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Method for preparing isomonoolefin-polyene hydrocarbon copolymer

A technology of iso-mono-olefin and poly-olefin, applied in the field of preparing iso-mono-olefin-poly-olefin copolymer, can solve problems such as gel

Active Publication Date: 2013-10-09
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Regarding the method of adjusting the molecular weight distribution or processability of butyl rubber, patents US2781334 and US2729626 propose adding a coupling agent divinylbenzene (DVB) to the polymerization system to couple some molecular chains to generate a small amount of high molecular weight branched macromolecules To improve the initial strength of the polymer, but a little more DVB will cause obvious gel problems

Method used

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  • Method for preparing isomonoolefin-polyene hydrocarbon copolymer
  • Method for preparing isomonoolefin-polyene hydrocarbon copolymer
  • Method for preparing isomonoolefin-polyene hydrocarbon copolymer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0073] Inject 8.06ml of refined methylene chloride into a 60ml croissant at -70°C, EtAlCl 2 (0.9M in hexane) 0.89ml, and DCC (0.04M in dichloromethane) 0.83ml, HCl (0.15M in dichloromethane) 0.22ml, [HCl] / ([HCl]+[DCC] )=50mol%, forming an initiator solution, and aging the initiator solution at this temperature for 4min, ready for use.

[0074] The polymerization reaction is carried out in a nitrogen operating box. In a low-temperature cooling bath at -100°C, 128g of monochloromethane, 32g of isobutylene and isoprene at -80°C are injected into a 500ml glass reactor equipped with strong constant speed stirring. 0.82 g, forming a monomer solution. The temperature of the monomer solution was lowered to -97°C, and 6 ml of the aged initiator solution was added dropwise over 8 minutes. During this period, liquid nitrogen was used to control the temperature, and the polymerization temperature was maintained at -94.6°C to -101.7°C. The polymerization time was 8 minutes, which corresp...

Embodiment 2

[0076] Inject 8.14ml of refined dichloromethane, EtAlCl 2 (0.9M in hexane) 0.89ml, DCC (0.04M in dichloromethane) 0.42ml, and HCl (0.15M in dichloromethane) 0.45ml, [HCl] / ([HCl]+[DCC] )=80.0mol%, forming an initiator solution, and aging the initiator solution at this temperature for 5 minutes, ready for use. Subsequently, the method of Example 1 was repeated, except that 6 ml of the aged initiator solution was added dropwise to the monomer solution over 10 minutes, during which the polymerization temperature was controlled at -94.7°C to -100.9°C. As a result, 22.1g of the polymer was obtained, and the weight yield was 67.3%. n =261000, M w =831000, M w / M n = 3.18.

Embodiment 3

[0078] Inject 8.31ml of refined methylene chloride into a 60ml croissant at -70°C, EtAlCl 2 (0.9M in hexane) 0.89ml, DCC (0.04M in dichloromethane) 0.28ml, and HCl (0.15M in dichloromethane) 0.52ml, [HCl] / ([HCl]+[DCC] )=87.5mol%, forming an initiator solution, and aging the initiator solution at this temperature for 3min, ready for use. The method of Example 1 was then repeated, except that 5 ml of the aged initiator solution was added dropwise to the monomer solution over 10 minutes, during which the polymerization temperature was controlled at -95.3°C to -101.3°C. As a result, polymer 19.7g, weight yield 60.0%, M n =250700, M w =751000, M w / M n = 3.00.

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Abstract

The invention relates to a method for preparing isomonoolefin-polyene hydrocarbon copolymer. According to the method, at least one C4-C8 isomonoolefin monomer and at least one C4-C14 polyene hydrocarbon monomer contact with an initiator system containing halogen multifunctional organic halide shown as a formula (I), halogen hydride shown as a formula (II) and monoalkyl dihalogenate aluminium shown as a formula (III) or an initiator system containing halogen multifunctional organic halide shown as the formula (I), monoalkyl dihalogenate aluminium shown as the formula (III) and dialkyl aluminium halide shown as a formula (IV), at -120- -20 DEG C with existence of inertia organic solvent; and variables in compounds (I), (II), (III) and (IV) are defined in the instruction. The method for preparing isomonoolefin-polyene hydrocarbon copolymer can easily adjust a molecular weight distribution of an obtained copolymer, which has a high molecular weight. HY(II); AlRY'2 (III); AlR'2Y'' (IV).

Description

technical field [0001] The present invention relates to a method for preparing an isomonoolefin-polyene copolymer by which the molecular weight distribution of the isomonoolefin-polyene copolymer can be easily adjusted. More specifically, the present invention relates to a method in the presence of an initiator system comprising a halogen polyfunctional organic halide, a hydrogen halide and a monoalkylaluminum dihalide, or in the presence of a halogen polyfunctional organic halide, a mono In the presence of an initiator system of alkyl aluminum dihalide and dialkyl aluminum halide, the method of copolymerizing isomonoolefin and polyene to obtain isomonoolefin-polyene copolymer with adjustable molecular weight distribution. Background technique [0002] Butyl rubber (IIR) has been available as a commodity for more than sixty years, and has become the most important rubber due to its excellent air tightness, damping, heat aging resistance, ozone resistance and weather resistan...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F210/12C08F4/52
Inventor 邱迎昕张雷赵丽娜龚惠勤刘海明
Owner CHINA PETROLEUM & CHEM CORP