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Production method of diacetyl monoxime

A production method, diacetyl technology, applied in chemical instruments and methods, oxime preparation, chemical/physical/physicochemical processes, etc., can solve the problems of high toxicity of exhaust gas, excessive ethyl nitrite, complicated operation steps, etc. Achieve the effect of meeting the needs of large-scale continuous production, shortening the reaction time, and increasing the product yield

Pending Publication Date: 2020-04-10
湖州柏特生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] It can be seen that the operation steps of the traditional process are complicated and cumbersome; and the temperature is high, and the operation is relatively dangerous; the ethyl nitrite in the reaction is greatly excessive, the tail gas is highly toxic and difficult to handle, and is flammable and explosive, which will bring potential dangers

Method used

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  • Production method of diacetyl monoxime

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 7.2kg methyl ethyl ketone and 1kg catalyst were pre-mixed and preheated to 40°C, 7.65kg ethyl nitrite was preheated to 40°C respectively and pumped into the microtube reactor at the same time through the metering pump and the gas metering pump. The reaction was carried out under the pressure of 0.4MPa, and the reaction time was 45 seconds. After the reaction was completed, samples were taken for detection, and the butanone content was 1.36%, and the diacetyl monoxime content was 83.44%.

Embodiment 2

[0027] Pre-mix 7.2kg of methyl ethyl ketone and 1kg of catalyst, preheat to 40°C, and preheat 10.8kg of tert-butyl nitrite to 40°C, and pump them into the microtube reactor at the same time through metering pump and gas metering pump respectively. The reaction was carried out under a pressure of 0.4 MPa, and the reaction time was 45 seconds. After the reaction was completed, samples were taken for detection, and the butanone content was 1.64%, and the diacetyl monoxime content was 82.47%.

Embodiment 3

[0029] 7.2kg methyl ethyl ketone and 1kg catalyst were pre-mixed and preheated to 40°C, 7.65kg ethyl nitrite was preheated to 40°C respectively and pumped into the microtube reactor at the same time through the metering pump and the gas metering pump. The reaction was carried out under the pressure of 0.5 MPa, and the reaction time was 60 seconds. After the reaction was completed, samples were taken for detection, and the butanone content was 0.85%, and the diacetyl monoxime content was 85.32%.

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Abstract

The invention discloses a production method of diacetyl monoxime, and relates to a method for producing diacetyl monoxime by reacting butanone with alkyl nitrite in a microtube reactor under the catalysis of a mixed catalyst system. . The method comprises the following steps: respectively adding premixed liquid of the catalyst and the butanone and the alkyl nitrite into the microtube reactor through a metering pump, wherein the mass ratio of the catalyst to the butanone is (0.1-0.2): 1, the molar ratio of the alkyl nitrite to the butanone is (1.01-1.1): 1, and the reaction pressure in the microtube reactor is 0.1-0.5 MPa, the reaction temperature is set to be 30-50 DEG C, the reaction time is 30-60 seconds and the catalyst is a mixture of concentrated hydrochloric acid, phosphorus pentachloride and concentrated phosphoric acid. The method has the beneficial effects that the moisture in the reaction system is reduced, the excessive use of raw materials is avoided, the production cost issaved, the production efficiency is improved and the pollution of excessive reactants to the environment is reduced and the reaction safety is improved; and the equipment investment is low, the occupied area is small and mass production is facilitated.

Description

technical field [0001] The invention relates to the technical field of production of oxime compounds, in particular to a production method of diacetyl monoxime. Background technique [0002] Diacetyl monoxime is an important chemical reagent, which is often used as a detection reagent, mainly for the analysis and detection of nickel and palladium, and can also be used for the detection of trace urea; the sodium and potassium salts of diacetyl monoxime are also a high The main active ingredient in toxic chemical disinfectants. [0003] In the prior art, diacetyl monoxime is still produced according to the method (Org. Synth. 1930, 10, 22) reported by W. L. Semon and V. R. Damerell, mainly comprising the following steps: (1) in the presence of sodium nitrite and sulfuric acid , ethanol reacts with nitrous acid to generate ethyl nitrite; (2) hydrochloric acid is used as a catalyzer, butanone and ethyl nitrite react to generate diacetyl monoxime; (3) post-processing method of t...

Claims

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Application Information

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IPC IPC(8): C07C249/10C07C251/38B01J27/16B01J19/00
CPCC07C249/10B01J27/16B01J19/0093B01J27/10B01J27/14B01J35/19C07C251/38
Inventor 熊攀刘凤能许娇王云峰陈璐
Owner 湖州柏特生物科技有限公司
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