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Process method for preparing polyisobutene and polymerization device

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

Active Publication Date: 2013-07-24
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
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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.

Method used

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  • Process method for preparing polyisobutene and polymerization device

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

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

[0031] Add 4000ml of the mixture of isobutylene monomer and dichloromethane into storage tank 1, the monomer concentration is 2.0mol / L, and the dichloromethane and AlCl 3 Add 900ml of the mixed solution B into storage tank 2, where the initiator is 0.25 mol / L. When the materials in storage tank 1 and storage tank 2 are cooled to about -25°C, respectively, the two are separated by a double plunger metering pump. The strands are fed into the premixing tube in the high-gravity rotating packed bed reactor at a volume ratio of 10:1, and the mixture 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 rotating packed bed The reaction was continued for 1 min in a tubular reactor with an aspect ratio of 15:1. The rotor speed of the supergravity rotating packed bed reactor...

Embodiment 2

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

[0034] Implementation column 3

[0035] The process flow and steps are the same as in Example 1. The monomer concentration is 1.5 mol / L, the initiator concentration is 0.35 mol / L, and the material volume ratio is 15:1. The reaction in the tubular reactor is 10s. The gravity level is 500g. The number average molecular weight of the obtained polyisobutylene product M n The molecular weight distribution index is 1400, the molecular weight distribution index is 2.02, the yield is 90%, and the alpha-double bond content at the molecular end is 91%.

[0036] Implementation column 4

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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 polymerization device for preparing polyisobutylene by a slurry method, and also relates to the expanded application of supergravity technology in the polymerization reaction of polyisobutylene. High-activity polyisobutylene products with a number average molecular weight in the range of 800-5000 Daltons can be prepared by the high-gravity method. technical background [0002] Polyisobutylene is an important chemical substance, widely used in chemical, pharmaceutical, food and other industries, and its development and utilization prospects are very broad. Polyisobutylene is usually made of Friedel-Crafts acid (such as AlCl 3 ) Initiation, isobutylene is prepared by slurry polymerization in methyl chloride medium. Polyisobutylene is insoluble in methyl chloride and precipitates out of the solution as particles, thereby forming a slurry system. The polymerization is usually carried out at a temperature of about -20°C. ...

Claims

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Application Information

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Patent Type & Authority Patents(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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