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Cationic polymerization method

A cationic polymerization and carbocation technology, which is applied in the field of cationic polymerization, can solve problems such as unsatisfactory, high technical requirements for the preparation of aluminoxane, difficulty in preparing the initiator system, etc., and achieve reduced energy consumption and high polymer yield , leading to the effect of improving efficiency

Active Publication Date: 2016-11-23
CHINA PETROLEUM & CHEM CORP +1
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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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preparation example 1

[0075] Preparation Example 1: Synthesis of 2-chloro-2,4,4-trimethylpentane (TMPCl)

[0076] Place a 250mL three-necked round-bottom flask in an ice-water bath, and then add 30mL of 2,4,4-trimethyl-1-pentene and 30mL of dichloromethane. Under the condition of continuously feeding dry hydrogen chloride gas, the reaction was carried out for 5h. The mixture obtained by the reaction was neutralized with sodium bicarbonate, then anhydrous magnesium sulfate was added to the solution, and then filtered, the liquid mixture was collected, and vacuum distillation was carried out to collect the fraction at 44°C (2.1332kPa) (yield: 70 % by weight, its purity was determined to be 93% by gas chromatography analysis). After characterization, it was confirmed that the fraction was 2-chloro-2,4,4-trimethylpentane. in, 1 H-NMR (δ, ppm): 1.06(-C(CH 3 ) 3 ), 1.67(-C(CH 3 ) 2 Cl), 1.88(-CH 2 -).

preparation example 2

[0077] Preparation Example 2: Synthesis of Dicumyl Chloride

[0078] Put a 500mL three-necked round-bottomed cauldron equipped with bottomed inlet and outlet pipes and a magnetic stirring device in an ice-water bath, and then add 8g of p-dicumyl alcohol and 10g of CaCl 2 and 100 g of dichloromethane. Continuously feed dry hydrogen chloride gas into the three-necked flask, and stir and react for 10 hours. After the reaction was completed, it was filtered to obtain a clear solution. Hydrogen chloride and methylene chloride were removed in vacuo to obtain 9.1 g of colorless needle crystals (yield: 96% by weight). Dissolve the obtained needle-shaped crystals in 50 mL of n-hexane, filter to remove insoluble impurities, cool the remaining liquid phase to -20°C to -30°C, crystallize with stirring, separate the precipitated crystals from the mother liquor, and collect the crystals. The crystal was determined to be p-dicumyl chloride through characterization. in, 1 H-NMR (δ, ppm): ...

preparation example 3

[0079] Preparation Example 3: Synthesis of p-dicumyl bromide

[0080] p-Dicumyl bromide was prepared in a method similar to Preparation Example 2, except that hydrogen chloride gas was replaced by hydrogen bromide gas. in, 1 H-NMR (δ, ppm): 2.11 7.06 (phenyl).

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Abstract

The invention discloses a cationic polymerization method. The method comprises the following steps that on the solution polymerization condition, monoolefine shown in the formula II and conjugated diene shown in the formula II make contact with components in an initiator system in a polymerization solvent, the initiator system contains compounds capable of providing carbocation, lewis acid and an activating agent, 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 simple C+ / lewis acid initiator system, the initiating efficiency of the method is remarkably improved, and the higher polymer yield can be obtained at the higher polymerization rate; polymers of different molecular weights can be obtained on different polymerization conditions by adjusting the content and varieties of the activating agent in the initiator system; in addition, the method can perform polymerization under the higher temperature, and energy consumption in the polymerization reaction process is effectively lowered.

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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IPC IPC(8): C08F210/12C08F236/08C08F4/54C08F2/06
Inventor 龚惠勤张雷张月红邱迎昕周新钦徐宏德
Owner CHINA PETROLEUM & CHEM CORP
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