Norbornene-cyclohexene-vinylene carbonate ternary copolymerization catalyst and ternary copolymerization method

A vinylene carbonate ternary copolymerization catalyst and vinylene carbonate 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 low reaction temperature , Solubility and toughness improvement, the effect of high copolymer yield

Active Publication Date: 2017-06-13
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 copolymers, small molecular weight of copolymers, and low degree of alternation of copolymers.

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 gas atmosphere, 0.001 moles of tris(cyclopentadienyl)gadolinium(III) and 0.006 moles of 8-hydroxyquinoline were dissolved in 10 ml of benzene, and 0.010 moles of tetraiso Titanium propoxide was dropped into the above solution, and after the drop was completed, the mixture was stirred at a constant temperature of 60° C. for 40 minutes at the same stirring rate to obtain a gadolinium-titanium complex catalyst.

[0025] Add 0.01 mole of bicyclo[2,2,1]hept-2-ene, 0.01 mole of cyclohexene and 0.01 mole of vinylene carbonate into an autoclave evacuated several times and filled with nitrogen, and add 20ml of benzene to dissolve. According to the amount of tri(cyclopentadienyl) gadolinium (Ⅲ) in the catalyst, it is taken as 0.06% of the total weight of bicyclo[2,2,1]hept-2-ene, cyclohexene and vinylene carbonate The above-mentioned gadolinium-titanium complex catalyst is injected into the above-mentioned mixture with a syringe. React at...

Embodiment 2

[0028] In a three-necked flask with a dry inert gas atmosphere, 0.001 moles of tris(cyclopentadienyl)gadolinium (III) and 0.007 moles of α, α'-bipyridine were dissolved in 10 ml of toluene, and 0.016 moles of Tetraisopropoxytitanium was dropped into the above solution, and then stirred at the same stirring rate at 30° C. for 50 minutes at a constant temperature to obtain a gadolinium-titanium complex catalyst.

[0029] Add 0.01 mole of bicyclo[2,2,1]hept-2-ene, 0.01 mole of cyclohexene and 0.01 mole of vinylene carbonate into an autoclave evacuated several times and filled with nitrogen, and add 20ml of toluene to dissolve. According to the amount of tri(cyclopentadienyl) gadolinium (III) in the catalyst, it is taken as 0.01% of the total weight of bicyclo[2,2,1]hept-2-ene, cyclohexene and vinylene carbonate The above-mentioned gadolinium-titanium complex catalyst is injected into the above-mentioned mixture with a syringe. React at a constant temperature of 100°C and a press...

Embodiment 3

[0031] In a three-necked flask with a dry inert gas atmosphere, 0.001 moles of tris(cyclopentadienyl)gadolinium (III) and 0.010 moles of phenanthroline were dissolved in 10 milliliters of tetrahydrofuran, and at 450 rpm, 0.008 moles of tetraisopropyl Titanium oxide was added dropwise into the above solution, and after the drop was completed, it was stirred at the same temperature at 60° C. for 50 minutes at a constant temperature to obtain a gadolinium-titanium complex catalyst.

[0032] Add 0.01 mole of 1-methylbicyclo[2,2,1]hept-2-ene, 0.01 mole of cyclohexene and 0.01 mole of vinylene carbonate to several vacuum-evacuated and nitrogen-filled autoclaves, add 20ml of tetrahydrofuran dissolve. The total weight of 1-methylbicyclo[2,2,1]hept-2-ene, cyclohexene and vinylene carbonate is calculated according to the amount of tri(cyclopentadienyl)gadolinium(III) in the catalyst 0.10% of the above-mentioned gadolinium-titanium complex catalyst was injected into the above-mentioned ...

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PUM

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Abstract

The present invention relates to a norbornene-cyclohexene-vinylene carbonate ternary copolymerization catalyst. The preparation method comprises: in a three-necked flask in a dry inert gas atmosphere, dissolving tris(cyclopentadiene)gadolinium (III) and a ligand in a first solvent, adding titanium tetraisopropanolate in a dropwise manner under 300-500 rpm, and carrying out constant temperature stirring for 30-60 min at a temperature of 30-60 DEG C at the same stirring rate after adding the titanium tetraisopropanolate to obtain a gadolinium-titanium complex catalyst; taking a norbornene monomer, a cyclohexene monomer and a vinylene carbonate monomer according to a molar ratio of 1:1:1, adding to a reaction kettle being subjected to multiple vacuumizing and nitrogen filling, adding a second solvent, and dissolving; adding the gadolinium-titanium complex catalyst, and carrying out a reaction for 1-6 h at a temperature of 30-100 DEG C under a pressure of 0.1-6 MPa; and pouring the product obtained through the reaction into a hydrochloric acid-containing ethanol solution, washing the obtained precipitate by using ethanol to achieve a neutral state, and carrying out vacuum drying to obtain the norbornene-cyclohexene-vinylene carbonate ternary copolymer.

Description

technical field [0001] The invention relates to the field of high polymers, in particular to a ternary copolymerization catalyst of norbornene, cyclohexene and vinylene carbonate 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. After the oxygen-containing compound is inserted into the main chain of polynorbornene, the cohesiveness and solubility of the polymer can be improved, and the light absorption rate of the material itself can be reduced. This copolymer can be used as a photoresist material in 193nm photolithography. Moreover, the development of the microelectronics industry requires components with smaller sizes. For the exposure technology suitable for line widt...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F232/08C08F232/04C08F218/00C08F4/6592C08F4/643C08F4/649
CPCC08F4/643C08F4/6495C08F4/65922C08F218/00C08F218/24C08F232/04C08F232/08
Inventor 胡敏杰王江波高浩其房江华杨建平王志强陈斌
Owner NINGBO UNIVERSITY OF TECHNOLOGY
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