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Norbornene, hexafluoropropylene and N-phenyl maleimide ternary polymerization catalyst and method

A maleimide ternary copolymerization catalyst and norbornene technology, which is applied in the field of high polymer synthesis catalyst and high polymer synthesis, can solve the problem of low degree of copolymer alternation, low yield of copolymer, and small molecular weight of copolymer and other problems, to achieve the effects of easy washing and separation, low reaction temperature and high catalytic efficiency

Active Publication Date: 2017-05-10
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 copolymer, small molecular weight of copolymer, low degree of alternation of copolymer, etc. Little research has been done on imine terpolymerization

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 atmosphere, dissolve 0.001 mole of molybdenum acetate and 0.001 mole of 8-hydroxyquinoline in 10 ml of benzene to obtain a mixed solution; install an electric stirrer to stir, and drop 0.001 mole of titanium tetrachloride into the mixture In the solution, stir at a constant temperature of 20° C. for 30 minutes after dripping to obtain a molybdenum-titanium complex catalyst.

[0023] Add 0.01 mole of bicyclo[2,2,1]hept-2-ene, 0.01 mole of hexafluoropropylene and 0.01 mole of N-phenylmaleimide to several vacuum-pumped, nitrogen-filled autoclaves, add 20ml Benzene dissolves. The amount of molybdenum acetate in the catalyst is 0.01% of the total weight of norbornene, hexafluoropropylene and N-phenylmaleimide. Take the above-mentioned molybdenum-titanium complex catalyst and inject it into the above-mentioned mixture with a syringe. . React at a constant temperature of 80° C. and a pressure of 0.1 MPa for 5 hours. The product is po...

Embodiment 2

[0026] In a three-necked flask with a dry inert atmosphere, dissolve 0.001 mole of molybdenum acetate and 0.006 mole of α, α'-bipyridine in 10 ml of toluene to obtain a mixed solution; install an electric stirrer to stir, and drop 0.004 mole of titanium tetrachloride Put it into the mixed solution, and stir it at 40°C for 40 minutes after dropping, to obtain the molybdenum-titanium complex catalyst.

[0027] Add 0.01 mole of bicyclo[2,2,1]hept-2-ene, 0.01 mole of hexafluoropropylene and 0.01 mole of N-phenylmaleimide to several vacuum-pumped, nitrogen-filled autoclaves, add 20ml Toluene dissolves. The amount of molybdenum acetate in the catalyst is 0.06% of the total weight of norbornene, hexafluoropropylene and N-phenylmaleimide. Take the above molybdenum-titanium complex catalyst and inject it into the above mixture with a syringe. . React at a constant temperature of 140° C. and a pressure of 5 MPa for 6 hours. The product is poured into an ethanol solution containing 5w...

Embodiment 3

[0029] In a dry three-necked flask with an inert atmosphere, dissolve 0.001 mole of molybdenum acetate and 0.010 mole of phenanthroline in 10 ml of tetrahydrofuran to obtain a mixed solution; install an electric stirrer to stir, and drop 0.004 mole of titanium tetrachloride into the mixed solution After dripping, stir at a constant temperature of 30°C for 50 minutes to obtain a molybdenum-titanium complex catalyst.

[0030] Add 0.01 mol of 1-methylbicyclo[2,2,1]hept-2-ene, 0.01 mol of hexafluoropropylene and 0.01 mol of N-phenylmaleimide into a vacuum-evacuated, nitrogen-filled autoclave In, add 20ml tetrahydrofuran to dissolve. The amount of molybdenum acetate in the catalyst is 1.0% of the total weight of norbornene, hexafluoropropylene and N-phenylmaleimide. Take the above-mentioned molybdenum-titanium complex catalyst and inject it into the above-mentioned mixture with a syringe. . The reaction was carried out at a constant temperature of 120° C. and a pressure of 8 MPa ...

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Abstract

The invention relates to a norbornene, hexafluoropropylene and N-phenyl maleimide ternary polymerization catalyst and method. The ternary polymerization catalyst and method is characterized in that a preparation method of the catalyst includes: dissolving molybdenum acetate and ligand in a first solvent in a dry three-mouth flask with inert atmosphere to obtain a mixed solution; dropping titanium tetrachloride into the mixed solution at 150-250rpm, and stirring at 20-50 DEG C for 20-50min after dropping to obtain a molybdenum-titanium complex catalyst; adding norbornene monomer, hexafluopropylene and N-phenyl maleimide monomer into a high-pressure kettle which is vacuumized and nitrogenized several times according to a molar ratio of 1:1:1, and adding a second solvent for dissolving; adding the molybdenum-titanium complex catalyst, and allowing reaction at 30-150 DEG C and 0.1-8MPa for 1-6h; washing a reaction product, washing obtained precipitate to neutral, and vacuum drying to obtain norbornene, hexafluoropropylene and N-phenyl maleimide ternary copolymer.

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 N-phenylmaleimide, 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 copolymers as...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F232/08C08F214/28C08F222/40C08F4/78C08F4/76
CPCC08F4/76C08F4/78C08F214/28C08F222/40C08F232/08
Inventor 胡敏杰李颖房江华高浩其
Owner NINGBO UNIVERSITY OF TECHNOLOGY
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