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A continuous production process and device for mixed acid nitration synthesis

A mixed acid and process technology, which is applied in the continuous production process and equipment field of mixed acid nitration synthesis, can solve the problems of multi-nitrogen and oxidation, easy combustion, explosion, small size of micro-reaction channel, etc., and achieve simple process flow, Solve the effect of large heat release and low equipment investment

Active Publication Date: 2022-05-03
TIANJIN UNIV
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  • 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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  • A continuous production process and device for mixed acid nitration synthesis

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 is 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 top of the reactor 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 production, and provides a process and device for continuous synthesis of mixed acid nitration, liquid CO 2 As a solvent mixed with the solid material in the batching tank, it enters the reactor, and the heat generated by the reaction process is produced by CO 2 The phase change takes away, the CO coming out from the top of the reactor 2 After passing through the compressor and condenser into liquid CO 2 , and return to the batching tank to continue to be used as a solvent; the reacted product is continuously extracted by the pump. Process method is also provided, the steps are as follows: liquid CO 2 As a solvent mixed with solid raw materials in the batching tank; nitric acid and H 2 S0 4 The mixture is fed into the mixed acid storage tank according to a certain ratio; the mixed reaction materials are continuously fed into the lower part of the reactor; the mixed acid is continuously fed into the upper part of the reactor to react with the raw materials; CO 2 The gas continuously enters the bottom of the reactor as the power of the reactor; the gas coming out of the top of the reactor becomes liquid CO through the compressor and condenser 2 , and return to the batching tank to continue to be used as a solvent; the reacted product is continuously extracted by the 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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Patent Type & Authority Patents(China)
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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