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Method for preparing chlorocyclohexane

A technology of chlorocyclohexane and cyclohexane, which is applied in the field of preparation of chlorocyclohexane, can solve the problems of long production cycle, low conversion rate, and low product purity, and achieve low production cost, production safety, and high product quality. The effect of high purity

Inactive Publication Date: 2005-08-31
锦化化工(集团)有限责任公司
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  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] So far, the industrial production technology of chlorocyclohexane mainly includes cyclohexanol method and cyclohexane photochlorination method. The former uses cyclohexanol and hydrochloric acid as raw materials, and zinc chloride as catalyst; the raw material cost of this method is high , Low product purity, long production cycle, and a large amount of dilute hydrochloric acid that seriously pollutes the environment
The latter uses cyclohexane and chlorine as raw materials and reacts under light; this method not only has complicated equipment and low conversion rate, but also has serious safety problems, and is very prone to explosion accidents
Recently, someone improved the photochlorination method of cyclohexane, that is, irradiated with blue light with a wavelength of 350-425nm, and added a small amount of cyclohexanone peroxide, but failed to solve the fundamental problem

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] Get 158g hexanaphthene and add in the four-necked flask that agitator, thermometer, reflux condenser and chlorine-through pipe are housed, add 0.1g composite catalyst, place the four-necked flask in a dark place, start stirring, rotating speed 100 rpm, Heat up to 60°C and feed chlorine gas at a rate of 0.05l / min for 10-20min; then cool down to 40°C and increase the rate of chlorine gas feed so that 50g of chlorine gas is fed within 4 hours. After the reaction material was neutralized with sodium carbonate and washed with water, it was first distilled under normal pressure to obtain 101.5 g of unreacted cyclohexane for the next synthesis, and then the fraction at 81-85°C was collected under a vacuum of 0.08 MPa to obtain chlorocyclohexane Hexane 68.2g. The product was analyzed by HP6890 gas chromatography, the content was 99.65%, the one-pass conversion rate of cyclohexane was 35.8%, the selectivity was 88.9%, and the yield was 85.5%.

Embodiment 2

[0015] Get 158g hexanaphthene and add in the four-necked flask that agitator, thermometer, reflux condenser and chlorine-through pipe are housed, add 0.2g composite catalyst, place the four-necked flask in a dark place, start stirring, rotating speed 100 rpm, Heat up to 70°C, feed chlorine gas at a rate of 0.05 l / min, and maintain for 10 minutes; then lower the temperature to 55°C, increase the rate of chlorine gas feed, so that 60 g of chlorine gas is fed within 4 hours. After the reaction material was neutralized with sodium carbonate and washed with water, it was first distilled under normal pressure to obtain 90.7 g of unreacted cyclohexane for the next synthesis, and then the fraction at 81-85°C was collected under a vacuum of 0.08 MPa to obtain chlorocyclohexane Hexane 80.9g. The product was analyzed by HP6890 gas chromatography, the content was 99.35%, the one-pass conversion rate of cyclohexane was 42.6%, the selectivity was 88.0%, and the yield was 85.2%.

Embodiment 3

[0017] Add 800kg of cyclohexane into the 1.5m tank with PTFE distributor and cooling coil 3 Add 5.5kg of composite catalyst to the glass-lined reactor, stir at 110 rpm, pour hot water into the jacket of the glass-lined reactor, raise the temperature to 40°C, 3 Chlorine gas is introduced at a speed of about 40-60min, and then 20-30m 3 Chlorine gas is fed in at a rate of 1 / h. After the chlorination tail gas is condensed by the reflux condenser, it is then treated by conventional methods such as spray washing and gas-liquid separation and enters the absorption tower. It is absorbed into hydrochloric acid by water. During the chlorination reaction, it passes through the jacket and cooling The mediation of the cooling water in the coil maintains the reaction temperature at 40-50°C. Pass into 168kg chlorine gas, finish reaction. After the reaction material was neutralized with sodium carbonate and washed with water, it was first distilled under normal pressure to obtain 632kg of u...

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Abstract

A process for preparing chlorocyclohexane includes such steps as intermittent liquid-phase chlorination reaction between cyclohexane, chlorine gas and composite catalyst at 30-80 deg.C, neutralizing the chlorinated liquid, water washing, distilling to recover cyclohexane, and collecting the fraction at 81-85 deg.C under 0.08 MPa to obtain chlorocyclohexane.

Description

(1) Technical field [0001] The invention relates to a preparation method of chemical products, in particular to a preparation method of chlorocyclohexane. (2) Background technology [0002] So far, the industrial production technology of chlorocyclohexane mainly includes cyclohexanol method and cyclohexane photochlorination method. The former uses cyclohexanol and hydrochloric acid as raw materials, and zinc chloride as catalyst; the raw material cost of this method is high , low product purity, long production cycle, while producing a large amount of dilute hydrochloric acid which seriously pollutes the environment. The latter uses cyclohexane and chlorine as raw materials and reacts under light; this method not only has complicated equipment and low conversion rate, but also has serious safety problems and is very prone to explosion accidents. Someone recently improved the cyclohexane photochlorination method, that is, irradiated with blue light with a wavelength of 350-4...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/093C07C23/10
Inventor 吴广铎赵厚义蒋春丽王萍张丽华
Owner 锦化化工(集团)有限责任公司
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