Norbornene, styrene and nikasol ternary polymerization catalyst and ternary polymerization method

A vinyl acetate ternary copolymerization catalyst and vinyl acetate technology, applied in the field of high polymer synthesis catalyst and high polymer synthesis, can solve the problems of low degree of alternation of copolymers, small molecular weight of copolymers, low yield of copolymers, etc. , to achieve the effects of improved solubility and toughness, low reaction temperature and high copolymer yield

Active Publication Date: 2016-06-22
NINGBO UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Existing synthetic methods all have disadvantages such as long reaction time, low yield

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] In a three-necked flask with a dry inert atmosphere, 0.001 moles of (pentamethylcyclopentadiene) iridium chloride, 0.001 moles of triisobutylaluminum and 0.001 moles of 8-hydroxyquinoline were dissolved in 10 milliliters of benzene, with each Minutes at 120 rpm and constant temperature stirring at 20°C for 20 minutes to obtain an iridium-aluminum complex catalyst.

[0026] Add 0.01 mole of bicyclo[2,2,1]hept-2-ene, 0.01 mole of styrene and 0.01 mole of vinyl acetate into an autoclave evacuated several times and filled with nitrogen, and add 20ml of benzene to dissolve. According to the amount of (pentamethylcyclopentadiene) iridium chloride in the catalyst, it is 0.01% of the total weight of norbornene, styrene, and vinyl acetate to get the above-mentioned iridium-aluminum complex catalyst, and inject the above-mentioned in the mixture. React at a constant temperature of 80° C. and a pressure of 0.1 MPa for 5 hours. The product is poured into an ethanol solution conta...

Embodiment 2

[0029] In a three-necked flask with a dry inert atmosphere, 0.001 moles of (pentamethylcyclopentadiene) iridium chloride, 0.012 moles of triethylaluminum and 0.006 moles of α, α'-bipyridine were dissolved in 10 ml of toluene to 120 revolutions per minute, stirring at a constant temperature of 50°C for 50 minutes to obtain an iridium-aluminum complex catalyst.

[0030] Add 0.01 mole of 1-methylbicyclo[2,2,1]hept-2-ene, 0.01 mole of styrene and 0.01 mole of vinyl acetate into an autoclave evacuated several times and filled with nitrogen, and add 20ml of toluene to dissolve. According to the amount of (pentamethylcyclopentadiene) iridium chloride in the catalyst, it is 1.5% of the total weight of norbornene, styrene, and vinyl acetate to get the above-mentioned iridium-aluminum complex catalyst, and inject the above-mentioned in the mixture. React at a constant temperature of 120°C and a pressure of 8 MPa for 6 hours. The product is poured into an ethanol solution containing 5w...

Embodiment 3

[0032] In a three-necked flask with a dry inert atmosphere, 0.001 moles of (pentamethylcyclopentadiene) iridium chloride, 0.006 moles of triisobutylaluminum and 0.008 moles of phenanthroline were dissolved in 10 milliliters of tetrahydrofuran at a rate of Stir at 120 rpm at 30°C for 40 minutes at a constant temperature to obtain an iridium-aluminum complex catalyst.

[0033] Add 0.01 mole of 5-methylbicyclo[2,2,1]hept-2-ene, 0.01 mole of styrene and 0.01 mole of vinyl acetate into an autoclave evacuated several times and filled with nitrogen, and add 20 ml of tetrahydrofuran to dissolve. According to the amount of (pentamethylcyclopentadiene) iridium chloride in the catalyst, it is 0.5% of the total weight of norbornene, styrene, and vinyl acetate to get the above-mentioned iridium-aluminum complex catalyst, and inject the above-mentioned in the mixture. React at a constant temperature of 150° C. and a pressure of 10 MPa for 4 hours. The product is poured into an ethanol sol...

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PUM

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Abstract

The invention relates to a norbornene, styrene and nikasol ternary polymerization catalyst and a ternary polymerization method. The preparation method of the catalyst comprises the steps that (pentamethyl cyclopentadiene) iridium chloride, aluminum alkyl and a ligand are dissolved into a first solvent in a dry three-mouth flask in the inertia atmosphere, stirring is performed at the constant temperature of 20-50 DEG C at the speed of 110-130 rpm for 20-50 min, and an iridium-aluminum complex catalyst is obtained. The polymerization method comprises the steps that a norbornene monomer, a styrene monomer and a nikasol monomer are taken and added into a reaction kettle, and a second solvent is added for dissolution; then, the iridium-aluminum complex catalyst is added, a reaction is performed under the certain stable pressure, and the product is washed to obtain the terpolymer. Catalytic activity can be generated at low temperature, norbornene, styrene and nikasol ternary polymerization is catalyzed, the reaction temperature is low, the catalysis efficiency is high, the copolymer yield is high, and the terpolymer is good in photoetching performance.

Description

technical field [0001] The invention relates to a high polymer synthesis catalyst and high polymer synthesis, specifically a norbornene, styrene and vinyl acetate ternary copolymerization catalyst 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. Cohesion and solubility of the polymer are usually improved by copolymerization with other materials, and the light absorption rate of the material itself is reduced. [0003] At present, the preparation methods of norbornene copolymer mainly include methods such as free radicals, active free radicals, and metal catalysts. For example, A.E.Feiring and Q.Feng et al. carry out four-membered copolymerization of norbornene, tetraflu...

Claims

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Application Information

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IPC IPC(8): C08F232/08C08F212/08C08F218/08C08F4/80C08F4/52
CPCC08F212/08C08F218/08C08F232/08C08F4/80C08F4/52
Inventor 房江华高浩其胡敏杰
Owner NINGBO UNIVERSITY OF TECHNOLOGY
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