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Norbornene, acrylonitrile and vinyl acetate ternary polymerization catalyst and ternary polymerization method

A vinyl acetate ternary copolymerization catalyst and vinyl acetate ternary technology, applied in the field of high polymers, can solve the problems of small molecular weight of copolymers, low degree of alternation of copolymers, and low yield of copolymers, and achieve improved adhesion properties, low catalytic reaction temperature, and high copolymer yield

Active Publication Date: 2016-09-07
NINGBO UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, these synthetic methods all have the disadvantages of long reaction time, low yield of copolymer, small molecular weight of copolymer, and low degree of alternation of copolymer.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] In a three-necked flask with a dry inert atmosphere, dissolve 0.001 mol of tris(dibenzylideneacetone) dipalladium, 0.001 mol of 8-hydroxyquinoline and 0.001 mol of titanium tetrachloride in 10 ml of benzene, and stir with an electric stirrer , and stirred at 170 rpm at 20°C for 20 minutes at a constant temperature to obtain a palladium-titanium complex catalyst.

[0025] Add 0.01 mole of bicyclo[2,2,1]hept-2-ene, 0.01 mole of acrylonitrile 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 tris(dibenzylideneacetone) dipalladium in the catalyst, it is 0.01% of the total weight of norbornene, acrylonitrile and vinyl acetate. Take the above-mentioned palladium-titanium complex catalyst and inject the above-mentioned mixture with a syringe. middle. React at a constant temperature of 90° C. and a pressure of 0.1 MPa for 4 hours. The product is poured into an etha...

Embodiment 2

[0028] In a three-necked flask with a dry inert atmosphere, 0.001 mol of tris(dibenzylideneacetone) dipalladium, 0.006 mol of α, α'-bipyridine and 0.004 mol of titanium tetrachloride were dissolved dropwise in 10 ml of toluene, and the Stir with an electric stirrer, and stir at a constant temperature of 140 rpm and 50° C. for 40 minutes to obtain a palladium-titanium complex catalyst.

[0029] Add 0.01 mole of bicyclo[2,2,1]hept-2-ene, 0.01 mole of acrylonitrile 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 tris(dibenzylideneacetone) dipalladium in the catalyst, it is 0.06% of the total weight of norbornene, acrylonitrile and vinyl acetate. Take the above-mentioned palladium-titanium complex catalyst and inject the above-mentioned mixture with a syringe. middle. React at a constant temperature of 140° C. and a pressure of 6 MPa for 7 hours. The product is pour...

Embodiment 3

[0031] In a three-necked flask with a dry inert atmosphere, 0.001 moles of tris(dibenzylideneacetone) dipalladium, 0.008 moles of phenanthroline and 0.003 moles of titanium tetrachloride were dissolved in 10 milliliters of tetrahydrofuran, and stirred with an electric stirrer, Stir at 160 rpm and 30° C. for 50 minutes at a constant temperature to obtain a palladium-titanium complex catalyst.

[0032] Add 0.01 mole of 1-methylbicyclo[2,2,1]hept-2-ene, 0.01 mole of acrylonitrile 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 tris(dibenzylideneacetone) dipalladium in the catalyst, it is 1.0% of the total weight of norbornene, acrylonitrile and vinyl acetate. Take the above-mentioned palladium-titanium complex catalyst and inject the above-mentioned mixture with a syringe. middle. The reaction was carried out at a constant temperature of 120° C. and a press...

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PUM

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Abstract

The invention relates to a norbornene, acrylonitrile and vinyl acetate ternary polymerization catalyst and a ternary polymerization method. The preparation method of the catalyst is characterized by comprising the following steps that tris(dibenzylideneacetone)dipalladium, a ligand and titanium tetrachloride are dissolved into a first solvent in a three-mouth flask in a dry inert atmosphere, an electric stirrer is installed to stir the materials, constant-temperature stirring is conducted for 20 min to 60 min at the speed of 130 rpm to 170 rpm at the temperature of 20 DEG C to 60 DEG C, and then a palladium-titanium complex catalyst is obtained; norbornene, acrylonitrile and vinyl acetate monomers are taken according to the molar ratio of 1:1:1, added into a high-pressure kettle which is vacuumized and subjected to nitrogen filling for many times and dissolved by adding a second solvent; the palladium-titanium complex catalyst is added, and reacting is conducted for 1 hour to 8 hours at the temperature of 20 DEG C to 150 DEG C under the pressure of 0.1 MPa to 8 MPa; a product obtained through reacting is poured into an ethanol solution containing 4 wt%-5 wt% of hydrochloric acid, an obtained precipitate is washed with ethanol until the precipitate is neutral, vacuum drying is conducted, and then the norbornene, acrylonitrile and vinyl acetate terpolymer is obtained.

Description

technical field [0001] The invention relates to the field of high polymers, in particular to a ternary copolymerization catalyst of norbornene, acrylonitrile and vinyl acetate 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. [0003] At present, the methods for synthesizing norbornene-based copolymers mainly include free radicals, active free radicals, and metal catalysts. For example, A.E.Feiring and Q.Feng etc. carried out ternary copolymerization of norbornene with tetrafluoroethylene, styrene, and acrylate by free radical method, the photolithographic material disclosed in Proceedings of SPIE Vol.5039 (2003) pages 80-92 The synthesis of the peroxide is used as the c...

Claims

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Application Information

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IPC IPC(8): C08F4/80C08F232/08C08F220/44C08F218/08
CPCC08F4/80C08F218/08C08F220/44C08F232/08
Inventor 房江华胡敏杰高浩其
Owner NINGBO UNIVERSITY OF TECHNOLOGY
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