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Complexation-system ionic liquid catalyst-HF solution, preparation method and application thereof

A catalyst and ionic liquid technology, which is applied in the field of complex system ionic liquid catalyst-HF solution, can solve the problems of low yield of reaction products, complicated process, etc., and achieves convenient and easy-to-control process operation, good catalytic activity, and mild reaction conditions. Effect

Inactive Publication Date: 2010-05-12
UNIV OF JINAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Patent FR0101245 involves the issue of fluorinating chlorinated hydrocarbons with ionic liquid catalysts, but it only fluorinates chlorinated hydrocarbons with one or two carbon atoms, and the yield of reaction products is low, the process is complicated, and the reaction equipment requires special materials

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Add 1 mol of N-methylimidazole and 1.2 mol of n-octane chloride to a three-neck flask equipped with a stirrer, reflux condenser, thermometer and nitrogen conduit, and add 1 g of Li 2 CO 3 and Al(OH) 3 (The mass ratio is 20:0.6) The compound is catalyst, nitrogen protection, microwave radiation heating, power is 200W, 40 ℃ stirring reaction 5h, the viscous liquid obtained is repeatedly washed with a small amount of ethyl acetate, and heated at 70 ℃ After vacuum drying to remove the residual ethyl acetate, the yield was 98% white solid product chloride 1-n-octyl-3-methylimidazole. Under the protection of nitrogen, the obtained chlorinated 1-n- Octyl-3-methylimidazole and 1.1 mol SbF 5 Mix well in a closed stainless steel reaction kettle, and stir at -20°C for 12 hours to obtain 1-n-octyl-3-methylimidazole chloride / SbF 5 The ionic liquid catalyst is sealed and stored for future use.

[0024] Add 1mol of 1-n-octyl-3-methylimidazole chloride / SbF to a fluoroplastic reacti...

Embodiment 2

[0026] Add 1 mol of N-methylimidazole and 1.1 mol of n-chlorobutane into a three-neck flask equipped with a stirrer, reflux condenser, thermometer and nitrogen conduit, and add 1 g of Li 2 CO 3 and Al(OH) 3 (The mass ratio is 20:0.6) The compound is used as a catalyst, protected by nitrogen gas, heated by microwave radiation, the power is 300W, stirred and reacted at 60°C for 4h, the obtained viscous liquid is washed repeatedly with a small amount of ethyl acetate, and heated at 70°C After drying under vacuum to remove residual ethyl acetate, the white solid product 1-n-butyl-3-methylimidazolium chloride [bmim]Cl was obtained. Under the protection of nitrogen, the obtained [bmim]Cl and 1.1mol SbCl 5 Mix well in a stainless steel reactor and stir at 10°C for 6 hours to obtain [bmim]Cl / SbCl 5 The ionic liquid catalyst is sealed and stored for future use.

[0027] Add 1mol [bmim]Cl / SbCl to a fluoroplastic reaction bottle equipped with a stirrer and a condenser 5 For the ioni...

Embodiment 3～8

[0029] Other examples of the complex ionic liquid catalyst-HF solution of the present invention obtained in the same manner as in Example 2 are summarized in the following table.

[0030] implement

[0031] * is an equimolar mixture of the two.

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Abstract

The invention discloses a complexation-system ionic liquid catalyst-HF solution, a preparation method and application thereof. The solution comprises an ionic liquid catalyst and anhydrous fluorinated hydrocarbon which are in a molar ratio of 1:5-50. The invention also discloses the application of the complexation-system solution in the fluorination of hydrochloric ether. The method comprises: adding hydrochloric ether and the complexation-system ionic liquid catalyst-HF solution to a high-pressure reactor; raise temperature to between 30 and 100 DEG C within one hour; performing reaction for 3 to 20 hours under the pressure between 1 and 2 MPa; and obtaining fluorine chlorine alkane by separating and purifying products after the reaction is over. The method has the advantages of mild conditions, low system pressure, easy separation and purification of fluorination products, easy control over convenient process operation and suitability for industrial production. Through appropriate treatment, the complexation-system solution can be regenerated and repeatedly used but still has good catalytic activity.

Description

technical field [0001] The invention relates to a complex system ionic liquid catalyst-HF solution and a preparation method and application thereof. Background technique [0002] Perchlorofluorocarbons (CFCs for short) have excellent physical and chemical properties and are widely used in refrigeration, air conditioning, foaming, cleaning, fire protection, aerosol and other industries, and occupy an important position in the national economy. Since this type of compound is the main chemical substance that destroys the atmospheric ozone layer and produces the greenhouse effect, it has become the object to be phased out and eventually banned. Since the 1980s, the development of alternatives to CFCs has been one of the most active research topics in the field of organic fluorine chemistry and catalysis. [0003] Hydrochlorofluorocarbons and hydrofluorocarbons have similar physical and chemical properties to CFCs, and their ozone depletion potential (ODP) and room temperature e...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/38B01J31/30B01J31/26C07C19/10C07C17/35C07C17/087
Inventor 张书香李辉施强耿兵张炉青
Owner UNIV OF JINAN
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