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Ternary polymerization catalyst and ternary polymerization method for norbornylene, vinylacetate and octafluorocyclopentene

An octafluorocyclopentene ternary copolymerization catalyst and technology of ternary copolymerization catalysts, which are applied in the field of high polymers, can solve the problems of little research, low yield of copolymers, and low degree of alternation of copolymers, and achieve easy washing Separation, high copolymer yield, and high catalytic efficiency

Inactive Publication Date: 2015-01-07
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 copolymer, small molecular weight of copolymer, low degree of copolymer alternation, etc. little research

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Get 0.001 mole of tris(cyclopentadiene) praseodymium, 0.004 mole of two (triphenylphosphine) nickel chloride and 0.003 mole of α, α,-bipyridine is dissolved in 10 milliliters of cyclohexanone, put into after repeatedly pumping Vacuum and nitrogen-filled single-mouth glass bottle, the bottle mouth is sealed with a latex tube, put into a constant temperature water tank at 50°C for 30 minutes, and the praseodymium-nickel complex ternary copolymerization catalyst is obtained.

[0024] Add 0.01 mole of bicyclo[2,2,1]hept-2-ene, 0.01 mole of vinyl acetate and 0.01 mole of octafluorocyclopentene into a nitrogen-filled and dried autoclave, and add 20ml of cyclohexanone to dissolve. According to the amount of three (cyclopentadiene) praseodymium in the catalyst, it is 1% of norbornene, vinyl acetate, octafluorocyclopentene three gross weights to get the above-mentioned praseodymium-nickel complex ternary copolymerization catalyst, use Syringe into the above mixture. Constant te...

Embodiment 2

[0027] Get 0.001 mole of tris(cyclopentadiene) praseodymium, 0.001 mole of two (triphenylphosphine) nickel chloride and 0.006 mole of α, α,-bipyridine is dissolved in 10 milliliters of toluene, put into after repeatedly vacuumizing, In a one-mouth glass bottle filled with nitrogen and baked, the bottle mouth is sealed with a latex tube, put into a constant temperature water bath at 50°C for 30 minutes, and the praseodymium-nickel complex ternary copolymerization catalyst is obtained.

[0028] Add 0.01 mol of bicyclo[2,2,1]hept-2-ene, 0.01 mol of vinyl acetate and 0.01 mol of octafluorocyclopentene into the autoclave that has been filled with nitrogen and dried, and add 20ml of toluene to dissolve. According to the amount of three (cyclopentadiene) praseodymium in the catalyst, it is 1% of norbornene, vinyl acetate, octafluorocyclopentene three gross weights to get the above-mentioned praseodymium-nickel complex ternary copolymerization catalyst, use Syringe into the above mixt...

Embodiment 3

[0030] Take 0.001 mole of tris(cyclopentadiene)praseodymium, 0.002 mole of bis(triphenylphosphine)nickel chloride and 0.008 mole of ethyl acetoacetate and dissolve them in 10 ml of benzene, put them into a vacuum-pumped, nitrogen-charged oven for several times. In a baked single-mouth glass bottle, the bottle mouth is sealed with a latex tube, put into a constant temperature water tank at 50°C for 30 minutes, and the praseodymium-nickel complex ternary copolymerization catalyst is obtained.

[0031] Add 0.01 mole of 1-methylbicyclo[2,2,1]hept-2-ene, 0.01 mole of vinyl acetate and 0.01 mole of octafluorocyclopentene into a nitrogen-filled autoclave, and add 20ml of benzene to dissolve. According to the amount of three (cyclopentadiene) praseodymium in the catalyst, it is 2% of norbornene, vinyl acetate, octafluorocyclopentene three gross weights to get the above-mentioned praseodymium-nickel complex ternary copolymerization catalyst, use Syringe into the above mixture. Constan...

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PUM

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Abstract

The invention relates to a ternary polymerization catalyst and a ternary polymerization method for norbornylene, vinylacetate and octafluorocyclopentene. The ternary polymerization catalyst is prepared by steps as follows: tris(cyclopentadienyl)praseodymium, bis(triphenylphosphine)nickel(II)chloride, a ligand and a first solvent are placed in a dry single-ported glass bottle filled with inert gas, a bottle mouth is sealed by a latex tube, the constant temperature in a range from 45 DEG C to 55 DEG C is kept for 25-35 min, and after dissolving, the ternary polymerization catalyst is obtained. Co-monomers are taken in proportion, the catalyst is added, and terpolymers are obtained through reaction at certain temperature and pressure. The provided catalyst can generate catalytic activity in a nitrogen production system at the temperature of 50 DEG C-150 DEG C and under the pressure of 0.1 MPa-6 MPa and catalyze ternary polymerization of norbornylene, vinylacetate and octafluorocyclopentene, and a polymerization product is very easy to wash and separate; the copolymer yield is high, the reaction temperature is low, raw materials of the catalyst are cheap and easy to obtain, and the catalytic efficiency is high.

Description

technical field [0001] The invention relates to the field of high polymers, in particular to a ternary copolymerization catalyst of norbornene, vinyl acetate and octafluorocyclopentene 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 photolithographic materials, and th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F4/70C08F4/52C08F232/08C08F218/08C08F232/04
Inventor 房江华王江波李正辉陈斌高浩其胡敏杰杨建平
Owner NINGBO UNIVERSITY OF TECHNOLOGY
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