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Splitblip molecular weight distribution high-cis-polydiene and preparation method thereof

A molecular weight distribution, polydiene technology, applied in the field of bimodal molecular weight distribution high cis polydiene and its preparation, can solve the problems of difficulty in preparing polybutadiene or polyisoprene products, high price and the like , to achieve the effect of stable and easy control of the polymerization process

Inactive Publication Date: 2007-12-12
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

CN1528794 proposes adding a small amount of butadiene to participate in aging on the basis of adding a small amount of butadiene to the three-way catalyst of rare earth salt / alkylaluminum / chlorine compound, by adding alkoxyalumoxane (MAO) or modified alkoxyalumoxane ( MMAO) can adjust the molecular weight and molecular weight distribution of butadiene rubber, and the distribution index is between 1.5 and 4.0, but the price of MAO or MMAO is relatively expensive
[0009] Furthermore, none of the above catalyst systems are useful for the production of polybutadiene or polyisoprene products with bimodal molecular weight distributions

Method used

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  • Splitblip molecular weight distribution high-cis-polydiene and preparation method thereof
  • Splitblip molecular weight distribution high-cis-polydiene and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] at 50°C and N 2 Under protection, add neodymium octanoate (0.088mmol) and 2-ethylhexanoic acid (0.088mmol) into a dry catalyst preparation bottle at 50°C and mix the solution for 2 hours before adding chloroform (1.2mmol), trichloro Ethyl acetate (0.13mmol) and triisobutylaluminum (Al(i-Bu) 3 ) (1.41mmol) in the mixed solution reacted at 50°C for 1 hour, after the two solutions were fully mixed, they were aged at 50°C for 1 hour to prepare a light gray blue transparent homogeneous catalyst system.

[0034] in N 2 Under protection, add 40ml of butadiene and raffinate (i.e. C 6 ~C 8 alkane mixed solution) mixed solution (wherein monomer mass concentration is 20%) and above-mentioned catalyst solution (catalyst / monomer=0.9mmol / mol) start polymerization, after reacting for 3 hours, add 2,6 containing 0.1% by mass - Ethanol solution of di-tert-butyl-p-cresol and hydrochloric acid to terminate the polymerization. After removing the solvent and unreacted monomers, the pol...

Embodiment 2

[0036] at 50°C and N 2 Under protection, neodymium octanoate (0.088mmol) and 2-ethylhexanoic acid (0.04mmol) were pre-mixed in a dry catalyst preparation bottle at 0°C for 160 hours, then added to chloroform (0.99mmol), dichloromethane ( 0.08mmol), ethyl trichloroacetate (0.11mmol) and triisobutylaluminum (Al(i-Bu) 3 )(1.41mmol) and diisobutylaluminum hydride Al(i-Bu) 2 H) (0.12 mmol) in the solution after reacting at 50° C. for 1 hour, after the two solutions were fully mixed, aged at 50° C. for 1 hour to prepare a light gray blue transparent homogeneous catalyst system.

[0037] in N 2 Under protection, add 40ml of butadiene and raffinate (i.e. C 6 ~C 8 alkane mixed solution) mixed solution (wherein monomer mass concentration is 20%) and above-mentioned catalyst solution (catalyst / monomer=0.7mmol / mol) start polymerization, after reacting for 2.2 hours, add 2,6 containing 0.1% by mass - Ethanol solution of di-tert-butyl-p-cresol and hydrochloric acid to terminate the pol...

Embodiment 3

[0039] at 40°C and N 2 Under protection, in a dry catalyst preparation bottle, mix solution of neodymium octanoate (0.088mmol) and 2-ethylhexanoic acid (0.02mmol) in advance, then add trichloroethane (0.088mmol), 2-phenyl-2- Chloropropane (0.01mmol) and triisobutylaluminum (Al(i-Bu) 3 ) (1.41mmol), mixed uniformly and then aged for 2 hours to prepare a light gray blue transparent homogeneous catalyst system A.

[0040] at 50°C and N 2 Under protection, ethyl trichloroacetate (0.13mmol) was reacted with triisobutylaluminum (Al(i-Bu)3) (1.41mmol) in a dry catalyst preparation bottle for 1 hour, and then neodymium octanoate (0.088 mmol) and 2-ethylhexanoic acid (0.36mmol), mix uniformly and continue to age at 50°C for 1 hour to prepare a light gray blue transparent homogeneous catalyst system B.

[0041] in N 2 Under protection, add 40ml of butadiene and raffinate (i.e. C 6 ~C 8 alkane mixed solution) mixed solution (wherein monomer mass concentration is 20%) and above-ment...

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Abstract

The invention relates to a kind of sym-form polydiene rubber with bimodal molecular weight distribution and the preparation method. The conjugated polydiene with bimodal / acromion molecular weight distribution can be produced in one single reactor directly. The invention is characterized by high catalytic activity, stable catalytic property, easy controllable polymerization and conjugated polydiene with structure unit larger than 96%. The polymer produced in this invention can not only retain mechanical performance of high molecular part, but aslo retains the processing performance of low molecular weight part.

Description

Technical field: [0001] The invention relates to a bimodal molecular weight distribution high cis polydiene and a preparation method thereof. More specifically, the method of the invention is a method for synthesizing a bimodal molecular weight distribution high cis polydiene in a reactor. Background technique: [0002] It is well known that the molecular weight and molecular weight distribution of polymers are important factors in determining the physical, mechanical and rheological properties of polymers. The so-called bimodal molecular weight distribution means that the polymer molecular weight distribution curve measured by gel permeation chromatography (GPC) presents two or more peaks, which is called bimodal molecular weight distribution, referred to as bimodal molecular weight distribution. [0003] A way to improve the processability of polymers is to produce polymers with bimodal molecular weight distribution, which has been extensively studied in the field of polye...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F36/02C08F4/602
Inventor 吴一弦郭青磊朱寒赵姜维
Owner BEIJING UNIV OF CHEM TECH
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