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Microwave synthesis for producing polyketone ionic liquid

A technology for ionic liquid and microwave synthesis, which is applied in the field of microwave synthesis to achieve the effects of simple operation, environmental friendliness and improved yield

Inactive Publication Date: 2007-04-04
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In 2002, they further studied the effect of microwave power on NH 4 BF 4 with [C 4 The influence of MIM]Cl on the preparation of ionic liquids, but only a small amount of [C 4 MIM]Cl(1mmol) and NH 4 BF 4 (1.05mmol) for a tentative reaction

Method used

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  • Microwave synthesis for producing polyketone ionic liquid
  • Microwave synthesis for producing polyketone ionic liquid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] Add 0.5mol N-methylimidazole and 0.6mol n-butane bromide successively into two-necked flasks (special microwave instruments), and carry out ionization in the WF-4000 atmospheric pressure microwave rapid reaction system purchased by Shanghai Yiyao Analytical Instrument Co., Ltd. Liquid preparation. Magnetic stirring, microwave power of 300W, 80°C, 4min to end the reaction. The product was washed three to four times with ethyl acetate, and dried under vacuum at room temperature for 6 h to obtain 107.3 g of 1-n-butyl-3-methylimidazolium bromide with a yield of 98%.

[0017] Add 0.5 mol of 1-n-butyl-3-methylimidazolium bromide, 0.6 mol of sodium fluoroborate, and 150 ml of deionized water into a two-neck bottle (special microwave instrument), stir magnetically, and set the microwave power to 300W. 100°C, 10 minutes to complete the reaction, a clear and transparent light yellow liquid can be obtained. After the liquid is cooled, add the prepared lead fluoroborate aqueous s...

Embodiment 2

[0022]Add 0.5 mol N-methylimidazole and 0.6 mol bromo-n-butane into a two-neck bottle (special microwave equipment) in sequence, stir magnetically, microwave power is 200W, 80°C, 10min to end the reaction. The product was washed three to four times with ethyl acetate, and dried under vacuum at room temperature for 6 h to obtain 106.2 g of 1-n-butyl-3-methylimidazolium bromide with a yield of 97%.

[0023] Add 0.5 mol of 1-n-butyl-3-methylimidazolium bromide, 0.6 mol of sodium fluoroborate, and 150 ml of deionized water into a two-neck bottle (special microwave instrument), stir magnetically, and set the microwave power to 200W. 100°C, 15 minutes to complete the reaction, a clear and transparent light yellow liquid can be obtained. After the liquid is cooled, add the prepared lead fluoroborate aqueous solution to it dropwise until no white precipitate is formed in the solution. At 0°C, let it stand for more than 6 hours. After filtering and collecting the filtrate, the water ...

Embodiment 3

[0025] Add 0.5 mol N-methylimidazole and 0.6 mol bromo-n-butane into a two-neck flask (special microwave equipment) in sequence, stir magnetically, microwave power is 400W, 80°C, 3min to end the reaction. The product was washed three to four times with ethyl acetate, and dried under vacuum at room temperature for 6 h to obtain 105.1 g of 1-n-butyl-3-methylimidazolium bromide with a yield of 96%.

[0026] Add 0.5 mol of 1-n-butyl-3-methylimidazolium bromide, 0.6 mol of sodium fluoroborate, and 150 ml of deionized water into a two-necked bottle (special equipment for microwave), stir magnetically, and set the microwave power to 400W. 100°C, 8min to end the reaction. , a clear and transparent light yellow liquid can be obtained. After the liquid is cooled, add the prepared lead fluoroborate aqueous solution to it dropwise until no white precipitate is formed in the solution. At 0°C, let it stand for more than 6 hours. After filtering and collecting the filtrate, the water was ...

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Abstract

Micro-wave synthesis of putting N-methyl imidazole or pyridine and bromic ether, bromo-n-butane, bromo-n-hexane, bromo-n-octane or bromo-cetane into reactor, reacting at 20-150 degree and 100W-500W for 2-30mins, washing by acetic ether, drying to obtain bromo-alkyl-imidazolium or bromo-alkyl-pyridinium, microwave reacting bromo-alkyl-imidazolium or bromo-alkyl-pyridinium with tetrafluoroborate salt or toluene-p-sulfonic acid or amido-sulfonic acid in deionized water or acetone, dripping into tetrafluoroborate salt, filtering while removing water to obtain the ionic liquid, or micro-wave reacting bromo-alkyl-imidazolium or bromo-alkyl-pyridinium with hexafluorophosphate in deionized water or acetone, and filtering while removing water to obtain the final product. It's simple and efficient, has short reactive time and gentle reactive environment.

Description

technical field [0001] The invention relates to a microwave synthesis method for preparing polyketone ionic liquid, which belongs to the preparation technology of carbon monoxide and olefin copolymerization for preparing polyketone ionic liquid. Background technique [0002] The aliphatic polyketone synthesized by the copolymerization of carbon monoxide and olefin is a new type of functional polymer material. Due to its regular structure, good mechanical strength, especially its photodegradability, it has attracted widespread attention as a new type of environmentally friendly material. At present, the palladium system is often used for catalysis in the synthesis of polyketones. Due to the high cost of palladium in this system, the production of polyketones has not been able to achieve large-scale industrialization. In the existing catalytic system, whether to explore a new way to reuse the catalyst precious metal palladium (II) is one of the problems to be solved urgently ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G67/02
Inventor 郭锦棠张欣朱成才田晶许湧深
Owner TIANJIN UNIV
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