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A cationic polymerization method

A cationic polymerization and proton technology, applied in the field of cationic polymerization, can solve the problems of high technical requirements for aluminoxane preparation, difficult and unsatisfactory preparation of the initiator system, etc., achieve high polymer yield, reduce energy consumption, initiate Efficiency improvement effect

Active Publication Date: 2018-10-16
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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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0082] (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.

[0083]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.

[0084] (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...

Embodiment 2

[0089] Adopt the method identical with embodiment 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.

[0090] Polymer yields are listed in Table 1 along with the degree of unsaturation, molecular weight and molecular weight distribution index of the resulting polymers.

Embodiment 3

[0092] Adopt the method identical with embodiment 1 to carry out polymerization, difference is, in step (1), aging time is 30min, and in the initiator solution that obtains, by weight, the concentration of tetrachloro-p-benzoquinone is 800ppm; Step ( 2), the amount of the initiator solution added was 10mL, the temperature in the reactor was kept in the range of -85°C to -90°C during the dripping process of the initiator solution and the polymerization reaction process, and the polymerization reaction time was 15min.

[0093] Polymer yields are listed in Table 1 along with the degree of unsaturation, molecular weight and molecular weight distribution index of the resulting polymers.

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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 present invention relates to a cationic polymerization method. 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 solution polymerization method is more in line with the environmental protection requirements than the slur...

Claims

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Application Information

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Patent Type & Authority Patents(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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