Preparing 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 the preparation of aluminoxane, difficult and unsatisfactory preparation of the initiator system, etc., 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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  • Abstract
  • Description
  • Claims
  • Application Information

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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 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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  • Preparing method of halogenated polymer
  • Preparing method of halogenated polymer
  • Preparing method of 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, in at least one polymerization solvent, at least one monoolefin and at least one conjugated diene are contacted with each component in the initiator system to obtain monoolefin-conjugated diolefin A solution of an olefin copolymer, the polymerization solvent being selected from alkanes;

[0036] (2) removing unreacted monomers in the solution containing the monoolefin-conjugated diene copolymer to obtain a solution after monomer removal;

[0037] (3) The monomer-removed solution is contacted with a halogen-containing compound, so that part of the hydrogen atoms in the molecular chain of the monoolefin-conjugated diene copolymer are replaced by halogen atoms.

[0038] In the present invention, "optionally" means including or not including, and "at least one" means one or...

experiment example 1

[0108] (1) Dissolve 0.0662g of chloro-p-benzoquinone in 80g of dichloromethane solution containing HCl (concentration: 0.0036mol / L), pre-cool the resulting solution to -80°C, and then sequentially add 2.6 mL of n-hexane solution of 0.9 mol / L ethylaluminum dichloride (EADC) and 1 mL of n-heptane solution of 1.0 mol / L diethylaluminum chloride (DEAC), after mixing evenly, put The resulting mixed solution was aged at -80° C. for 80 min to obtain an initiator solution. Wherein, by weight, the content of chloro-p-benzoquinone in the initiator solution is 800ppm.

[0109] (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 0.5 mL of isoprene pre-cooled to -20°C was mixed uniformly to obtain a monomer solution. Add 10mL of the initiator solution prepared in step (1) to the monomer solution, mix evenly and let it stand for 30 minute...

experiment example 2

[0112] Adopt the same method as Experimental Example 1 to carry out the polymerization, the difference is that in step (2), during the dropwise addition of the initiator solution and the polymerization reaction, the temperature of the cold bath is controlled to be in the range of -40°C to -50°C Inside, the amount of initiator solution was 15mL, and the polymerization reaction time was 50min.

[0113] The weight of the obtained polymer was measured, the polymer yield was calculated, and the molecular weight, molecular weight distribution index and degree of unsaturation of the polymer were measured, and the results are listed in Table 1.

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Abstract

The invention discloses a preparing method of a halogenated monoolefine-conjugated diene copolymer. The method comprises the steps that under the cationic polymerization condition, monoolefine shown in the formula II in the description and conjugated diene shown in the formula III in the description make contact with all components in an initiator system in alkane, unreacted monoolefine and conjugated diene in an obtained solution containing the monoolefine-conjugated diene copolymer are removed, then the solution makes contact with a compound including halogen, and a halogenating reaction is carried out, wherein the initiator system includes a compound capable of providing protons, lewis acid and an activating agent selected from a compound shown in the formula I-1 and a compound shown in the formula I-2. By means of the method, the polymerizing efficiency can be remarkably improved, and a higher polymer yield can be achieved; the polymer with a high molecular weight can be obtained. According to the method, the processes of solvent replacement and polymer redissolution necessary in a slurry polymerizing method are omitted, and the production technology is simplified.

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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Patent Type & Authority Applications(China)
IPC IPC(8): C08F210/00C08F236/04C08F8/20C08F2/06C08F4/00
Inventor 邱迎昕张雷龚惠勤张月红孟伟娟周新钦
Owner CHINA PETROLEUM & CHEM CORP
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