Preparation method of halogenated polymer

A compound and copolymer technology, applied in the field of preparation of halogenated polymers, can solve the problems of difficult and unsatisfactory preparation of initiator system, and high technical requirements for the preparation of aluminoxane, so as to reduce energy consumption, improve initiation efficiency, Effect of High Polymer Yield

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 unsatisfacto

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  • Preparation method of halogenated polymer
  • Preparation 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, at least one monoolefin and at least one conjugated diene are contacted with each component in the initiator system in a polymerization solvent to obtain a monoolefin-conjugated diene copolymer containing a solution, the polymerization solvent is composed of at least one first polymerization solvent and at least one second polymerization solvent, the first polymerization solvent is selected from halogenated alkanes, and the second polymerization solvent is selected from alkanes;

[0036] (2) Replace the halogenated alkane in the solution containing the monoolefin-conjugated diene copolymer with at least one replacement solvent and remove unreacted monomers to obtain a replacement solvent containing the monoolefin-conjugated diene copolymer After the solution, the replace...

preparation example 1

[0107] Preparation Example 1: Synthesis of 2-chloro-2,4,4-trimethylpentane (TMPCl)

[0108] A 250 mL round-bottomed three-neck flask was placed in an ice-water bath, and then 30 mL of 2,4,4-trimethyl-1-pentene and 30 mL of dichloromethane were added. 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

[0109] Preparation Example 2: Synthesis of Dicumyl Chloride

[0110] 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): ...

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Abstract

The invention discloses a preparation method of a halogenated monoolefine-conjugated diene copolymer. The method comprises steps as follows: under the cationic polymerization condition, monoolefine shown in a formula II and conjugated diene shown in a formula III are contacted with components in an initiator system in a mixed solvent of alkane and haloalkane, halogenated alkane in a solution obtained through polymerization is replaced with alkane, besides, after unreacted monomers are removed, a product is contacted with a compound containing halogen for a halogenating reaction, the initiator system contains a compound capable of providing carbocation, lewis acid and an activator, and the activator is selected from a compound shown in the formula I-1 and a compound shown in a formula I-2. By means of the method, the polymerization efficiency can be remarkably improved, and the higher polymer yield is obtained; the polymer with higher molecular weight can also be obtained. By means of the method, the polymer redissolving process required with a slurry polymerization method is omitted, and the production process 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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IPC IPC(8): C08F210/12C08F4/54C08F8/22
Inventor 龚惠勤邱迎昕张月红张雷周新钦
Owner CHINA PETROLEUM & CHEM CORP
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