Norbornene, vinylcyclohexane and perfluoromethyl vinyl ether ternary copolymerization catalyst and ternary copolymerization method

A perfluoromethyl vinyl ether ternary copolymerization catalyst, perfluoromethyl vinyl ether technology, applied in the field of high polymers, can solve the problem of small molecular weight of copolymers, low degree of alternation of copolymers, low yield of copolymers, etc. problem, to achieve the effects of low polymerization reaction temperature, easy washing and separation, and high copolymer yield

Inactive Publication Date: 2017-06-20
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 yield of copolymers, small molecular weight of copolymers, and low degree of alternation of copolymers.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] In a three-necked flask with a dry inert gas atmosphere, dissolve 0.001 moles of bis-(1,5-cyclooctadiene) nickel and 0.001 moles of 8-hydroxyquinoline in 10 milliliters of benzene to obtain a mixed solution; install an electric stirrer Stirring, drop 0.006 mol tetraisopropoxytitanium into the mixed solution at 250 rpm, and stir at 30° C. for 60 minutes at a constant temperature after dropping, to obtain a nickel-titanium complex catalyst.

[0023] Add 0.01 mole of bicyclo[2,2,1]hept-2-ene, 0.01 mole of vinylcyclohexane and 0.01 mole of perfluoromethyl vinyl ether into the autoclave that has been evacuated several times and filled with nitrogen, and add 20ml Benzene dissolves. According to the amount of bis-(1,5-cyclooctadiene) nickel in the catalyst, it is bicyclo[2,2,1]hept-2-ene, vinyl cyclohexane and perfluoromethyl vinyl ether 0.01% of the total weight is taken from the above-mentioned nickel-titanium complex catalyst, and injected into the above-mentioned mixture ...

Embodiment 2

[0026] In a three-necked flask with a dry inert gas atmosphere, 0.001 moles of bis-(1,5-cyclooctadiene) nickel and 0.006 moles of α, α'-bipyridine were dissolved in 10 milliliters of toluene to obtain a mixed solution; Stir with an electric stirrer, drop 0.001 mole of tetraisopropoxytitanium into the mixed solution at 350 rpm, and stir at 40° C. for 40 minutes at a constant temperature to obtain a nickel-titanium complex catalyst.

[0027] Add 0.01 mole of bicyclo[2,2,1]hept-2-ene, 0.01 mole of vinylcyclohexane and 0.01 mole of perfluoromethyl vinyl ether into the autoclave that has been evacuated several times and filled with nitrogen, and add 20ml Toluene dissolves. According to the amount of bis-(1,5-cyclooctadiene) nickel in the catalyst, it is bicyclo[2,2,1]hept-2-ene, vinyl cyclohexane and perfluoromethyl vinyl ether 1.00% of the total weight is taken from the above-mentioned nickel-titanium complex catalyst, and injected into the above-mentioned mixture with a syringe....

Embodiment 3

[0029] In a three-necked flask with a dry inert gas atmosphere, dissolve 0.001 mole of bis-(1,5-cyclooctadiene) nickel and 0.012 mole of phenanthroline in 10 milliliters of tetrahydrofuran to obtain a mixed solution; install an electric stirrer to stir , drop 0.010 moles of tetraisopropoxytitanium into the mixed solution at 300 rpm, and stir at 50° C. for 60 minutes at a constant temperature to obtain a nickel-titanium complex catalyst.

[0030]Add 0.01 mole of 1-methylbicyclo[2,2,1]hept-2-ene, 0.01 mole of vinylcyclohexane and 0.01 mole of perfluoromethyl vinyl ether into a vacuum-pumped, nitrogen-filled autoclave In, add 20ml tetrahydrofuran to dissolve. 1-methylbicyclo[2,2,1]hept-2-ene, vinylcyclohexane and perfluoromethylethylene based on the amount of bis-(1,5-cyclooctadiene)nickel in the catalyst 0.08% of the total weight of the three base ethers is taken from the above-mentioned nickel-titanium complex catalyst, and injected into the above-mentioned mixture with a syri...

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PUM

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Abstract

The invention relates to a norbornene, vinylcyclohexane and perfluoromethyl vinyl ether ternary copolymerization catalyst and a ternary copolymerization method. In a three-neck flask with dry inert gas atmosphere, bis-(1,5-cyclooctadiene) nickel and ligand are dissolved into a first solvent, so that a mixed solution is obtained; then, under stirring, titanium tetraisopropanolate is dripped into the mixed solution, the mixed solution continues to be stirred under 30 DEG C to 70 DEG C for 30 to 70 minutes, and thereby a nickel-titanium complex catalyst is obtained; a norbornene monomer, vinylcyclohexane and a perfluoromethyl vinyl ether monomer are added into a high-pressure kettle which is vacuumized multiple times and filled with nitrogen, and a second solvent is added for dissolution; the nickel-titanium complex catalyst is then added, and reaction takes place under certain temperature and pressure for 1 to 8 hours; the product obtained by the reaction is poured into ethanol solution containing 4 to 5wt percent of hydrochloric acid, the obtained precipitate is washed with ethanol to become neutral, and after vacuum drying, a norbornene, vinylcyclohexane and perfluoromethyl vinyl ether ternary copolymer is obtained.

Description

technical field [0001] The invention relates to the field of high polymers, in particular to a ternary copolymerization catalyst of norbornene, vinyl cyclohexane and perfluoromethyl vinyl ether 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 157nm ultraviolet lithography. The main disadvantages of this material are brittleness, poor viscosity and low molecular weight. After fluorine-containing vinyl is inserted into the main chain of polynorbornene, the cohesiveness and solubility of the polymer can be improved, and the light absorption rate of the material itself can be reduced. This copolymer can be used as a photoresist material for 157nm printing technology, such as A.E. Feiring and M.Toriumi used norbornene, tetrafluoroethylene and acrylate copolymers as photolithographic materials, and thei...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F232/08C08F210/14C08F216/14C08F4/80
CPCC08F232/08C08F4/80C08F210/14C08F216/1408
Inventor 周国权王江波房江华高浩其胡敏杰杨建平王志强陈斌
Owner NINGBO UNIVERSITY OF TECHNOLOGY
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