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Catalyst for norbornene, acrylate and pentene copolymerization, and copolymerization method

A technology of acrylates and norbornene is applied in the field of high polymer synthesis, which can solve the problems of low yield of copolymer, unachieved yield, long reaction time and the like, and achieves high yield of copolymer, low reaction temperature, The effect of high catalytic efficiency

Inactive Publication Date: 2013-10-23
NINGBO UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The synthesis of existing norbornene, maleic anhydride, acrylate, tetrafluoroethylene or styrene copolymer mainly adopts the free radical polymerization method, and there are long reaction times and the acquisition of copolymerization in the synthesis process with metal complex catalysis. Disadvantages such as low yield
If a Ni / Al metal complex is used to catalyze the copolymerization of norbornene and tert-butyl methacrylate, the yield does not reach 10% after about 8 hours of polymerization

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Add 20 ml of tetrahydrofuran, 0.01 mole of zirconium chloride, 0.04 mole of 8-hydroxyquinoline and 0.10 benzyl chloride to a dry single-mouthed glass bottle that has been evacuated and baked with nitrogen, and keep the temperature in a water bath at 50°C for 30 minutes. After cooling, the zirconium complex catalyst is obtained.

Embodiment

[0028] Example Add 0.03 mole of bicyclo[2,2,1]hept-2-ene, 0.03 mole of methyl acrylate, and 0.03 mole of 1-pentene into an autoclave filled with nitrogen, and add 20ml of tetrahydrofuran to dissolve. Take 1% of the above catalyst according to the total weight of norbornene, methyl acrylate and 1-pentene, and inject it into the above mixture with a syringe. Constant temperature at 90°C, 1MP pressure, react for 3 hours. The product was poured into a methanol solution containing 5% hydrochloric acid to precipitate norbornene, methyl acrylate, and 1-pentene terpolymer. The precipitate was washed with methanol to neutrality and dried in vacuum. The reaction yield was measured to be 43.3 %.

[0029] The calculation of the reaction yield is:

[0030] Product weight / total weight of (norbornene + acrylate + pentene) monomers x 100%.

[0031] The same applies to each of the following examples.

Embodiment 2

[0033] Add 20 ml of anisole, 0.01 mol of zirconium chloride, 0.03 mol of α,α,-bipyridine and 0.08 mol of 1-bromo-1-benzene into a one-mouth glass bottle that has been evacuated several times and baked with nitrogen. Base ethane, keep the temperature in a water bath at 40°C for 30 minutes, and then get the zirconium complex catalyst after cooling.

[0034] Add 0.03 moles of bicyclo-1-methylbicyclo[2,2,1]hept-2-ene, 0.03 moles of methyl methacrylate, and 0.03 moles of 3-methyl-1-pentene into a nitrogen-filled autoclave In, add 20ml anisole to dissolve. Take 0.6% of the above-mentioned catalyst according to the total weight of norbornene, methyl methacrylate, and 3-methyl-1-pentene, and inject it into the above-mentioned mixture with a syringe. Constant temperature at 90°C, 5MP pressure, react for 6 hours. The product was poured into a methanol solution containing 5% hydrochloric acid to precipitate norbornene, methyl methacrylate, and 3-methyl-1-pentene terpolymer. The precipi...

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PUM

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Abstract

The invention relates to a catalyst for norbornene, acrylate and pentene copolymerization, and a ternary copolymerization method. The catalyst is characterized in that the preparation method of the catalyst comprises the following steps: dissolving zirconium chloride (ZrCl4), a ligand and halogenated hydrocarbon in a first solvent in a dry single-port glass bottle in the inert gas atmosphere, sealing the bottle port of the glass bottle with a latex tube, carrying out constant temperature treatment in a 40-50DEG C water bath for 10-30min, and cooling to obtain the zirconium complex catalyst. Compared with catalysts in the prior art, the catalyst provided by the invention is a novel zirconium complex catalyst, can generate a catalysis activity in a nitrogen protection system at 40-120DEG C under a certain pressure, allows products to be easily washed and separated after immersion in methanol when the catalyst is used for catalyzing the ternary copolymerization of norbornene, acrylate and pentene monomers, and has the characteristics of high copolymer yield, low reaction temperature, low price, easy obtaining, high catalysis efficiency and the like.

Description

technical field [0001] The invention relates to the field of high polymer synthesis, in particular to a catalyst and a copolymerization method for the copolymerization of norbornenes, acrylates and pentenes. 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 polynorbornene are poor brittleness, poor viscosity and low molecular weight. After inserting acrylate and pentene 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, improves its fragility in film formation, and It can reduce the absorbance of the material itself, and this copolymer can be used as a photolithography material in 157nm photolithography technology. As the development of the microelectronics industry requires sma...

Claims

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Application Information

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IPC IPC(8): C08F232/08C08F220/14C08F220/18C08F210/14C08F4/76
Inventor 房江华高浩其杨建平胡敏杰肖勋文方烨汶
Owner NINGBO UNIVERSITY OF TECHNOLOGY
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