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Preparation method of halogenated polymer

A compound and copolymer technology, applied in the field of preparation of halogenated polymers, can solve the problems of difficulty in preparing an initiator system, unsatisfactory, high technical requirements for aluminoxane preparation, etc. The effect of improving polymerization efficiency

Active Publication Date: 2016-11-23
CHINA PETROLEUM & CHEM CORP +1
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  • Description
  • Claims
  • Application Information

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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

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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-alk...

experiment example 1

[0115] (1) 0.0532g 2,3-dichloro-5,6-dicyano-p-benzoquinone is dissolved in 66.3g and contains HCl (concentration is 0.0037mol / L) in the dichloromethane solution, the solution obtained is pre- Cool to -85°C, and then sequentially add 3.2 mL of 0.9 mol / L ethylaluminum dichloride (EADC) n-hexane solution and 1.2 mL of 1.0 mol / L diethylaluminum chloride to the solution (DEAC) n-heptane solution, after mixing evenly, place the obtained mixed solution in a cold bath at -85° C. to age for 100 min, thereby obtaining an initiator solution. Wherein, by weight, the content of 2,3-dichloro-5,6-dicyano-p-benzoquinone in the initiator solution is 770ppm.

[0116] (2) Place a 250mL three-necked flask in a low-temperature cooling bath whose temperature is controlled from -80°C to -85°C, and add 85mL of n-hexane cooled to -80°C, 15mL of isobutylene cooled to -80°C and 0.62 mL of normal temperature (25° C.) p-methylstyrene (98% by weight) was mixed uniformly to obtain a monomer solution. Add ...

experiment example 2

[0120] Polymerization was carried out in the same manner as in Experimental Example 1, except that diethylaluminum chloride was not used in step (1), and diethylaluminum chloride was replaced by ethylaluminum dichloride in an equimolar amount. 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, and the halogenated monoolefine-alkyl styrol copolymer is obtained, 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): C08F210/10C08F212/12C08F4/54
Inventor 邱迎昕龚惠勤张月红孟伟娟周新钦张雷
Owner CHINA PETROLEUM & CHEM CORP
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