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A kind of rare earth butyl rubber and its preparation method

A butyl rubber and rare earth technology, applied in the field of rare earth butyl rubber and its preparation, can solve the problems of low production efficiency, short production cycle, high energy consumption, etc., and achieve the effects of low cost, extended production cycle and easy synthesis

Active Publication Date: 2019-08-20
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the industrial production method of butyl rubber is based on the cationic polymerization mechanism and adopts the slurry process. Because the cationic polymerization reaction has the characteristics of low temperature and high speed, it needs to rely on two-stage refrigeration to complete the polymerization at about -100°C, which consumes a lot of energy and is difficult to control. , frequent blocking leads to short production cycle and low production efficiency

Method used

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  • A kind of rare earth butyl rubber and its preparation method
  • A kind of rare earth butyl rubber and its preparation method
  • A kind of rare earth butyl rubber and its preparation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] Embodiment 1 monocyclocene dialkyl scandium complex (C 5 Me 4 SiMe 3 )Sc(CH 2 SiMe 3 ) 2 Preparation of (THF)

[0013] In the glove box, weigh 3.26g Sc(CH 2 SiMe 3 ) 3 (THF) 2 (7.25mmol) was put into a 100mL round bottom flask filled with a magnetic stirrer, and 10mL of n-hexane solvent was added to dissolve it. Weigh 1.41g trimethylsilyltetramethylcyclopentadiene C 5 Me 4 H(SiMe 3 ) (7.25mmol), dissolved with 1mL of n-hexane, and added dropwise to the reaction flask at room temperature. After stirring for 2 h, the solution was concentrated under reduced pressure to about 1 mL, left standing overnight at -35°C, and recrystallized to obtain 2.73 g of colorless crystals (C 5 Me 4 SiMe 3 )Sc(CH 2 SiMe 3 ) 2 (THF).

Embodiment 2

[0014] Embodiment 2 Preparation of isobutylene homopolymer

[0015] In a glove box under the protection of inert gas nitrogen, add 15ml of toluene solution to a 100ml stainless steel reaction kettle, use a low-temperature constant temperature bath to control the polymerization reaction temperature, the polymerization reaction temperature is -35°C, add 3.2g of isobutylene monomer, turn on the stirring, add The prepared catalyzer of above-mentioned embodiment 1, rare earth catalyst Sc consumption is 20umol, rare earth catalyst (C 5 Me 4 SiMe 3 )Sc(CH 2 SiMe 3 ) 2 (THF) and organoboron reagent [Ph 3 C][B(C 6 f 5 ) 4 ] molar ratio [Sc] / [B] is 1, after 60 minutes of polymerization reaction, methanol is added to terminate the reaction, the glue is post-treated, and the product is vacuum-dried. Analytical test: the number average molecular weight of isobutylene homopolymer is 13.47×10 4g / mol, molecular weight distribution HI is 1.85.

Embodiment 3

[0016] Embodiment 3 Preparation of isobutylene homopolymer

[0017] The polymerization temperature is -45°C, other polymerization conditions are the same as in Example 2, analysis and test: the number average molecular weight of the isobutylene homopolymer is 29.89×10 4 g / mol, molecular weight distribution HI is 1.61.

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Abstract

The invention relates to a rare-earth butyl rubber and a preparation method thereof. The rare-earth butyl rubber is a homopolymer prepared by using a rare-earth catalyst to catalyze isobutylene polymerization, or a copolymer prepared by catalyzing isobutylene-comonomer polymerization. The number-average molecular weight is 1-100*10<4>. The mol percent of the comonomer is 1-20%. The comonomer is selected from one or mixture of more of olefins and olefin derivatives, wherein the olefins are selected from alpha-olefins, conjugated olefins and cycloolefins; and the olefin derivatives are selected from alpha-olefin derivatives, conjugated olefin derivatives and cycloolefin derivatives containing nitrogen, oxygen, chlorine and bromine atom functional groups. The rare-earth catalyst comprises A and B, wherein A is rare-earth coordination compounds CpLnR2Xn, Ln is a rare-earth metal, and B is an organic boron reagent. The rare-earth catalyst has the advantages of high activity and stable valence state; the polymerization reaction can be competed at higher temperature; and thus, the method has the advantages of energy saving, high safety, long production cycle, no corrosion, no toxicity and environment friendliness.

Description

technical field [0001] The invention belongs to the technical field of advanced manufacturing of high-performance polymer materials, and relates to a kind of rare earth butyl rubber and a preparation method thereof. Background technique [0002] Butyl rubber (IIR) has excellent air tightness, low glass transition temperature, good damping and aging resistance, and has been widely used in the fields of automobile tires, construction materials and biomedicine. At present, the industrial production method of butyl rubber is based on the cationic polymerization mechanism and adopts the slurry process. Because the cationic polymerization reaction has the characteristics of low temperature and high speed, it needs to rely on two-stage refrigeration to complete the polymerization at about -100°C, which consumes a lot of energy and is difficult to control. , Frequent blocking leads to short production cycle and low production efficiency. Realizing the production of butyl rubber at ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F110/10C08F210/12C08F236/08C08F210/10C08F236/22C08F232/08C08F212/08C08F236/14C08F236/16C08F212/14C08F214/14C08F4/52
Inventor 李杨李婷婷杨珂谭睿郭方史正海牛慧
Owner DALIAN UNIV OF TECH
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