogenating reaction, the initiator system contains a compound, lewis acid and an activating agent capable of providing protons, and the activating agent is selected from a compound shown as the formula I-1 and a compound shown as the formula I-2. According to the method, the polymerization efficiency can be obviously improved, and the higher polymer yield can be obtained. The polymer with the high molecular weight can be obtained; meanwhile, the polymer redissolving process necessary for a slurry polymerization method is omitted, and the production process is simplified. The formula is shown in the specification.

Description

technical field [0001] The invention relates to a preparation method of a halogenated polymer, more particularly, to a preparation method of a halogenated monoolefin-conjugated diene copolymer. Background technique [0002] At present, the slurry polymerization method using dichloromethane as diluent is widely used in the world to produce butyl rubber. The main reason is that the slurry polymerization method has high production efficiency, and the product has high molecular weight and good processability. [0003] Compared with the slurry polymerization method, the solution polymerization method has no obvious advantages in these aspects, especially the products obtained by the solution polymerization method have low molecular weight and poor processability, so it is difficult to compete with the products obtained by the slurry polymerization method in the market . However, the development space of the solution polymerization method is relatively broad. For example, the sol...

Claims

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Application Information

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IPC IPC(8): C08F210/12C08F4/54C08F8/22
Inventor 邱迎昕孟伟娟周新钦张雷龚惠勤张月红
Owner CHINA PETROLEUM & CHEM CORP
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