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Norbornene, maleic anhydride and n-phenylmaleimide ternary copolymerization catalyst and ternary copolymerization method

A technology of maleimide ternary and norbornene, which is applied in the field of polymers, can solve the problems of low degree of copolymer alternation, small molecular weight of copolymers, and low yield of copolymers, and achieve improved solubility and toughness, The effect of low reaction temperature and high copolymer yield

Active Publication Date: 2019-05-07
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] In a glove box under a nitrogen atmosphere, 0.001 mol of [1,1'-bis(diphenylphosphino)ferrocene]palladium dichloride and 0.001 mol of 8-hydroxyquinoline were dissolved in 10 ml of benzene in an Erlenmeyer flask. , at 250rpm, under stirring with a magnetic stirrer, drop 0.003 moles of tetraisopropoxytitanium into the above solution, stir at the same stirring rate at 20°C for 30 minutes at a constant temperature after dripping, evaporate 5ml of benzene, and let stand for 5 hours, solid crystals were obtained, and the palladium-titanium complex catalyst was obtained by filtration.

[0025] Add 0.01 mole of bicyclo[2,2,1]hept-2-ene, 0.01 mole of maleic anhydride and 0.01 mole of N-phenylmaleimide to the single-port glass polymerization with vacuum pumping and nitrogen charging for several times In the bottle, add 20ml of benzene to dissolve. Get the above-mentioned palladium-titanium complex catalyst by 0.09% of the total weight of bicyclo[2,2,1]hept-2-ene, maleic anhydride...

Embodiment 2

[0028] In a glove box under a nitrogen atmosphere, 0.001 mol of [1,1'-bis(diphenylphosphino)ferrocene]palladium dichloride and 0.006 mol of α,α'-bipyridine were dissolved in a Erlenmeyer flask for 10 Milliliter of toluene, at 300rpm, under stirring with a magnetic stirrer, drop 0.005 mole of tetraisopropoxytitanium into the above solution, after the dripping, stir at the same stirring rate at 40°C for 40 minutes at a constant temperature, evaporate 7.5ml of toluene, After standing still for 2 hours, solid crystals were obtained, and the palladium-titanium complex catalyst was obtained by filtration.

[0029] Add 0.01 mole of bicyclo[2,2,1]hept-2-ene, 0.01 mole of maleic anhydride and 0.01 mole of N-phenylmaleimide to the single-port glass polymerization with vacuum pumping and nitrogen charging for several times Bottle, add 20ml toluene to dissolve. Get the above-mentioned palladium-titanium complex catalyst by 0.08% of the total weight of bicyclo[2,2,1]hept-2-ene, maleic anh...

Embodiment 3

[0031] In a glove box under a nitrogen atmosphere, 0.001 moles of [1,1'-bis(diphenylphosphino)ferrocene]palladium dichloride and 0.010 moles of phenanthrocene were dissolved in 10 milliliters of tetrahydrofuran in an Erlenmeyer flask, At 400rpm, under stirring with a magnetic stirrer, drop 0.004 moles of tetraisopropoxytitanium into the above solution, after the dripping, stir at a constant temperature at the same stirring rate of 30°C for 50 minutes, evaporate 7.5ml of tetrahydrofuran, and let it stand for 3 hours, solid crystals were obtained, and the palladium-titanium complex catalyst was obtained by filtration.

[0032]Add 0.01 mole of 1-methylbicyclo[2,2,1]hept-2-ene, 0.01 mole of maleic anhydride and 0.01 mole of N-phenylmaleimide to several times of vacuum pumping and nitrogen charging Add 20ml of tetrahydrofuran to dissolve in a single-necked glass polymerization bottle. Get the above-mentioned palladium-titanium complex catalyst by 0.07% of the three gross weights o...

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Abstract

The invention relates to a norbornene, maleic anhydride and N-phenyl maleimide ternary polymerization catalyst and a ternary polymerization method. The invention is characterized in that the preparation method of the catalyst includes: in a glove box of nitrogen atmosphere, dissolving [1, 1'-bis(diphenylphosphino)ferrocene]palladium dichloride and a ligand in a first solvent in a conical flask, adding titanium iso-propylate dropwise under magnetic stirring, then performing constant temperature stirring at 20-50DEG C under a same stirring rate, steaming off part of the first solvent, conducting standing for 2-5h, performing filtering to obtain solid crystals, i.e. a palladium-titanium complex catalyst, adding a norbornene monomer, maleic anhydride and an N-phenyl maleimide monomer in a ratio of 1:1:1 into a single-mouth glass polymerization bottle subjected to repeated vacuum pumping and nitrogen charged baking, and adding a second solvent for dissolving; and then adding the palladium-titanium complex catalyst for reaction, washing the product to obtain precipitate, i.e. a norbornene, maleic anhydride and N-phenyl maleimide terpolymer.

Description

technical field [0001] The invention relates to the field of high polymers, in particular to a ternary copolymerization catalyst of norbornene, maleic anhydride 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 193nm ultraviolet lithography. The main disadvantages of this material are brittleness, poor viscosity and low molecular weight. After the oxygen-containing compound is inserted into the main chain of polynorbornene, the cohesiveness and solubility of the polymer can be improved, and the light absorption rate of the material itself can be reduced. This copolymer can be used as a photoresist material in 193nm photolithography. 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): C08F232/08C08F222/06C08F222/40C08F4/70
CPCC08F4/70C08F222/06C08F222/40C08F232/08
Inventor 史玉立李正辉王江波胡敏杰高浩其房江华杨建平王志强
Owner NINGBO UNIVERSITY OF TECHNOLOGY