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Norbornene, hexafluoropropylene and 1-hexene ternary copolymerization catalyst and ternary copolymerization method

A hexene ternary copolymerization catalyst and the technology of norbornene are applied in the field of high polymer synthesis catalyst and high polymer synthesis, which can solve the problems of low copolymer yield, few researches, and small molecular weight of the copolymer, and achieve The effect of high copolymer yield, easy washing and separation, and low reaction temperature

Active Publication Date: 2016-04-27
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. At present, studies on the ternary copolymerization of norbornene, hexafluoropropylene and 1-hexene have been carried out. rare

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Take 0.001 mole of pentapentyl iron, 0.001 mole of titanium tetrachloride and 0.001 mole of 8-hydroxyquinoline and dissolve them in 10 ml of benzene, put them into a single-necked glass bottle that has been evacuated several times, filled with nitrogen and baked and dried. Seal the latex tube and put it into a constant temperature water bath at 20°C for 20 minutes to obtain the iron-titanium complex catalyst.

[0024] Add 0.01 mole of bicyclo[2,2,1]hept-2-ene, 0.01 mole of hexafluoropropylene and 0.01 mole of 1-hexene into an autoclave that has been evacuated several times and filled with nitrogen, and dissolved in 20 ml of benzene. The amount of dipentyl iron in the catalyst is 0.02% of the total weight of norbornene, hexafluoropropylene, and 1-hexene. Take the above-mentioned iron-titanium complex catalyst and inject it into the above-mentioned mixture with a syringe. The temperature was kept at 60° C. and the pressure was 0.1 MP, and the reaction was carried out for ...

Embodiment 2

[0027] Dissolve 0.001 mole of pentapentyl iron, 0.010 mole of titanium tetrachloride and 0.004 mole of α, α'-bipyridine in 10 ml 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 with a latex tube, put it into a constant temperature water bath at 50°C for 30 minutes, and obtain the iron-titanium complex catalyst.

[0028] Add 0.01 mole of 1-methylbicyclo[2,2,1]hept-2-ene, 0.01 mole of 0.01 mole of hexafluoropropylene, and 0.01 mole of 1-hexene into an autoclave evacuated several times and filled with nitrogen, and add 20ml of toluene was dissolved. The amount of dipentyl iron in the catalyst is 0.1% of the total weight of norbornene, hexafluoropropylene, and 1-hexene. Take the above-mentioned iron-titanium complex catalyst and inject it into the above-mentioned mixture with a syringe. The temperature was kept at 30°C and the pressure was 4MP, and the reaction was carried out for 6...

Embodiment 3

[0030] Dissolve 0.001 mole of pentapentyl iron, 0.002 mole of titanium tetrachloride and 0.008 mole of phenanthroline in 10 ml of tetrahydrofuran, put them into a single-necked glass bottle that has been evacuated several times, filled with nitrogen and baked dry, and the mouth of the bottle is made of latex The tube was sealed and placed in a constant temperature water bath at 40°C for 25 minutes to obtain an iron-titanium complex catalyst.

[0031] Add 0.01 mole of 5-methylbicyclo[2,2,1]hept-2-ene, 0.01 mole of hexafluoropropylene and 0.01 mole of 1-hexene into a vacuum-evacuated and nitrogen-filled autoclave, add 20ml of tetrahydrofuran dissolve. The amount of dipentyl iron in the catalyst is 0.3% of the total weight of norbornene, hexafluoropropylene, and 1-hexene. Take the above-mentioned iron-titanium complex catalyst and inject it into the above-mentioned mixture with a syringe. Constant temperature at 100°C, under 7MP pressure, react for 5 hours. The product was pour...

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Abstract

The invention relates to a norbornene, hexafluoropropylene and 1-hexene ternary copolymerization catalyst and a ternary copolymerization method. The catalyst is characterized in that a preparation method of the catalyst includes: in a dry single-opening glass bottle in an inert atmosphere, dissolving ferrocene, titanium tetrachloride and a ligand in a first solvent; using a latex tube to seal the opening of the bottle; maintaining constant temperature at 20-50 DEG C for 20-50 min to obtain an iron-titanium complex catalyst; the ternary copolymerization method includes: taking and adding norbornene, hexafluoropropylene and 1-hexene monomer according to a molar ratio of 1:1:1 into a high-pressure kettle vacuumized for many times and filled with nitrogen, and adding a second solvent for dissolution; adding the iron-titanium complex catalyst for reaction at 30-130 DEG C for 2-6 h. Raw materials of the catalyst are low in cost and easy to get, the catalyst can generate catalytic activity at low temperature and is low in reaction temperature and high in catalytic efficiency, and a product can be washed and separated quite easily and high in copolymer yield.

Description

technical field [0001] The invention relates to a high polymer synthesis catalyst and high polymer synthesis, specifically a catalyst for ternary copolymerization of norbornene, hexafluoropropylene and 1-hexene 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 inserting hexafluoropropylene and maleic anhydride into the main chain of polynorbornene, the cohesiveness and solubility of the polymer can be improved, and after fluorine-containing alkenes are inserted into the main chain of polynorbornene, the cohesiveness of the polymer can be improved And solubility, and reduce the absorbance of the material itself. This terpolymer can be used as a photoresist material ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F232/08C08F214/28C08F210/14C08F4/80C08F4/76
CPCC08F210/14C08F214/285C08F232/08C08F4/80C08F4/76
Inventor 房江华高浩其胡敏杰
Owner NINGBO UNIVERSITY OF TECHNOLOGY
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