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Norbornene and 2,5-dihydro-2,5-dimethoxy furan binary polymerization catalyst and binary polymerization method

A dimethoxyfuran binary copolymerization catalyst and dimethoxyfuran technology are applied in the field of high polymers and can solve the problems of insufficient rigidity of the copolymer ring, small molecular weight of the copolymer, influence on the heat resistance of the copolymer, etc. Effects of shortened polymerization time, improved polymerization efficiency, and improved heat resistance

Pending Publication Date: 2017-12-15
NINGBO UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, this polymer is a copolymer of norbornene and open-chain olefin, the ring rigidity of the copolymer is not enough, and the heat resistance of the copolymer is not as good as the copolymerization of cyclic olefin. At the same time, in the ZL 200810063783. In the preparation method of maleic anhydride copolymer, because maleic anhydride is a strong electron-withdrawing monomer, the molecular weight of copolymer is less, generally at 10 3 order of magnitude, also affects the heat resistance of the copolymer

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] In a three-necked flask with a dry inert gas atmosphere, dissolve 0.001 mole of cobalt dichloride and 0.001 mole of 8-hydroxyquinoline in 10 milliliters of benzene to obtain a mixed solution; The base lithium was dropped into the mixed solution, and after the dropping was completed, it was stirred at a constant temperature of 30°C for 60 minutes, 7.5ml of solvent was evaporated, and the mixture was left to stand for 3 hours to obtain solid crystals, which were filtered to obtain a cobalt-lithium complex catalyst.

[0024] Add 0.01 mole of bicyclo[2,2,1]hept-2-ene and 0.01 mole of 2,5-dihydro-2,5-dimethoxyfuran into an autoclave that has been evacuated several times and filled with nitrogen. 20ml of benzene was dissolved. Get the above-mentioned cobalt-lithium complex catalyst by 0.01% of the total weight of bicyclo[2,2,1]hept-2-ene and 2,5-dihydro-2,5-dimethoxyfuran, add in the above mixture. React at a constant temperature of 90°C and a pressure of 1 MPa for 5 hours....

Embodiment 2

[0030] In a three-necked flask with a dry inert gas atmosphere, dissolve 0.001 mol of cobalt dichloride and 0.016 mol of α, α'-bipyridyl in 10 ml of toluene to obtain a mixed solution; install an electric stirrer to stir, and mix 0.010 mol of One mole of butyllithium was dropped into the mixed solution, and after the dropping was completed, it was stirred at a constant temperature of 60°C for 30 minutes, 5ml of solvent was evaporated, and the mixture was allowed to stand for 8 hours to obtain solid crystals, which were filtered to obtain a cobalt-lithium complex catalyst.

[0031] Add 0.01 mole of bicyclo[2,2,1]hept-2-ene and 0.01 mole of 2,5-dihydro-2,5-dimethoxyfuran into an autoclave that has been evacuated several times and filled with nitrogen. 20ml of toluene was dissolved. Get the above-mentioned cobalt-lithium complex catalyst by 0.05% of the total weight of bicyclo[2,2,1]hept-2-ene and 2,5-dihydro-2,5-dimethoxyfuran, add in the above mixture. React at a constant tem...

Embodiment 3

[0034] In a three-necked flask with a dry inert gas atmosphere, dissolve 0.001 mol of cobalt dichloride and 0.010 mol of o-phenanthroline in 10 ml of tetrahydrofuran to obtain a mixed solution; Lithium was added dropwise into the mixed solution, and after the drop was completed, it was stirred at a constant temperature of 30°C for 60 minutes, 6ml of solvent was evaporated, and the mixture was allowed to stand for 7 hours to obtain solid crystals, which were filtered to obtain a cobalt-lithium complex catalyst.

[0035]Add 0.01 mole of 1-methylbicyclo[2,2,1]hept-2-ene and 0.01 mole of 2,5-dihydro-2,5-dimethoxyfuran to the Kettle, add 20ml tetrahydrofuran to dissolve. According to 0.08% of the total weight of 1-methylbicyclo[2,2,1]hept-2-ene and 2,5-dihydro-2,5-dimethoxyfuran, the above-mentioned cobalt-lithium complex material catalyst, added to the above mixture. React at a constant temperature of 120° C. and a pressure of 7 MPa for 5 hours. The product was poured into an e...

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Abstract

The invention relates to a norbornene and 2,5-dihydro-2,5-dimethoxy furan binary polymerization catalyst and a binary polymerization method. A preparation method of the catalyst comprises the following steps: in a dry inert gas atmosphere container, dissolving cobalt dichloride and ligand into a first solvent so as to obtain a mixed solution; dropping butyl lithium into the mixed solution at a rotation speed of 200-600rpm, continuously stirring for 30-60 minutes at 30-60 DEG C, steaming off the first solvent which accounts for 1 / 2-3 / 4 of the volume, leaving to stand for 3-8 hours so as to obtain a solid crystal, and filtering so as to obtain a cobalt-lithium complex catalyst; putting a norbornene monomer and a 2,5-dihydro-2,5-dimethoxy furan monomer into a high-pressure kettle which is vacuumed and introduced with nitrogen for multiple times, and dissolving the components with a second solvent; performing a reaction on the cobalt-lithium complex catalyst for 1-6 hours at 20-150 DEG C at the pressure of 1-8MPa; and washing a product obtained from the reaction, thereby obtaining a biopolymer.

Description

technical field [0001] The invention relates to the field of high polymers, in particular to a norbornene and 2,5-dihydro-2,5-dimethoxyfuran binary copolymerization catalyst and a binary copolymerization method. Background technique [0002] CN201611177622.7 discloses a "norbornene and perfluoromethyl vinyl ether binary copolymerization catalyst and binary copolymerization method", the preparation method of the catalyst used is as follows: in a dry inert gas atmosphere container Dissolve antimony pentachloride and ligands in the first solvent, then add tetraisopropoxytitanium dropwise at 200-300rpm, and continue stirring at 30-50°C for 30-50 minutes after dropping, that is Obtain an antimony-titanium complex catalyst; take norbornene monomers and perfluoromethyl vinyl ether monomers in a molar ratio of 1:1 and add them to multiple vacuum-pumped, nitrogen-filled autoclaves, and add a second solvent to dissolve Then add the antimony-titanium complex catalyst and react at 30-1...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F232/08C08F234/02C08F4/70
CPCC08F232/08C08F4/70C08F4/7096C08F234/02
Inventor 徐卫红周国权王江波胡敏杰高浩其房江华杨建平王志强
Owner NINGBO UNIVERSITY OF TECHNOLOGY
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