Process method for preparing polyisobutene and polymerization device

A process method and technology for polyisobutylene, applied in the field of preparing polyisobutylene by slurry method, can solve the problems of short residence time, high micro-mixing degree, affecting the polymerization reaction process, etc., so as to reduce operating costs, reduce operating costs, and improve mixing The effect of efficiency

Active Publication Date: 2012-05-23
BEIJING UNIV OF CHEM TECH
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Problems solved by technology

[0005] However, due to the diversity and complexity of polymer polymerization systems, high-gravity technology is not generally applicable to the polymerization processes of different systems, and different technical solutions need to be designed according to the characteristics of different polymerization processes. Polyisobutylene polymerization systems and butyl rubber polymerization systems are both It belongs to the cationic slurry polymerization system, which requires a very high degree of microscopic mixing when the monomer initiates the polymerization
However, butyl rubber has a higher molecular weight, and the polymerization reaction is usually completed instantaneously at a lower temperature (about -100°C), and the reaction rate is faster, while the polymerization reaction of polyisobutylene needs to be carried out at a higher temperature (about -20°C). The rate is lower than that of butyl rubber, and a certain macro-mixing time must be guaranteed to complete the polymerization reaction, otherwise it is difficult to obtain high-quality products
In view of the different characteristics of the above two reaction systems, if only the known hypergravity reaction method and device are used, the residence time of the polymer material in the equipment is too short, and it is difficult to complete the polymerization process of polyisobutylene well.
In addition, studies have shown that after the polymerization raw materials enter the high-gravity rotating bed reactor, there is a phenomenon of local macro-inhomogeneity, and the initial macro-inhomogeneity will reduce to micro-mixing efficiency, which will affect the polymerization process.

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  • Process method for preparing polyisobutene and polymerization device
  • Process method for preparing polyisobutene and polymerization device

Examples

Experimental program
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Effect test

Embodiment 1

[0030] use figure 1 In the setup shown, the high gravity reactor is a rotating packed bed reactor.

[0031] Add 4000ml of the mixed solution A of isobutylene monomer and dichloromethane into storage tank 1, the monomer concentration is 2.0mol / L, mix dichloromethane and AlCl 3 900ml of the mixed liquid B was added to storage tank 2, wherein the initiator was 0.25mol / L. When the materials in storage tank 1 and storage tank 2 were cooled to about -25°C respectively, the two The stock material is sent to the premixing tube in the high-gravity rotary packed bed reactor at a volume ratio of 10:1, and the mixed material is sprayed into the rotor packing layer by the liquid distributor to initiate preliminary polymerization, and the reaction liquid enters through the liquid outlet of the rotary packed bed The reaction was continued for 1 min in a tubular reactor with an aspect ratio of 15:1. Adjust the rotor speed of the supergravity rotating packed bed reactor so that the supergrav...

Embodiment 2

[0033] The technical process and steps are the same as in Example 1, the monomer concentration is 1.5mol / L, the initiator concentration is 0.15mol / L, and the material volume ratio is 5:1. The number average molecular weight M of the obtained polyisobutylene product is n The molecular weight distribution index is 1300, the molecular weight distribution index is 1.95, the yield is 94%, and the α-double bond content at the molecular end is 90%.

[0034] Implementation column 3

[0035] The technical process and steps are the same as in Example 1, the monomer concentration is 1.5mol / L, the initiator concentration is 0.35mol / L, the material volume ratio is 15:1, and the reaction is carried out in a tubular reactor for 10s. The gravity level is 500g. The number average molecular weight M of gained polyisobutylene product n The molecular weight distribution index is 1400, the molecular weight distribution index is 2.02, the yield is 90%, and the α-double bond content at the molecul...

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Abstract

The invention relates to a process method for preparing polyisobutene and a polymerization device. An integrated reactor consisting of a premixer, a supergravity reactor and a tubular reactor is used as a polymerization reactor; a mixed liquid containing a monomer and diluent and a mixed liquid containing initiator and diluent are introduced to the supergravity reactor after being premixed by thepremixer according to a ratio, and cationic polymerization reaction is initiated under the condition of supergravity, and the reaction liquid enters into the tubular reactor from an outlet of the supergravity reactor to continuously finish macroscopic polymerization reaction. The average molecular weight of the polyisobutene as the obtained product is controllable and ranges from 800 daltons to 5000 daltons, the molecular weight distribution index ranges from 1.8 to 2.5, and the content of a chain end alpha-double bond can be up to over 90%. By using the supergravity polymerization process provided by the invention, the microcosmic mixing, mass transferring and heat transferring processes of a reaction is greatly enhanced; compared with the traditional stirring polymerization method, the process method ensures that the average residence time of materials in the supergravity reactor is at least shortened to over 20-30 times; and in addition, the equipment volume is greatly reduced, andthe operating cost is reduced.

Description

technical field [0001] The invention relates to a process and a polymerization device for preparing polyisobutylene by a slurry method, and also relates to the extended application of high gravity technology in polyisobutylene polymerization. Highly active polyisobutylene products with a number average molecular weight in the range of 800-5000 Daltons can be prepared by the supergravity method. technical background [0002] Polyisobutylene is an important chemical substance, which is widely used in chemical, pharmaceutical, food and other industries, and its development and utilization prospects are very broad. Polyisobutylene is usually prepared from Friedel-Crafts acid (such as AlCl 3 ) initiation, isobutene is prepared by slurry polymerization reaction in the medium of methyl chloride. Polyisobutylene is insoluble in methyl chloride and precipitates out of solution as particles, thus forming a slurry system. Polymerization is usually carried out at a temperature of abo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F10/10C08F2/14C08F2/01
Inventor 陈建峰吴一弦吕丽丽邹海魁初广文刘冲王伟
Owner BEIJING UNIV OF CHEM TECH
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