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Norbornene, octafluorocyclopentene and tetrafluoroethylene ternary polymerized catalyst and ternary polymerization method

The technology of a tetrafluoroethylene terpolymerization catalyst and octafluorocyclopentene is applied in the field of polymer synthesis catalyst and polymer synthesis technology, and can solve the problem of small molecular weight of copolymer, low degree of copolymer alternation and high yield of copolymer. Low reaction temperature, easy washing and separation, and high yield of copolymer

Inactive Publication Date: 2015-12-09
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

[0024] Dissolve 0.001 mole of bis(triphenylphosphine)nickel chloride, 0.001 mole of triisopropoxyaluminum and 0.008 mole of 8-hydroxyquinoline in 10 milliliters of benzene, and put it into the vacuum-pumped and nitrogen-filled oven to dry In a single-necked glass bottle, seal the bottle mouth with a latex tube, put it into a constant temperature water bath at 20°C for 15 minutes, and obtain the nickel-aluminum complex catalyst.

[0025] Add 0.01 mole of bicyclo[2,2,1]hept-2-ene, 0.01 mole of octafluorocyclopentene and 0.01 mole of tetrafluoroethylene into an autoclave evacuated several times and filled with nitrogen, and add 20ml of benzene to dissolve. According to the amount of bis(triphenylphosphine) nickel chloride in the catalyst, it is 0.1% of the total weight of norbornene, octafluorocyclopentene and tetrafluoroethylene to get the above nickel-aluminum complex catalyst and inject it with a syringe in the above mixture. React at a constant temperature of 20°C and a pres...

Embodiment 2

[0028] Take 0.001 mole of bis(triphenylphosphine) nickel chloride, 0.020 mole of tert-butoxyaluminum and 0.001 mole of α, α'-bipyridyl dissolved in 10 ml of toluene, put into the vacuum and bake with nitrogen for many times. In a dry single-necked glass bottle, the mouth of the bottle is sealed with a latex tube, and placed in a constant temperature water tank at 50°C for 40 minutes to obtain a nickel-aluminum complex catalyst.

[0029] Add 0.01 mole of 1-methylbicyclo[2,2,1]hept-2-ene, 0.01 mole of octafluorocyclopentene and 0.01 mole of tetrafluoroethylene into the autoclave that has been evacuated several times and filled with nitrogen, and add 20ml Toluene dissolves. According to the amount of bis(triphenylphosphine) nickel chloride in the catalyst, it is 2.5% of the total weight of norbornene, octafluorocyclopentene and tetrafluoroethylene to get the above-mentioned nickel-aluminum complex catalyst and inject it with a syringe in the above mixture. The reaction was carr...

Embodiment 3

[0031] Get 0.001 mole of bis(triphenylphosphine) nickel chloride, 0.020 mole of triisopropoxyaluminum and 0.005 mole of phenanthroline and dissolve it in 10 milliliters of tetrahydrofuran, put it into a vacuum-pumped, nitrogen-filled, baked and dried In a single-necked glass bottle, seal the bottle mouth with a latex tube, put it in a constant temperature water bath at 30°C for 25 minutes, and obtain the nickel-aluminum complex catalyst.

[0032] Add 0.01 mole of 5-methylbicyclo[2,2,1]hept-2-ene, 0.01 mole of octafluorocyclopentene and 0.01 mole of tetrafluoroethylene into the autoclave that has been evacuated several times and filled with nitrogen, and add 20ml THF dissolved. According to the amount of bis(triphenylphosphine) nickel chloride in the catalyst, it is 0.8% of the total weight of norbornene, octafluorocyclopentene and tetrafluoroethylene to get the above-mentioned nickel-aluminum complex catalyst and inject it with a syringe in the above mixture. React at a cons...

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Abstract

The invention relates to a norbornene, octafluorocyclopentene and tetrafluoroethylene ternary polymerized catalyst and a ternary polymerization method. The norbornene, octafluorocyclopentene and tetrafluoroethylene ternary polymerized catalyst is characterized in that a preparation method of the catalyst comprises steps as follows: bis(triphenylphosphine)nickel dichloride, alkoxy aluminum and a ligand compound are dissolved in a first solvent in a dry glass bottle with an inert gas atmosphere, the glass bottle is sealed and placed at a constant temperature of 20-50 DEG C for 15-40 min, and a nickel-aluminum complex catalyst is obtained, wherein the mole ratio of bis(triphenylphosphine)nickel dichloride to the ligand compound is (1:8)-(8:1), the mole ratio of bis(triphenylphosphine)nickel dichloride to alkoxy aluminum is (1:20)-(20:1), alkoxy aluminum is selected from aluminum Isopropoxide and aluminum tert-butoxide. The raw materials of the catalyst are low in cost and easy to obtain, the catalyst can generate catalytic activity at a low temperature and catalyze norbornene, octafluorocyclopentene and tetrafluoroethylene ternary polymerization, the reaction temperature is low, the catalytic efficiency is high, a product is very easy to wash and separate, and the yield of a copolymer is high.

Description

technical field [0001] The invention relates to a high polymer synthesis catalyst and a high polymer synthesis process, in particular to a norbornene, octafluorocyclopentene and tetrafluoroethylene 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 157nm ultraviolet lithography. The main disadvantages of this material are brittleness, poor viscosity and low molecular weight. After inserting acrylate and fluorine-containing vinyl into the main chain of polynorbornene, it can improve the cohesiveness and solubility of the polymer, and reduce the light absorption rate of the material itself. This copolymer can be used as a photoresist material for 157nm photocopying technology , For example, A.E.Feiring and M.Toriumi used norbornene, tetrafluoroethylene and acrylate co...

Claims

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Application Information

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IPC IPC(8): C08F232/08C08F232/04C08F214/26C08F4/70
Inventor 房江华杨建平徐卫红李正辉胡每杰高浩其
Owner NINGBO UNIVERSITY OF TECHNOLOGY
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