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Method for preparing ion liquor

A technology of ionic liquids and cations, which is applied in the field of preparation of ionic liquids, can solve the problems of inability to produce ionic liquids on a large scale, difficulty in guaranteeing product purity, high solubility of methylimidazole, etc., and achieves simple structure, saving operation steps and low price Effect

Inactive Publication Date: 2007-05-09
CHANGZHOU INST OF ENERGY STORAGE MATERIALS &DEVICES
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  • Abstract
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AI Technical Summary

Problems solved by technology

However, there are two problems in this patent: 1. Methylimidazole is unstable at 170°C and easy to decompose
2. A small amount of ethyl acetate is difficult to achieve the purpose of purification, the solubility of methylimidazole in the product is still very large, and the purity of the product is difficult to guarantee
This system also needs to control the stability by stopping the microwave irradiation, which is an intermittent reaction; and it is expensive, and cannot produce ionic liquids on a large scale
[0011] At present, the synthesis of ionic liquids uses microwave technology, mainly using microwave batch reactors, and the processing capacity is very small and the operation is cumbersome, while microwave continuous reactors can overcome the above Insufficient, but there are no reports at home and abroad on the use of microwave continuous reaction equipment to synthesize ionic liquids

Method used

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Examples

Experimental program
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Effect test

Embodiment 1

[0055] Example 1 New microwave continuous reaction equipment

[0056] A novel microwave continuous reaction equipment of the present invention, as shown in Fig. Separation device 7, product collection device 8, feed pipe 9, discharge pipe 10, side pipe 11, top pipe 12, condensate inflow pipe 13, condensate outflow pipe 14, reactor bracket 15, microwave emission source 16, Glass container 17, iron stand 18, microwave oven 19, stirrer 20, feed funnel 21, side hole 22, top hole 23, condensate outflow interface 24, condensate inflow interface 25, feed interface 26, material discharge interface 27, Rubber plug I28, pump head 29, rubber plug II30 and material prevention valve 31.

[0057] The microwave oven 19 of the present invention is Haier's new rotary wave furnace MF-2070EGZ; the microwave cavity cavity 4 of the present invention is the microwave cavity cavity of the microwave oven 19; the microwave emission source 16 is welded on the bottom of the microwave cavity cavity 4, a...

Embodiment 2

[0065] Example 2 Preparation of ionic liquid 1-hexyl-3-methylimidazolium bromide with microwave continuous reaction equipment of the present invention

[0066] Take 79ml (1mol) of 1-methylimidazole and 139ml (1mol) of 1-bromohexane and mix them, flow them into a 250ml three-necked bottle through the feeding funnel, stir evenly, and flow into the reactor through the feeding pipe under the drive of the constant flow pump Medium (microwave power is 280W). Adjust the flow rate of the magnetic stirrer to make it stir evenly, adjust the flow rate of the constant flow pump (adjust the value of the constant flow pump to 1.0, and the flow rate is 1.86ml.s -1 ), the flow time of the reaction materials in the reactor is 2.5 minutes, and water is passed into the cooling device for heat exchange to achieve a controlled reaction temperature of 60-65°C. Driven by the constant flow pump, the reactant material flows into the separatory funnel from the reactor through the discharge pipe, and a...

Embodiment 3

[0073] Example 3 Preparation of ionic liquid ionic liquid 1-octyl-3-methylimidazolium chloride salt with microwave continuous reaction equipment of the present invention

[0074] Take 79ml (1mol) of 1-methylimidazole and 170ml (1mol) of 1-chlorooctane and mix them, flow them into a 250ml three-neck bottle through the feeding funnel, stir evenly, and flow into the reactor through the feeding pipe under the drive of the constant flow pump Medium (microwave power is 420W). Adjust the flow rate of the magnetic stirrer to make it stir evenly, adjust the flow rate of the constant flow pump (adjust the value of the constant flow pump to 0.5, and the flow rate is 0.67ml.s -1 ), the flow time of the reaction materials in the reactor is 3 minutes, and water is passed into the cooling device for heat exchange to achieve a controlled reaction temperature of 65-70°C. Driven by the constant flow pump, the reactant material flows into the separatory funnel from the reactor through the disch...

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Abstract

This invention relates to a method for preparing ionic liquid. The continuous microwave reaction equipment used is designed, modified and assembled on the basis of domestic microwave oven. The general chemical formula of the ionic liquid is A+B-, where A+ is organic cation, and B- is inorganic anion. The melting point of the ionic liquid is lower than 100 deg.C under an atmosphere (101.325 kPa). The method can increase the reaction rate by 10-1000 times, thus can shorten the time of ionic liquid synthesis from a week to within an hour. Besides, the process is continuous.

Description

technical field [0001] The invention relates to a method for preparing an ionic liquid, in particular to a method for preparing an ionic liquid using microwave continuous reaction equipment. technical background [0002] Chemical reactions often require heating or high temperature and high pressure. Most of the previous heating methods use heat conduction and heat convection. These heating methods conduct heat from the outside to the inside of the reactor, and the heating speed is slow, and the external temperature of the reaction system is higher than the internal temperature. The temperature and uneven heating lead to unsatisfactory reaction yield and selectivity, and it is difficult to meet the requirements of certain chemical reactions. Microwaves can directly irradiate each molecule in the reaction mixture, including solvents, reaction materials and catalysts, and the reaction vessel is made of materials such as borosilicate, quartz, and polytetrafluoroethylene that do ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D233/08
CPCY02P20/582
Inventor 陈继胡旭刘郁
Owner CHANGZHOU INST OF ENERGY STORAGE MATERIALS &DEVICES
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