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Norbornene, octafluorocyclopentene and cyclohexene ternary polymerization catalyst and ternary polymerization method

A cyclohexene-based ternary copolymerization catalyst, octafluorocyclopentene technology, applied in organic chemistry and other directions, can solve the problems of low copolymer yield, little research and small molecular weight of copolymer, etc., and achieve copolymer yield. The effect of high rate, easy washing and separation, and low reaction temperature

Active Publication Date: 2015-12-02
NINGBO UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

These synthetic methods currently used have disadvantages such as long reaction time, low copolymer yield, small molecular weight of the copolymer, and low degree of copolymer alternation. little research

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Take 0.001 mole of tris(triphenylphosphine)rhodium chloride, 0.001 mole of triethylaluminum and 0.008 mole of 8-hydroxyquinoline and dissolve them in 10 milliliters of benzene, and put them into a single-port chamber that has been repeatedly vacuumed and nitrogen-filled to dry. In a glass bottle, seal the mouth of the bottle with a latex tube, put it into a constant temperature water bath at 20°C for 20 minutes, and obtain a rhodium-aluminum complex catalyst.

[0026] Add 0.01 mole of bicyclo[2,2,1]hept-2-ene, 0.01 mole of octafluorocyclopentene and 0.01 mole of cyclohexene into an autoclave evacuated several times and filled with nitrogen, and add 20ml of benzene to dissolve. According to the amount of three (triphenylphosphine) rhodium chloride in the catalyst, it is 0.1% of the total weight of norbornene, octafluorocyclopentene and cyclohexene to get the above-mentioned rhodium-aluminum complex catalyst and inject it with a syringe in the above mixture. The reaction...

Embodiment 2

[0029] Take 0.001 mole of tris(triphenylphosphine) rhodium chloride, 0.010 mole of triisobutylaluminum and 0.001 mole of α, α'-bipyridyl dissolved in 10 ml of toluene, and put it into the oven after repeated vacuuming and nitrogen filling. In a dry single-necked glass bottle, seal the bottle mouth with a latex tube, put it into a constant temperature water bath at 30°C for 30 minutes, and obtain the rhodium-aluminum complex catalyst.

[0030] Add 0.01 mole of 1-methylbicyclo[2,2,1]hept-2-ene, 0.01 mole of octafluorocyclopentene and 0.01 mole of 1-methylcyclohexene into the autoclave that was evacuated several times and filled with nitrogen In, add 20ml of toluene to dissolve. According to the amount of three (triphenylphosphine) rhodium chloride in the catalyst, it is 0.4% of the total weight of norbornene, octafluorocyclopentene, and 1-methylcyclohexene to get the above-mentioned rhodium-aluminum complex catalyst , inject the above mixture with a syringe. The reaction was c...

Embodiment 3

[0032] Take 0.001 mole tris(triphenylphosphine) rhodium chloride, 0.010 mole dichloroethylaluminum and 0.005 mole o-phenanthroline and dissolve them in 10 milliliters of tetrahydrofuran, and put them into a single-port chamber that has been repeatedly vacuumed and dried with nitrogen. In a glass bottle, seal the mouth of the bottle with a latex tube, put it into a constant temperature water bath at 25°C for 25 minutes, and obtain a rhodium-aluminum complex catalyst.

[0033]Add 0.01 mole of 5-methylbicyclo[2,2,1]hept-2-ene, 0.01 mole of octafluorocyclopentene and 0.01 mole of 3-methylcyclohexene to several vacuum-evacuated, nitrogen-filled autoclaves In, add 20ml tetrahydrofuran to dissolve. According to the amount of three (triphenylphosphine) rhodium chloride in the catalyst, it is 0.8% of the total weight of norbornene, octafluorocyclopentene, and 3-methylcyclohexene to get the above-mentioned rhodium-aluminum complex catalyst , inject the above mixture with a syringe. Re...

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Abstract

The invention relates to a norbornene, octafluorocyclopentene and cyclohexene ternary polymerization catalyst and a ternary polymerization method. The catalyst is characterized in that a preparation method for the catalyst comprises the following steps: rhodium(I) tris(triphenylphosphine) chloride, alkyl aluminium and a ligand ompound are dissolved in a first solvent in a single-mouth glass bottle with the dry inert atmosphere, the bottle mouth is sealed through a latex tube, and heat preservation is carried out for 20-30 minutes at 20-30 DEG C, so as to obtain a rhodium-aluminum complex catalyst, wherein the mole ratio of rhodium(I) tris(triphenylphosphine) chloride to the ligand is (1:8)-(8:1). The catalyst provided by the invention is a novel rhodium-aluminum complex catalyst mixture, raw materials of the catalyst are cheap and accessible, norbornene, octafluorocyclopentene and cyclohexene ternary polymerization can be catalyzed since catalytic activity can be generated at lower temperature, the reaction temperature is low, catalytic efficiency is high, the product is easy to wash and separate, and the yield of the copolymer is high.

Description

technical field [0001] The invention relates to a high polymer synthesis catalyst and high polymer synthesis, specifically a norbornene, octafluorocyclopentene and cyclohexene ternary copolymerization catalyst and a ternary copolymerization method. Background technique [0002] Polynorbornene is a special polymer with excellent mechanical properties, heat resistance, solubility in organic solvents and transparency, and can be used for 193nm ultraviolet lithography. The main disadvantages of this material are brittleness, poor viscosity and low molecular weight. After octafluorocyclopentene is inserted into the main chain of polynorbornene, the cohesiveness and solubility of the polymer can be improved, and after fluorine-containing vinyl is inserted into the main chain of polynorbornene, the cohesiveness and solubility of the polymer can be improved , and reduce the absorbance of the material itself. This terpolymer can be used as a photoresist material in 193nm photocopyi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F232/08C08F232/04C08F4/52C07F19/00
Inventor 房江华胡每杰徐卫红李正辉杨建平高浩其
Owner NINGBO UNIVERSITY OF TECHNOLOGY
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