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Preparation method of butyl rubber

A technology of butyl rubber and dialkyl, which is applied in the field of preparing butyl rubber by rare earth catalyst, can solve the problems of affecting product quality, difficult to meet the economical production of industrialized production, and high metal residues in polymerization activity.

Active Publication Date: 2022-05-06
PETROCHINA CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the catalytic system composed of rare earth compounds chelated by cyclopentadiene ligands and organic boron salts can only catalyze the polymerization of isobutylene up to 4000 times, and the polymerization activity is difficult to meet the economical requirements of industrial production.
Moreover, the lower catalytic activity increases the amount of catalyst used, resulting in excessive metal residues in the product, which seriously affects product quality (ash residues are not up to standard)

Method used

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  • Preparation method of butyl rubber
  • Preparation method of butyl rubber
  • Preparation method of butyl rubber

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0032] Preparation process of boron nitrogen heterocyclic rare earth compounds a and b

[0033] Under nitrogen or argon atmosphere, react 2 mol of borazine ligand 1 with 2 mol of n-butyllithium in 10 mL of tetrahydrofuran solution at -40°C for 1 hour, then slowly add the solution dropwise to 2 mol of ScCl at room temperature 3 tetrahydrofuran (10mL) suspension, then reacted at room temperature for 1 hour, slowly added 4 mol of trimethylsilyl methylene lithium to the above solution, reacted at room temperature for about 1 hour, vacuumed all the solvents, and used 20mL of toluene was extracted, concentrated, and recrystallized at -35°C to obtain borazine heterocyclic rare earth compound a.

[0034] In the same way, ligand 2 was used to prepare borazine heterocyclic rare earth compound b.

[0035] Borazine Ligand Ligand

[0036]

Embodiment 1

[0038] Preparation of isobutylene homopolymer

[0039] Under nitrogen protection, 9.4 grams of 30 wt% isobutylene toluene solution was added to a 50 ml reaction kettle at -30°C, and then 10 micromoles of compound a and 10 micromoles of organoboron salt [Ph 3 C][B(C 6 f 5 ) 4 ] composition in toluene (1 ml) and polymerization was initiated. After stirring and reacting at -30°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 85. %. The number average molecular weight M of gained polyisobutylene is tested by gel chromatography n =6.14×10 4 ,M w / M n =2.21; glass transition temperature T g = -71°C.

Embodiment 2

[0041] Preparation of isobutylene homopolymer

[0042] Under nitrogen protection, 11.2 grams of 30 wt% isobutylene toluene solution was added to a 25 ml reaction kettle at -20°C, and then 10 micromoles of compound a and 10 micromoles of organoboron salt [Ph 3 C][B(C 6 f 5 ) 4 ] composition in toluene (1 ml) and polymerization was initiated. After stirring and reacting at -20°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 in a vacuum oven at 60°C to constant weight, and the monomer conversion rate was 81. %. The number average molecular weight M of gained polyisobutylene is tested by gel chromatography n =3.24×10 4 ,M w / M n =2.04; glass transition temperature T g = -69°C.

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Abstract

The invention discloses a preparation method of butyl rubber, which adopts a catalyst system composed of a boron-nitrogen heterocyclic rare earth dialkyl compound in a formula I and an organic boron salt to prepare polyisobutene rubber through solution polymerization reaction at the temperature of-70-20 DEG C. The boron-nitrogen heterocyclic ring ligand introduced in the invention has a unique electronic effect, compared with a traditional butyl rubber preparation process, the energy consumption of polymerization reaction is greatly reduced, the catalytic activity and efficiency are higher, and the method has a wide application prospect. The formula I is shown in the specification.

Description

technical field [0001] The invention relates to a method for preparing butyl rubber with a rare earth catalyst, in particular to a method for efficiently preparing butyl rubber with a rare earth catalyst. Background technique [0002] Butyl rubber is a kind of synthetic rubber, which is mainly composed of isobutylene structural units. It has good chemical stability, thermal stability, excellent air tightness and water tightness, and is used in automobile tire inner tubes, anti-vibration rubber, and industrial rubber sheets. , medical rubber and other fields have a wide range of applications. The isobutylene monomer has two α-methyl groups, which greatly increases the electron cloud density of the carbon-carbon double bond, and is easily attacked by cations for cationic polymerization. So far, the industrial production of butyl rubber mainly utilizes AlCl 3 , BF 3 、TiCl 4 Lewis acid and a certain amount of water molecules, alcohol, etc. form an initiating system, and use ...

Claims

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Application Information

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IPC IPC(8): C08F210/12C08F4/54
CPCC08F210/12C08F4/545Y02T10/86
Inventor 黄安平徐人威李广全郝萍高琳涂晓燕李艳芹陈雪蓉樊杰王卓妮杨世元李朋朋张平生杨柳
Owner PETROCHINA CO LTD
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