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Mixed acid nitration synthesis continuous production process and device

A mixed acid, continuous technology, applied in the direction of ammonia compounds, feeding devices, chemical/physical/physicochemical processes, etc., can solve the problems of polynitrates and oxidation, prone to combustion, explosion, small size of micro-reaction channels, etc. Achieve the effects of simple process flow, large heat release and low equipment investment

Active Publication Date: 2021-03-19
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The development process of the traditional tank-type batch or tank-type series nitration process is often based on small-scale reactions in the laboratory, and large-scale production is realized by expanding the capacity. The enlargement of the reaction vessel leads to changes in the specific surface area, and the heat transfer efficiency and mass transfer effect have certain effects. Limitations, and then cause regional over-nitration or hot spots, heat accumulation, easy to generate side reactions such as polynitrogen and oxidation, and easy to burn and explode
In recent years, although microchannel reactors have been used in nitrification reactions, due to the small size of the microreaction channels, usually between a few microns and several hundred microns, the reactants are slightly viscous or the particles are large, which will block the channels, especially It cannot be applied at all when the raw material is solid or the product is solid

Method used

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  • Mixed acid nitration synthesis continuous production process and device

Examples

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Effect test

Embodiment 1

[0022] O-methyl-N-nitroisourea 30kg and 100kg of CO 2 The liquid is mixed in the mixing tank, the temperature of the mixing tank is 15°C, and the pressure is 5.2MPa; the mixed material enters the reactor continuously at a flow rate of 13kg / h, the temperature in the reactor is 15°C, and the pressure is 5.0MPa Mixed acid is added in the mixed acid storage tank by HNO3:H2SO4=3:1 (mol), and mixed acid enters into the reactor continuously with the flow rate of 9.6kg / h and reacts with ammonium sulfamate to generate ammonium dinitramide. CO 2 The gas continuously enters the bottom of the reactor at a flow rate of 8Nm3 / h as the power of the reactor. The generated ammonium dinitramide and unreacted mixed acid are continuously extracted from the upper part of the reactor with a flow rate of 12.6kg / h by the product discharge pump; the unreacted CO 2 The discharge from the top of the reactor is compressed and condensed into CO by the compressor and condenser 2 The liquid is returned to...

Embodiment 2

[0024] Ammonium sulfamate 9.7kg and 44kg of CO 2 The liquid is mixed in the mixing tank, the temperature of the mixing tank is -40°C, and the pressure is 1.2MPa; the mixed material enters the reactor continuously at a flow rate of 5.37kg / h, the temperature in the reactor is -40°C, and the pressure 1.0MPa; mixed acid according to HNO 3 :H 2 SO 4 =5:1 (mol) is added in the mixed acid storage tank, and the mixed acid continuously enters the reactor with a flow rate of 5kg / h to react with ammonium sulfamate to generate ammonium dinitramide. CO 2 The gas continuously enters the bottom of the reactor at a flow rate of 5Nm3 / h as the power of the reactor. The ammonium dinitramide and unreacted mixed acid are continuously extracted from the reactor top with a flow rate of 6kg / h by the product discharge pump; 2 The discharge from the top of the reactor is compressed and condensed into CO by the compressor and condenser 2 The liquid is returned to the ingredients tank.

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Abstract

The invention belongs to the field of fine chemical industry production, and provides a mixed acid nitration synthesis continuous process and device. Liquid CO2 is used as a solvent to be mixed with asolid material in a batching tank; an obtained mixture enters a reactor; heat generated in the reaction process is taken away by phase change of CO2, and therefore, the CO2 coming out of the top of the reactor is changed into liquid CO2 through a compressor and a condenser, and returns to the batching tank to be continuously used as a solvent; and a product obtained after a reaction is continuously extracted by a pump. The invention further provides a technological method. The technological method comprises the following steps that: liquid CO2 serves as a solvent to be mixed with a solid rawmaterial in a batching tank; feeding a mixture of nitric acid and H2S04 into a mixed acid storage tank according to a certain ratio; the mixed reaction material is continuously fed into the lower partof a reactor; mixed acid is continuously fed into the upper part of the reactor to react with the raw material; CO2 gas continuously enters the bottom of the reactor to be used as power of the reactor; gas discharged from the top of the reactor is changed into liquid CO2 through a compressor and a condenser, and the liquid CO2 returns to the batching tank to be continuously used as a solvent; anda product obtained after the reaction is continuously extracted by a pump.

Description

technical field [0001] The invention belongs to the field of fine chemical production, and in particular relates to a continuous production process and device for mixed acid nitration synthesis. Background technique [0002] Nitrification reaction is an important chemical reaction, which is widely used in the production process of organic raw materials and intermediates, and its nitration products are used in the industrial production process of various products such as dyes, pesticides, medicines and explosives. At present, nitric-sulfur mixed acid composed of sulfuric acid and nitric acid is widely used as a nitrating agent in industry. The nitrification reaction process has the characteristics of large heat release and extremely fast reaction speed. The development process of the traditional tank-type batch or tank-type series nitration process is often based on small-scale reactions in the laboratory, and large-scale production is realized by expanding the capacity. The...

Claims

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Application Information

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IPC IPC(8): C01C1/00B01J4/00B01J19/00
CPCC01C1/00B01J4/007B01J4/008B01J19/00
Inventor 刘辉郭凯刘春江项文雨谢省宾成洁魏东旭韦昌鹏付娜胡清
Owner TIANJIN UNIV
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