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Cationic polymerization method

A cationic polymerization and proton technology, applied in the field of cationic polymerization, can solve problems such as unsatisfactory, difficult preparation of initiator system, high technical requirements for the preparation of aluminoxane, etc., to reduce energy consumption, improve initiation efficiency, high polymer production rate effect

Active Publication Date: 2016-11-23
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • 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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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0082] (1) Dissolve 0.133 g of tetrachloro-p-benzoquinone in 66.5 g of dichloromethane solution to obtain a tetrachloro-p-benzoquinone solution. By weight, the concentration of tetrachloro-p-benzoquinone in the solution is 2000 ppm.

[0083] At -80℃, add 20mL of dichloromethane solution containing HCl (concentration of 0.0044mol / L) and 1.5mL of ethyl aluminum dichloride (concentration of 0.9mol / L) pre-cooled to -80℃ into 60mL shofar. L) The n-hexane solution and 1 mL of the aforementioned tetrachloro-p-benzoquinone solution are mixed uniformly and aged at -80° C. for 15 minutes to obtain an initiator solution. By weight, the concentration of tetrachloro-p-benzoquinone in the initiator solution is 100 ppm.

[0084] (2) In a 500mL glass reactor equipped with strong constant speed stirring, add 100mL of monochloromethane precooled to -60℃, 80mL of n-hexane precooled to -60℃, and 32mL of isobutylene precooled to -60℃. And 1mL of isoprene pre-cooled to -20°C and mix well. The initiat...

Embodiment 2

[0089] The polymerization was carried out using the same method as in Example 1, except that in the initiator solution obtained in step (1), the concentration of tetrachloro-p-benzoquinone was 400 ppm by weight; in step (2), the concentration of the initiator solution The addition amount is 20 mL, the temperature in the reactor is maintained in the range of -60°C to -65°C during the dropping process of the initiator solution and the polymerization reaction, and the polymerization reaction time is 15 minutes.

[0090] The polymer yield and the degree of unsaturation, molecular weight and molecular weight distribution index of the obtained polymer are listed in Table 1.

Embodiment 3

[0092] The polymerization was carried out using the same method as in Example 1, except that in step (1), the aging time was 30 minutes, and the obtained initiator solution had a concentration of 800 ppm by weight of tetrachloro-p-benzoquinone; step ( In 2), the addition amount of the initiator solution is 10 mL, the temperature in the reactor is maintained in the range of -85°C to -90°C during the dropping process of the initiator solution and the polymerization reaction, and the polymerization reaction time is 15 minutes.

[0093] The polymer yield and the degree of unsaturation, molecular weight and molecular weight distribution index of the obtained polymer are listed in Table 1.

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Abstract

The invention discloses a cationic polymerization method. The method includes the step that under the solution polymerization condition, monoolefine shown in the formula II and conjugated diene shown in the formula III make contact with all components in an initiator system in a mixed solvent composed of alkane and haloalkane, wherein the initiator system contains a compound capable of providing protons, lewis acid and an activating agent, and the activating agent is selected from a compound shown in the formula I-1 and a compound shown in the formula I-2. Compared with a pure H+ / lewis acid initiator system, initiation efficiency of the method is obviously improved, and the higher polymer yield can be obtained at higher polymerization speed. Polymers with different molecular weights can be obtained under different polymerization conditions by adjusting the content and the variety of the activating agent in the initiator system. Besides, the method can achieve polymerization at higher temperature and effectively reduce energy consumption in the polymerization reaction process. Please see the formulas in the description.

Description

Technical field [0001] The invention relates to a cationic polymerization method. Background technique [0002] At present, the slurry polymerization method using monochloromethane as a 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 a high molecular weight and good processing performance. [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 processing performance, 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 polymerization method is more environmentally friendly than the slurry polymerization meth...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F210/12C08F236/08C08F4/54C08F2/06
Inventor 邱迎昕齐海英龚惠勤张雷周新钦
Owner CHINA PETROLEUM & CHEM CORP
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