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Preparation method of butyl rubber

A technology of butyl rubber and mixture solution, which is applied in the field of polymerization reaction, can solve the problems of incomparable cost and initiation efficiency, and achieve the effects of avoiding equipment operation and production instability, easy content control, and low cost

Active Publication Date: 2015-08-19
TSINGHUA UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Unfortunately, these initiation systems are far from comparable to existing industrial systems in terms of cost and initiation efficiency, negating their possible benefits in improving the controllability of the production process

Method used

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  • Preparation method of butyl rubber

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Effect test

Embodiment 1

[0040] This embodiment uses a T-shaped three-way mixer with a diameter of 0.5 mm. In the prepared monomer mixture solution, the isomeric monoolefin is selected from isobutene, the conjugated diene is selected from isoprene, the molar ratio of isobutene and isoprene is 40:1, the diluent is anhydrous dichloromethane, and the diluent Accounting for 90%wt of the monomer mixture solution. In the prepared initiator mixture solution, Lewis acid is selected from AlCl 3 , AlCl 3 The molar ratio with water is 1.6:1, the diluent is anhydrous dichloromethane, and the content of water in the initiator mixture solution is 16ppm. The flow rate of the monomer mixture solution is 8 mL / min, the flow rate of the initiator mixed solution is 8 mL / min, the reaction temperature is -80° C., and the reaction residence time is 1 s. The number average molecular weight Mn of the butyl rubber product is 1.5×10 5 , the molecular weight distribution index was 2.50, and the yield was 62%.

Embodiment 2

[0041] Example 2: The molar ratio of isobutylene to isoprene is 200:1, other conditions are the same as in Example 1, and the number average molecular weight Mn of the butyl rubber product obtained is 5.0×10 5 , the molecular weight distribution index was 1.80, and the yield was 100%.

Embodiment 3

[0042] Embodiment 3: the reaction temperature is controlled as -40 DEG C, and other conditions are the same as embodiment 1, and the number average molecular weight Mn that obtains butyl rubber product is 1.2 * 10 5 , the molecular weight distribution index was 2.04, and the yield was 40%.

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Abstract

The invention discloses a preparation method of butyl rubber. Monomer mixture solution M and initiator mixture solution I are respectively prepared by using a diluent; the M, the I, a micro-mixer and a phantastron are precooled to reaction temperature; the M and the I make contact with each other to be mixed in the micro-mixer, react for certain standing time in the phantastron behind the micro-mixer, and then are subjected to posttreatments such as diluent removal and dryingto obtain the butyl rubber. According to the preparation method, an efficient micro mixing technology is utilized, and the phenomena of unstable equipment operation and production caused by oligomer production as reaction system microenvironment is out of control are avoided, so that the standing time of a production system is shortened to be within 10s, the initiator amount is remarkably reduced, and reliable preparation of polymer products is realized under more mild temperature conditions (minus 92 DEG C to minus 40 DEG C), thus remarkably reducing production energy consumption and improving the stability of product quality.

Description

technical field [0001] The invention belongs to the technical field of polymerization reaction, in particular to a method for realizing rapid and continuous preparation of butyl rubber by micro-mixing technology. Background technique [0002] Butyl rubber is a copolymer containing isomeric monoolefins, such as isobutylene, as the main component, accounting for 80 to 99.5% of the weight of the reactive monomers, and 0.5 to 20% of the weight of the reactive monomers, as a subcomponent. Polyolefins, preferably conjugated olefins, such as isoprene. Since isomeric monoolefins have electron-donating groups on both sides of the double bond and the distribution of electron clouds is very uneven, cationic polymerization, that is, the polymerization method using carbocations as active species, is the only effective way to obtain its polymers. method. The copolymerization product of isobutylene and isoprene is referred to as IIR, which has excellent air tightness, moisture tightness ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F210/12C08F2/01C08F2/00
Inventor 吕阳成朱珊骆广生王凯
Owner TSINGHUA UNIV
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