Norbornene, styrene and maleic anhydride ternary polymerization catalyst and ternary polymerization method

An acid anhydride ternary copolymerization catalyst and norbornene technology, applied in the field of high polymer synthesis catalyst and high polymer synthesis, can solve the problems of low copolymer molecular weight, low copolymer alternation degree, low copolymer yield, etc., and achieve The effect of low reaction temperature, easy washing and separation, and high copolymer yield

Active Publication Date: 2016-01-06
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

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Dissolve 0.001 mole of rhodium trichloride, 0.001 mole of diethyl zinc and 0.001 mole of 8-hydroxyquinoline in 10 ml of benzene, put it into a single-neck glass bottle that has been evacuated for many times, filled with nitrogen, and baked and dried. Seal with a latex tube, put it into a constant temperature water tank at 40° C. for 15 minutes, and obtain a rhodium-zinc complex catalyst.

[0025] Add 0.01 moles of bicyclo[2,2,1]hept-2-ene, 0.01 moles of styrene and 0.01 moles of maleic anhydride into a single-neck glass bottle that has been evacuated many times, filled with nitrogen and baked and dried. The bottle mouth is made of latex. The tube is sealed and dissolved by adding 20 ml of benzene with a syringe. The amount of rhodium trichloride in the catalyst is 0.02% of the total weight of norbornene, styrene and maleic anhydride. The above rhodium-zinc complex catalyst is taken and injected into the above mixture with a syringe. The constant temperature was 40°C, a...

Embodiment 2

[0028] Dissolve 0.001 moles of rhodium trichloride, 0.020 moles of diethylzinc and 0.002 moles of α,α'-bipyridine in 10 ml of toluene, put them in a single-neck glass bottle that has been evacuated for many times, filled with nitrogen and baked and dried, The bottle mouth was sealed with a latex tube, and put into a constant temperature water tank at 50° C. for 30 minutes to obtain a rhodium-zinc complex catalyst.

[0029] Add 0.01 mol of 1-methylbicyclo[2,2,1]hept-2-ene, 0.01 mol of styrene and 0.01 mol of maleic anhydride into a single-neck glass bottle that was evacuated many times, filled with nitrogen and baked and dried, The bottle mouth is sealed with a latex tube, and 20ml of toluene is added to dissolve it with a syringe. The amount of rhodium trichloride in the catalyst is calculated as 0.1% of the total weight of norbornene, styrene and maleic anhydride. The above rhodium-zinc complex catalyst is taken and injected into the above mixture with a syringe. The constan...

Embodiment 3

[0031] Dissolve 0.001 mol of rhodium trichloride, 0.010 mol of diethyl zinc and 0.010 mol of phenanthroline in 10 ml of tetrahydrofuran, put it into a single-neck glass bottle that has been evacuated for many times, filled with nitrogen, and baked and dried. The latex tube was sealed, put into a constant temperature water tank at 50° C. for 25 minutes, and the rhodium-zinc complex catalyst was obtained.

[0032] Add 0.01 moles of 5-methylbicyclo[2,2,1]hept-2-ene, 0.01 moles of styrene and 0.01 moles of maleic anhydride into a single-neck glass bottle that was vacuumed many times, filled with nitrogen and baked and dried, The bottle mouth is sealed with a latex tube, and 20ml of tetrahydrofuran is added to dissolve it with a syringe. The amount of rhodium trichloride in the catalyst is calculated as 0.8% of the total weight of norbornene, styrene and maleic anhydride. The above rhodium-zinc complex catalyst is taken and injected into the above mixture with a syringe. The const...

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PUM

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Abstract

The invention relates to a norbornene, styrene and maleic anhydride ternary polymerization catalyst and a ternary polymerization method. The norbornene, styrene and maleic anhydride ternary polymerization catalyst is characterized in that a preparation method of the catalyst comprises the steps of dissolving rhodium chloride, iethylzinc and a ligand compound into a first solvent in a single-neck glass bottle with a dry inert atmosphere, sealing the bottleneck, and keeping the constant temperature of 40-50 DEG C for 15-30 minutes to obtain a rhodium-zinc complex catalyst. The ternary polymerization method comprises the steps of adding norbornene monomers, styrenes and maleic anhydride monomers into the multiply vacuumized and dried single-neck glass bottle with the dry inert atmosphere according to the molar ratio of 1:1:1, and then, adding a second solvent to dissolve; and then, adding the rhodium-zinc complex catalyst, and reacting at the temperature of 20-90 DEG C for 1-8 hours. The catalyst provided by the invention is cheap and available in raw materials, capable of generating catalytic activity at a relatively low temperature, low in polymerization reaction temperature and high in catalytic efficiency; and in addition, the catalyst is easily washed and separated, and the yield of copolymers is high.

Description

technical field [0001] The invention relates to a high polymer synthesis catalyst and high polymer synthesis, in particular to a ternary copolymerization catalyst of norbornene, styrene and maleic anhydride 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, which can be used for 193nm UV lithography. The main disadvantages of this material are brittleness, poor viscosity and low molecular weight. Moreover, the development of the microelectronics industry requires components with smaller sizes. For the exposure technology suitable for the line width of 1.3 μm and below, the 193nm lithography technology can be selected. These technologies involve all aspects of the lithography process and propose new of optical materials and their manufacturing and coating technologies, new resists, new materials for masks and their prot...

Claims

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Application Information

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IPC IPC(8): C08F4/70C08F232/08C08F212/08C08F222/06
Inventor 房江华胡敏杰高浩其
Owner NINGBO UNIVERSITY OF TECHNOLOGY
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