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A kind of preparation method of polyisobutylene and isobutylene copolymer

A technology of isobutylene copolymer and polyisobutylene, applied in the field of polyisobutylene, can solve the problems of complex polymerization process, low polymerization temperature and high energy consumption

Active Publication Date: 2020-10-23
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The present invention aims to solve the technical problems of the traditional butyl rubber and polyisobutylene preparation method in the prior art, the polymerization temperature is too low, the energy consumption is high, and the polymerization process is complicated, and a preparation method of polyisobutylene and isobutylene copolymer is provided

Method used

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  • A kind of preparation method of polyisobutylene and isobutylene copolymer
  • A kind of preparation method of polyisobutylene and isobutylene copolymer
  • A kind of preparation method of polyisobutylene and isobutylene copolymer

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preparation example Construction

[0031] The invention provides a kind of preparation method of polyisobutylene and isobutylene copolymer, comprises the following steps:

[0032] Under anhydrous and oxygen-free conditions, the heterocyclic fused cencene-based rare earth compound and the organoboron compound are formed in an organic solvent according to a certain ratio to form a catalyst composition, and then the organic solution of the catalyst composition is added to an organic solution containing a specific amount of isobutene (or contain a certain amount of copolymerized second monomer) in the reaction device, initiate the polymerization reaction, the polymerization reaction is at -80 ° C ~ 50 ° C, after polymerization for 1 / 6 ~ 24 hours, pour the polymerization solution into ethanol to settle the polymer, Dry to obtain polyisobutylene or isobutylene copolymer.

[0033] The catalyst composition is prepared from a heterocyclic condensed cenyl rare earth compound and an organic boron compound in an organic so...

Embodiment 1

[0049] Embodiment 1 isobutylene homopolymerization

[0050] Under the protection of nitrogen, add 9.4 grams of 30 wt% isobutylene toluene solution to a 100 ml reaction kettle at -45°C, and after the polymerization reaction device and the polymerization solution cool down to the set temperature, add 10 micromoles of rare earth compounds 1 and 10 Micromolar organoboron salt [Ph 3 C][B(C 6 f 5 ) 4 ] composition in toluene (2 ml), polymerization was initiated. After stirring and reacting at -45°C for 60 minutes, the polymerization solution was poured into a container containing 100 ml of ethanol to terminate the reaction, and the polyisobutene after sedimentation was dried to constant weight in a vacuum oven at 60°C, and the monomer conversion rate was 75. %. The number average molecular weight M of gained polyisobutylene is tested by gel chromatography n =3.03×10 4 ,M n / M w =2.39.

[0051] Following embodiment 2-23 except the condition described in the table, other pol...

Embodiment 24

[0054] Example 24 Copolymerization of isobutylene and the second monomer

[0055] Under the protection of nitrogen, add 18.8 grams of 30 wt% isobutylene toluene solution and 0.68 grams of isoprene to a 100 milliliter reaction kettle at -45 ° C. After the polymerization reaction device and the polymerization liquid cool down to the set temperature, add 10 micromolar rare earth compound 6 and 20 micromolar organoboron salt [Ph 3 C][B(C 6 f 5 ) 4 ] composition in toluene (2 ml), polymerization was initiated. After stirring and reacting at -45°C for 60 minutes, the polymerization solution was poured into a container containing 100 ml of ethanol to terminate the reaction, and the settled isobutylene copolymer was dried to constant weight in a vacuum oven at 60°C, and the monomer conversion was 65%. The number average molecular weight M of gained polyisobutylene is tested by gel chromatography n =2.19×10 4 ,M n / M w =2.39.

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Abstract

The invention relates to a preparation method of polyisobutylene and an isobutylene copolymer. The method adopts a catalyst composed of a heterocyclic fused cyclopentadienyl rare earth compound with aheterocyclic fused cyclopentadienyl ligand with a relatively large conjugation action and an organic boron salt to realize homo-polymerization of isobutylene and copolymerization of isobutylene witha second monomer in an organic solution. The catalyst composed of the heterocyclic fused cyclopentadienyl rare earth compound and the organic boron salt has high polymerization activity and high efficiency, high-activity polyisobutylene can be prepared at a relatively high temperature, polyisobutylene with high molecular weight and the isobutylene copolymer with high molecular weight can be also prepared at a relatively low temperature. The chelating ligand has simple synthesis and relatively low cost, and can be industrially produced. According to the provided preparation method of polyisobutylene and the isobutylene copolymer, a molecular weight of a polymer can be controlled by changing a ratio of the catalyst to monomers, polymerization temperature and other methods.

Description

technical field [0001] The invention relates to the technical field of preparation of polyisobutylene and isobutylene copolymers, in particular to a method for preparing polyisobutylene and isobutylene copolymers which utilize a rare earth metal catalyst to realize homopolymerization of isobutene and copolymerization of isobutene and a second monomer in an organic solution, And the molecular weight of the polymer can be regulated by changing the ratio of catalyst to monomer, polymerization temperature and other methods. Background technique [0002] In 1996, British scientists discovered that aluminocene methyl compound and organoboron salt B(C 6 f 5 ) 3 The constituted catalytic system can catalyze the copolymerization of isobutylene and isoprene at -78°C to -25°C to prepare high molecular weight polyisobutene (Angew.Chem.Int.Ed.1996, 35, 2226-2228). However, the polymerization activity of the catalytic system is closely related to the metal aluminum chelating ligands, a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F10/10C08F4/54C08F110/10C08F210/10C08F210/12C08F236/08C08F236/22C08F212/14C08F216/18
CPCC08F10/10C08F110/10C08F210/10C08F210/12C08F4/545C08F236/08C08F236/22C08F216/18C08F212/14
Inventor 崔冬梅李世辉姜洋
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI