Catalyst for use in ternary polymerization of norbornene, maleic anhydride and cyclohexene and ternary polymerization method

A cyclohexene ternary and norbornene technology, which is applied in the field of maleic anhydride, norbornene, and cyclohexene ternary copolymerization, can solve the problems of low copolymer yield, unreached yield, long reaction time, etc. , to achieve the effect of high copolymer yield, low reaction temperature and high catalytic efficiency

Inactive Publication Date: 2012-10-03
NINGBO UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The existing norbornene, maleic anhydride, acrylic acid ester or styrene copolymers are mainly synthesized by free radical polymerization, and the reaction time is long and the yield of the copolymer is obtained in the synthesis pro

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Add 20 ml of tetrahydrofuran, 0.01 mol of ferric chloride, 0.10 mol of 8-hydroxyquinoline, and 0.10 mol of triethylaluminum to a one-mouth glass bottle that has been evacuated several times and baked with nitrogen. Keep the temperature constant for 30 minutes, and then obtain the iron complex catalyst after cooling.

Embodiment 2

[0029] In a single-necked glass bottle that has been evacuated several times and baked with nitrogen, add 20 ml of anisole, 0.01 mol of ferric chloride, 0.08 mol of α,α,-bipyridine and 0.10 mol of triisobutylaluminum, Keep the temperature in a water bath at 50°C for 30 minutes, and then obtain the iron complex catalyst after cooling.

[0030] Add 0.024 moles of bicyclic 1-methylbicyclo[2,2,1]hept-2-ene, 0.024 moles of maleic anhydride, and 0.024 moles of 3-methylcyclohexene into a 25ml nitrogen-filled single-port polymerization bottle, and add 5ml of toluene was dissolved. Take 1% of the above-mentioned catalyst according to the total weight of norbornene, maleic anhydride and cyclohexene, and inject it into the above-mentioned mixture with a syringe. Put it into a constant temperature water tank, and react at 70° C. for 2 hours. The product was poured into methanol solution containing 5% hydrochloric acid to precipitate the terpolymer of norbornene, maleic anhydride and cyc...

Embodiment 3

[0032] Add 20 ml of 1,4-dioxane, 0.01 mol of ferric chloride, 0.07 mol of phenanthroline and 0.08 mol of triethylzinc into a single-mouthed glass bottle that has been evacuated several times and baked with nitrogen. , keep the temperature in a water bath at 50°C for 20 minutes, and after cooling, the iron complex catalyst is obtained.

[0033] Add 0.024 moles of bicyclic 5-methylbicyclo[2,2,1]hept-2-ene, 0.024 moles of maleic anhydride, and 0.024 moles of 4-methylcyclohexene into a 25ml nitrogen-filled single-port polymerization bottle, and add 5ml of toluene was dissolved. Take 0.1% of the above catalyst according to the total weight of norbornene, maleic anhydride and cyclohexene, and inject it into the above mixture with a syringe. Put it into a constant temperature water bath, and react at 60° C. for 2 hours. The product was poured into methanol solution containing 5% hydrochloric acid to precipitate the terpolymer of norbornene, maleic anhydride and cyclohexene. The pre...

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PUM

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Abstract

The invention relates to a catalyst for use in ternary polymerization of norbornene, maleic anhydride and cyclohexene and a ternary polymerization method. The catalyst is characterized by being prepared by using a method comprising the following steps of: dissolving ferric trichloride, a ligand and an alkyl metal compound into a first solvent, putting into a dry single-mouth glass bottle in an inert atmosphere, sealing a bottleneck with a latex tube, preserving heat in a water bath of 50 DEG C for 20-30 minutes, and cooling to obtain an iron complex catalyst; adding norbornene, maleic anhydride and cyclohexene into a dry single-mouth glass bottle in an inert atmosphere, adding a second solvent into the single-mouth glass bottle, dissolving, and sealing the bottleneck; adding the iron complex catalyst into the single-mouth glass bottle, and reacting at the constant temperature of 40-100 DEG C for 2-3 hours; and precipitating an obtained reaction product, washing and drying to obtain a norbornene-maleic anhydride-cyclohexene terpolymer. The catalyst provided by the invention can be used for catalyzing polymerization under the normal pressure at a low temperature, and the copolymer yield is high.

Description

technical field [0001] The present invention relates to the field of polymer synthesis, specifically a catalyst for ternary copolymerization of norbornene, maleic anhydride and cyclohexene and the use of the catalyst for ternary copolymerization of norbornene, maleic anhydride and cyclohexene Methods. 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 polynorbornene are poor brittleness, poor viscosity and low molecular weight. After inserting maleic anhydride and cyclohexene into the main chain of polynorbornene, it can improve the cohesiveness and solubility of the polymer, so that it has a high glass transition temperature and improves its fragility in film formation , and can reduce the absorbance of the material itself, this copolymer can be used as a photoresist material in ...

Claims

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Application Information

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IPC IPC(8): C08F232/08C08F222/06C08F232/04C08F4/70
Inventor 房江华高浩其胡敏杰肖勋文杨建平
Owner NINGBO UNIVERSITY OF TECHNOLOGY
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