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Norbornene, hexafluoropropylene and acrylonitrile ternary polymerization catalyst and ternary polymerization method

The technology of acrylonitrile terpolymerization catalyst and norbornene is applied in the field of high polymer, which can solve the problems of small molecular weight of copolymer, low copolymer alternating degree, low copolymer yield, etc. The effect of improved toughness and high yield of copolymer

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 of copolymer, small molecular weight of copolymer, low degree of alternation of copolymer, etc.

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, dissolve 0.001 mol of bis(pentamethylcyclopentadienyl) cerium chloride and 0.001 mol of 8-hydroxyquinoline in 10 ml of benzene, and stir at a rate of 120 revolutions per minute. 0.001 mole of titanium tetrachloride was dropped into the above solution, and then stirred at the same stirring rate at 30°C for 30 minutes at a constant temperature to obtain a cerium-titanium complex catalyst.

[0026] Add 0.01 mole of bicyclo[2,2,1]hept-2-ene, 0.01 mole of hexafluoropropylene and 0.01 mole of acrylonitrile into an autoclave evacuated several times and filled with nitrogen, and add 20 ml of benzene to dissolve. According to the amount of bis(pentamethylcyclopentadienyl) cerium chloride in the catalyst, it is 0.01% of the total weight of norbornene, hexafluoropropylene and acrylonitrile to get the above-mentioned cerium-titanium complex catalyst, and use a syringe Pour into the above mixture. React at a constant temperature ...

Embodiment 2

[0029] In a three-necked flask with a dry inert atmosphere, dissolve 0.001 mol of bis(pentamethylcyclopentadienyl) cerium chloride and 0.004 mol of α, α'-bipyridine in 10 ml of toluene at 120 rpm Under high-speed stirring, 0.003 mol of titanium tetrachloride was dropped into the above solution, and then stirred at the same stirring rate of 40° C. for 40 minutes at a constant temperature to obtain a cerium-titanium complex catalyst.

[0030] Add 0.01 mole of bicyclo[2,2,1]hept-2-ene, 0.01 mole of hexafluoropropylene and 0.01 mole of acrylonitrile into an autoclave evacuated several times and filled with nitrogen, and add 20 ml of toluene to dissolve. According to the amount of bis(pentamethylcyclopentadienyl) cerium chloride in the catalyst, it is 0.05% of the total weight of norbornene, hexafluoropropylene and acrylonitrile to get the above-mentioned cerium-titanium complex catalyst, and use a syringe Pour into the above mixture. React at a constant temperature of 110° C. and...

Embodiment 3

[0032] In a three-necked flask with a dry inert atmosphere, dissolve 0.001 mole of bis(pentamethylcyclopentadienyl) cerium chloride and 0.010 mole of phenanthroline in 10 milliliters of tetrahydrofuran, and stir at a rate of 110 revolutions per minute. , drop 0.004 moles of titanium tetrachloride into the above solution, and then stir at the same stirring rate at 30°C for 50 minutes at a constant temperature to obtain a cerium-titanium complex catalyst.

[0033] Add 0.01 mole of 1-methylbicyclo[2,2,1]hept-2-ene, 0.01 mole of hexafluoropropylene and 0.01 mole of acrylonitrile into an autoclave evacuated several times and filled with nitrogen, and add 20 ml of tetrahydrofuran to dissolve. According to the amount of bis(pentamethylcyclopentadienyl) cerium chloride in the catalyst, it is 1.0% of the total weight of norbornene, hexafluoropropylene and acrylonitrile to get the above-mentioned cerium-titanium complex catalyst, and use a syringe Pour into the above mixture. The react...

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Abstract

The invention relates to a norbornene, hexafluoropropylene and acrylonitrile ternary polymerization catalyst. The preparation method of the catalyst comprises the steps that (pentamethyl cyclopentadiene) cerium chloride and a ligand are dissolved into a first solvent in a dry three-mouth flask in the inertia atmosphere, titanium tetrachloride is dropped into the solution while stirring is performed, stirring is performed at the constant temperature of 30-60 DEG C for 30-60 min after dropping is performed, and a cerium-titanium complex catalyst is obtained. The polymerization method comprises the steps that a norbornene monomer, a hexafluoropropylene monomer and an acrylonitrile monomer are taken and added into a reaction kettle where repeated vacuumizing and nitrogen charging are performed, and a second solvent is added for dissolution; then, the cerium-titanium complex catalyst is added, a reaction is performed under the certain temperature and pressure, and the product is washed to obtain the terpolymer. Catalyst raw materials are low in price and easy to obtain, catalytic activity can be generated at low temperature, norbornene, hexafluoropropylene and acrylonitrile 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 the field of high polymers, in particular to a ternary copolymerization catalyst of norbornene, hexafluoropropylene and acrylonitrile 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, tetrafluoroethylene, st...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F232/08C08F214/28C08F220/44C08F4/76
CPCC08F4/76C08F214/28C08F220/44C08F232/08
Inventor 房江华李正辉胡敏杰高浩其
Owner NINGBO UNIVERSITY OF TECHNOLOGY
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