Ternary polymerization catalyst of norbornene, octafluorocyclopentene and styrene and ternary polymerization method

A styrene ternary copolymerization catalyst and technology of octafluorocyclopentene, applied in the field of high polymer, can solve the problems of low yield of copolymer, few research and development, small molecular weight of copolymer, etc., and achieve high yield of copolymer , Easy washing and separation, low reaction temperature

Inactive Publication Date: 2015-08-05
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. rare

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Dissolve 0.001 mol of neodymium trichloride, 0.001 mol of diethyl zinc and 0.010 mol of 8-hydroxyquinoline in 10 ml of benzene, and put them into a single-necked glass bottle that has been evacuated several times and filled with nitrogen to dry. Seal it with a latex tube, put it into a constant temperature water bath at 40°C for 20 minutes, and obtain a neodymium-zinc complex catalyst.

[0024] Add 0.01 mole of bicyclo[2,2,1]hept-2-ene, 0.01 mole of octafluorocyclopentene and 0.01 mole of styrene into an autoclave evacuated several times and filled with nitrogen, and add 20ml of benzene to dissolve. The amount of neodymium trichloride in the catalyst is 0.08% of the total weight of norbornene, octafluorocyclopentene, and styrene. Take the above-mentioned neodymium-zinc complex catalyst and inject it into the above-mentioned mixture with a syringe. The reaction was carried out at a constant temperature of 40° C. under a pressure of 0.1 MP for 6 hours. The product was po...

Embodiment 2

[0027] Dissolve 0.001 mole of neodymium trichloride, 0.020 mole of diethyl zinc and 0.001 mole of α, α,-bipyridine in 10 milliliters of toluene, and put them into a single-necked glass bottle that has been evacuated several times and baked and dried with nitrogen. Seal the mouth of the bottle with a latex tube, put it into a constant temperature water bath at 50°C for 30 minutes, and obtain the neodymium-zinc complex catalyst.

[0028] Add 0.01 mole of 1-methylbicyclo[2,2,1]hept-2-ene, 0.01 mole of octafluorocyclopentene and 0.01 mole of styrene into the autoclave that has been evacuated several times and filled with nitrogen, and add 20ml of toluene dissolve. The amount of neodymium trichloride in the catalyst is 0.09% of the total weight of norbornene, octafluorocyclopentene, and styrene. Take the above-mentioned neodymium-zinc complex catalyst and inject it into the above-mentioned mixture with a syringe. The reaction was carried out at a constant temperature of 20° C. and...

Embodiment 3

[0030] Dissolve 0.001 mol of neodymium trichloride, 0.010 mol of diethyl zinc and 0.005 mol of phenanthroline in 10 ml of tetrahydrofuran, put them into a single-necked glass bottle that has been vacuum-pumped several times, filled with nitrogen and baked and dried. Seal the latex tube, put it into a constant temperature water bath at 45°C for 25 minutes, and obtain the neodymium-zinc complex catalyst.

[0031] Add 0.01 mole of 5-methylbicyclo[2,2,1]hept-2-ene, 0.01 mole of octafluorocyclopentene and 0.01 mole of styrene into the autoclave that has been evacuated several times and filled with nitrogen, and add 20ml of tetrahydrofuran dissolve. The amount of neodymium trichloride in the catalyst is 0.10% of the total weight of norbornene, octafluorocyclopentene, and styrene. Take the above-mentioned neodymium-zinc complex catalyst and inject it into the above-mentioned mixture with a syringe. The reaction was carried out at a constant temperature of 50°C and a pressure of 0.9 ...

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Abstract

The invention relates to a ternary polymerization catalyst of norbornene, octafluorocyclopentene and styrene and a ternary polymerization method, wherein the catalyst is prepared through a following method comprising steps of: 1) dissolving neodymium trichloride, diethyl zinc and a ligand compound in a first solvent in a dried single-mouth glass bottle under an inert gas atmosphere; 2) sealing the mouth of the bottle by a latex pipe, performing a reaction at a constant temperature of 40-60 DEG C for 20-30 min to prepare a neodymium/zinc complex catalyst; 3) according to a ratio of 1:1:1, adding a norbornene monomer, an octafluorocyclopentene monomer and a styrene monomer into a high-pressure kettle which is vacuumized for several times and is filled with nitrogen, and adding a second solvent to dissolve the raw materials; 4) adding the neodymium/zinc complex catalyst, and carrying out a reaction at 20-90 DEG C for 0.1-6 MPa for 1-6 h; and 5) washing a reaction product to obtain a terpolymer. The raw materials of the catalyst are low in cost and are easy to obtain. The catalyst can generate catalytic activity at a low temperature and is high in catalytic efficiency. A product is very easy to wash and separate and the method is high in yield of the co-polymer.

Description

technical field [0001] The present invention relates to the field of high polymers, specifically a catalyst for norbornene, octafluorocyclopentene and styrene ternary polymers and a norbornene, octafluorocyclopentene and styrene ternary polymer the 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 ma...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F232/08C08F212/08C08F232/04C08F4/52C07F19/00
Inventor 房江华李正辉杨建平徐卫红胡每杰高浩其
Owner NINGBO UNIVERSITY OF TECHNOLOGY
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