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Preparation method of 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 aluminoxane preparation, unsatisfactory preparation, difficulty in preparing initiator system, etc., so as to improve polymerization efficiency and reduce energy consumption , The effect of simplifying the production process

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

[0004] However, the main problem of the solution polymerization method is that it is necessary to adopt a highly active initiator system adapted to the solution polymerization system to obtain high molecular weight products.
Although the initiation efficiency and polymerization rate of the initiator system disclosed in US6403747 have been improved to a certain extent, it is still unsatisfactory in the actual operation process, and the preparation of the initiator system is relatively difficult, especially the preparation technology of aluminoxane is very high.

Method used

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  • Preparation method of halogenated polymer
  • Preparation method of halogenated polymer
  • Preparation method of halogenated polymer

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preparation example Construction

[0036] The invention provides a kind of preparation method of halogenated monoolefin-alkylstyrene copolymer, the method comprises the following steps:

[0037](1) Under cationic polymerization conditions, in at least one polymerization solvent, at least one monoolefin and at least one alkylstyrene are contacted with each component in the initiator system to obtain monoolefin-alkylbenzene-containing The solution of ethylene copolymer, described polymerization solvent is selected from alkane, the condition of described contact makes, by weight, the content of the unreacted alkylstyrene in the described solution that contains monoolefin-alkylstyrene copolymer is Not higher than 1000ppm, preferably not higher than 500ppm, more preferably not higher than 200ppm;

[0038] (2) The solution containing the monoolefin-alkylstyrene copolymer obtained in step (1) is contacted with a halogen-containing compound, so that part of the hydrogen atoms in the molecular chain of the monoolefin-al...

experiment example 1

[0118] (1) 0.142g 2,3-dichloro-5,6-dicyano-p-benzoquinone is dissolved in 200g and contains dichloromethane of p-dicumyl chloride (concentration is 0.005mol / L), the obtained The solution was pre-cooled to -85°C, and then 5 mL of a 0.9 mol / L n-hexane solution of ethylaluminum dichloride (EADC) and 4.5 mL of 1.0 mol / L diethyl chloride were sequentially added to the solution The n-heptane solution of aluminum (DEAC) (the molar ratio of EADC to DEAC is 5 / 5), after mixing evenly, put the obtained mixed solution in a cold bath at -85° C. to age for 100 min, thereby obtaining an initiator solution.

[0119](2) Add 800 g of n-hexane pre-cooled to -80 °C, 100 g of isobutylene pre-cooled to -80 °C and 6 g of p-formaldehyde at room temperature (25 °C) in a 2000 mL stainless steel reactor equipped with strong constant speed Base styrene (content 98% by weight), mix well. Add the initiator solution prepared in step (1) dropwise to the reactor. Wherein, the adding amount of the initiator ...

experiment example 2

[0124] The brominated monoolefin-alkylstyrene copolymer was prepared in the same manner as Experimental Example 1, except that in step (1), the aging time was 60 min; in step (2), the polymerization reaction time was 60 min. The experimental results are listed in Table 1.

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Abstract

The invention discloses a preparation method of a halogenated monoolefine-alkyl styrol copolymer. The preparation method comprises the steps that monoolefine shown in the formula II and alkyl styrol shown in the formula III make contact with components in an initiator system in alkane under the condition of cationic polymerization, and the obtained solution containing the halogenated monoolefine-alkyl styrol copolymer makes with a compound containing halogen for a halogenating reaction, wherein the initiator system contains a compound capable of providing protons, lewis acid and an activating agent, and the activating agent is selected from the compound shown in the formula I-1 and the compound shown in the formula I-2. By means of the method, polymerization efficiency can be obviously improved, the higher polymer yield is obtained, the polymer with high molecular weight can be obtained, the solvent replacement process and the polymer redissolution process needed in a slurry polymerization are omitted, and the production process is simplified.

Description

technical field [0001] The invention relates to a preparation method of a halogenated polymer, more specifically, to a preparation method of a halogenated monoolefin-alkylstyrene 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. 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 solution polymer...

Claims

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Application Information

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IPC IPC(8): C08F210/00C08F212/12C08F4/00C08F8/20C08F2/06
Inventor 张雷邱迎昕龚惠勤周新钦张月红
Owner CHINA PETROLEUM & CHEM CORP
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