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Method and equipment for preparing diazomethane

A diazomethane and equipment technology, applied in the field of diazomethane preparation, can solve the problems of low raw material cost, short process route, high yield, etc., and achieve the effects of reduced production cost, high yield, and avoiding safety risks

Inactive Publication Date: 2016-03-23
YIBIN JIULING CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The object of the present invention is to provide a kind of preparation method of diazomethane and the equipment that implements this preparation method, to solve the defect of existing preparation method, realize having short process route, low raw material cost and high yield, and preparation process is safe, Environmental protection, can realize the effect of industrial continuous production

Method used

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  • Method and equipment for preparing diazomethane

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] The preparation method of diazomethane comprises the following steps:

[0035] Under completely sealed conditions, take the raw material N-nitroso-methylurea liquid, the molar mass fraction is 2.32 mol / liter, with the speed of 822 liters per hour (its flow rate is: V (A) * C=822 / 1000m3 / h×2.32kg / m3=1.907kg mol / h) and 25.1% NaOH are simultaneously injected into the static mixer at the feed end at a rate of 238 liters per hour, and the reaction temperature is controlled at -5°C, 30~ After 90 seconds, the reaction is complete, and the diazomethane generated is injected into the extractant ether, and the flow rate of the ether (m 3 / h) is 0.5 times the flow rate (kgmol / h) of the raw material compound N-nitroso-methylurea, and the flow rate is 954 liters per hour (extractant flow rate: 0.5×1.907=0.954 cubic meters / hour). Extract for 15 minutes, separate the water phase, the oil phase is diazomethane solution, the production rate of diazomethane solution is 946 liters / hour, ...

Embodiment 2

[0041] Under completely sealed conditions, the raw material 1-methyl-3-nitro-1-nitrosoguanidine solution, its molar mass fraction is 1.7 mol / liter, with the KOH of 791 liters of speed and mass fraction 25.0% per hour At a speed of 269 liters per hour, it enters the static mixer at the feed end synchronously, and the reaction temperature is controlled at -5°C. After 30 to 90 seconds, the reaction is complete, and the generated diazomethane is injected into the extraction agent tetrahydrofuran. The flow rate of tetrahydrofuran (m 3 / h) is 3.0 times the liquid flow rate (kgmol / h) of the raw material compound 1-methyl-3-nitro-1-nitrosoguanidine, the continuous feeding rate of THF is 4034 liters / hour, and the extraction is carried out for 30 minutes, The aqueous phase and the diazomethane solution were separated, and the diazomethane solution was obtained at a rate of 4045 liters / hour, with a content of 11.19 g / liter and a diazomethane production capacity of 45.26 kg / hour.

[0042]...

Embodiment 3

[0044] Under completely sealed conditions, the raw material N-methyl-N-nitroso-p-toluenesulfonamide solution has a molar mass fraction of 1.2 mol / liter, at a speed of 887 liters per hour and with a mass fraction of 25.1% NaOH At a rate of 173 liters per hour, it enters the static mixer at the feed end synchronously, and the reaction temperature is controlled at -10°C. After 30 to 90 seconds, the reaction is complete. The generated diazomethane is extracted with methyl tert-butyl ether, and methyl tert-butyl The flow rate of base ether (m 3 / h) is 0.8 times of the flow rate (kgmol / h) of the raw material compound N-methyl-N-nitroso-p-toluenesulfonamide solution, the injection flow rate is 852 liters / hour, the extraction is for 15 minutes, and the aqueous phase and the Diazomethane solution, namely 847 liters / hour of diazomethane solution, content of 40.2 g / liter, diazomethane production capacity of 34.0 kg / hour.

[0045] Conclusion: The yield of diazomethane is up to 76%, and e...

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Abstract

The invention relates to a method and equipment for preparing diazomethane, and belongs to the field of organic synthesis. The method and the equipment have the advantages that the method and the equipment aim to overcome shortcomings of existing methods for preparing diazomethane and are short in process route, low in raw material cost and high in yield, preparation procedures are safe and environmental friendly, and effects of industrial continuous production can be realized; the method for preparing the diazomethane is implemented by the aid of the equipment, the diazomethane can be generated from a N-methyl-N-nitroso material and alkali metal hydroxide by means of completely closed reaction, stable organic solution can be formed by means of timely extraction by the aid of extraction agents, accordingly, the retention time of the diazomethane in water can be shortened, the decomposition rate of the diazomethane which can generate methyl alcohol and nitrogen when in water can be reduced, the diazomethane yield can be increased, and safety risks of operator poisoning and explosion due to leakage of gaseous diazomethane can be prevented.

Description

technical field [0001] The invention belongs to the field of organic synthesis, in particular to a method for preparing diazomethane and equipment thereof. Background technique [0002] Diazomethane is a very important organic intermediate and synthetic factor in fine organic synthesis. It is mainly used in the production of medicines and pesticides, such as the production of L-phenylalanine chloromethyl ketone. Diazomethane is volatile and highly toxic , Inflammable, explosive and highly dangerous substances. It is a yellow gas with strong irritation and musty smell at normal temperature and pressure. The gas is heavier than air and can flow along the ground, which may cause fire at a distance. When reacting, a strong explosion can occur, and the concentrated solution is also prone to explosion in the presence of impurities. When the undiluted liquid or gas contacts alkali metal and calcium sulfate, rough object surface, strong impact or heating to 100 ℃ , or under high-in...

Claims

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Application Information

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IPC IPC(8): C07C245/16
CPCC07C245/16
Inventor 张国良方善伦袁晓波贾云峰高福元何红
Owner YIBIN JIULING CHEM
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