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Catalyst for terpolymerization of norbornene, acrylate and octafluorocyclopentene and ternary copolymerization method

An octafluorocyclopentene ternary copolymerization catalyst and technology of ternary copolymerization catalysts, which are applied in the field of high polymers, can solve the problems of little research, low yield of copolymers, and low degree of alternation of copolymers, and achieve easy washing Separation, low reaction temperature, high catalytic efficiency

Inactive Publication Date: 2016-04-06
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. Carried out very little

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Take 0.01 mol of 2-acetyl-6-(2-methylphenylimino)ethylpyridinium chloride, 0.01 mol of tris(butylcyclopentadienyl)yttrium, 0.01 mol of carbon tetrachloride and 20 ml of cyclohexyl Put the ketone into a single-mouthed glass bottle that has been evacuated several times and baked with nitrogen, and the bottle mouth is sealed with a latex tube to obtain the iron-gadolinium complex catalyst.

[0021] Add 0.01 mole of bicyclo[2,2,1]hept-2-ene, 0.01 mole of tert-butyl methacrylate and 0.01 mole of octafluorocyclopentene monomer into the one-port glass that has been evacuated several times and baked with nitrogen gas In the bottle, add 5ml cyclohexanone to dissolve. The amount of 2-acetyl-6-(2-methylphenylimino) ethylpyridinium iron chloride is 1% of the total weight of the three monomers to get the iron-gadolinium complex catalyst, and inject the above-mentioned mixture with a syringe. In the object, put the one-mouth glass bottle into a constant temperature water tank, and r...

Embodiment 2

[0025] Take 0.01 mole of 2-acetyl-6-(2-methylphenylimino)ethylpyridinium iron chloride, 0.08 mole of tris(butylcyclopentadiene)yttrium, 0.05 mole of carbon tetrachloride and 20 milliliters of toluene Put it into a single-necked glass bottle that has been evacuated several times and baked with nitrogen, and the bottle mouth is sealed with a latex tube to obtain the iron-gadolinium complex catalyst.

[0026] Add 0.01 mole of 1-methylbicyclo[2,2,1]hept-2-ene, 0.01 mole of ethyl acrylate and 0.01 mole of octafluorocyclopentene monomer into the single-port In a glass bottle, add 5ml of toluene to dissolve. The amount of 2-acetyl-6-(2-methylphenylimino) ethylpyridinium iron chloride is 4% of the total weight of the three monomers to get the iron-gadolinium complex catalyst, and inject the above mixture into the syringe , put the single-necked glass bottle into a constant temperature water tank, and react at 70°C for 4 hours. Pour the product into methanol solution containing 5% hy...

Embodiment 3

[0028] Take 0.01 mole of 2-acetyl-6-(2-methylphenylimino)ethylpyridinium iron chloride, 0.05 mole of tris(butylcyclopentadiene)yttrium, 0.04 mole of carbon tetrachloride and 20 milliliters of toluene Put it into a single-necked glass bottle that has been evacuated several times and baked with nitrogen, and the bottle mouth is sealed with a latex tube to obtain the iron-gadolinium complex catalyst.

[0029] Add 0.01 mole of bicyclo[2,2,1]hept-2-ene, 0.01 mole of methyl methacrylate and 0.01 mole of octafluorocyclopentene into a single-necked glass bottle that has been evacuated several times and baked with nitrogen. Add 5ml of toluene to dissolve. The amount of 2-acetyl-6-(2-methylbenimino) ethylpyridinium iron chloride is 3% of the total weight of the three monomers to get the iron-gadolinium complex catalyst, inject the above mixture with a syringe In the object, put the one-mouth glass bottle into a constant temperature water tank, and react at 90°C for 8 hours. The produc...

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Abstract

The invention relates to a norbornene, acrylics and octafluorocyclopentene ternary polymerization catalyst. The norbornene, acrylics and octafluorocyclopentene ternary polymerization catalyst is characterized in that Fe(6-[1-{(2-methyl)imino}ethyl]-2-acetylpyridine)Cl2, tris(n-butylcyclopentadienyl)yttrium, carbon tetrachloride and a first solvent are placed in an inertia dry single-opening glass bottle, the bottle opening is sealed through a latex tube, and the ternary polymerization catalyst is obtained after dissolution. Norbornene monomers, acrylics monomers and octafluorocyclopentene monomers are prepared according to the mole ratio of 1:1:1, the mixture is added to an inertia dry container, and a second solvent is added to the container so that the mixture can be dissolved. The ternary polymerization catalyst is added and reacts for 2 hours to 8 hours at the constant temperature of 30 DEG C to 90 DEG C, the product is poured into a methanol solution containing 4.5 wt% to 5.5 wt% of hydrochloric acid so that the copolymer can deposit, the sediment is washed through methyl alcohol to be neutral and then dried in vacuum, and then the norbornene, acrylics and octafluorocyclopentene terpolymer is obtained. Raw materials of the catalyst are low in price and can be easily obtained, the catalytic efficiency is high, the reaction temperature is low, and the copolymer yield is high.

Description

technical field [0001] The invention relates to the field of high polymers, in particular to a catalyst for terpolymerization of norbornene, acrylate and octafluorocyclopentene 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 . Moreover, the development of the microelectronics industry requires components with smaller sizes. For the exposure technology suitable for line ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F232/08C08F220/18C08F232/04C08F4/70
Inventor 房江华杨建平王江波李正辉高浩其胡敏杰丛杨
Owner NINGBO UNIVERSITY OF TECHNOLOGY
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