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Continuous preparation method of trinitromalonaldehydic acid dipotassium salt

A technology of dipotassium trinitropropionate and potassium nitrite, applied in the preparation of organic compounds, chemical instruments and methods, organic chemistry, etc., can solve the problem of not seeing the synthesis of dipotassium trinitropropionate By-product recovery and treatment, a large amount of waste liquid, environmental pollution and other problems, to achieve the effect of stabilizing product quality, solving pollution, and realizing recovery and recycling

Active Publication Date: 2013-10-09
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

So far, there is no bibliographical report on the preparation of this compound by the relevant continuous reaction method
In addition, a large amount of waste liquid will be produced in the process of preparing dipotassium trinitropropionaldehyde by traditional batch synthesis process, which not only pollutes the environment, but also may bring potential safety hazards
At present, there is no bibliographical report about the synthesis by-products and waste liquid recovery treatment of dipotassium trinitropropionylate

Method used

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  • Continuous preparation method of trinitromalonaldehydic acid dipotassium salt
  • Continuous preparation method of trinitromalonaldehydic acid dipotassium salt
  • Continuous preparation method of trinitromalonaldehydic acid dipotassium salt

Examples

Experimental program
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Effect test

Embodiment 1

[0031] A peristaltic pump is used as a continuous conveying equipment for liquid materials, a static mixer is used for the mixer, a translucent PTFE tube with an inner diameter of 3 mm is used for the liquid material conveying pipeline, and a vacuum filtration device is used for solid-liquid separation of materials. The pipeline is immersed in a cold water bath for heat dissipation, and an ultrasonic generator is installed on the heat dissipation pipeline.

[0032] Using 95.0% potassium nitrite by mass and 98.0% by mass mubromic acid as raw materials, first weigh 63 grams of mubromic acid and dissolve it in 320ml of 95% alcohol for use; in addition, weigh 105 grams of sub Potassium nitrate is dissolved in 380ml ethanol water-soluble solution with a volume concentration of 40% for use.

[0033] Two peristaltic pumps are used to control the flow of the raw material solution and the nitrating agent solution. The two solutions are mixed uniformly during the conveying process through th...

Embodiment 2

[0039] A mini plunger pump is used as a continuous conveying equipment for liquid materials, a static mixer is used for the mixer, a translucent polytetrafluoroethylene tube with an inner diameter of 3 mm is used for the liquid material conveying pipeline, and a vacuum filtration device is used for solid-liquid separation of materials, and liquid materials are mixed The rear pipeline is immersed in a cold water bath for heat dissipation, and two ultrasonic generators are arranged on the heat dissipation pipeline.

[0040] The same raw materials and continuous reaction process as in Example 1 were used to prepare dipotassium trinitropropionate, which only doubled the material conveying flow rate, that is, the flow rate of the mucous bromic acid solution was set to 1.2ml / min, potassium nitrite The flow rate is 1.6ml / min. After passing through the mixer, the material flows through a pipeline with an inner diameter of 3mm and a length of 30 meters. After the material is mixed, the res...

Embodiment 3

[0044] A peristaltic pump is used as a continuous conveying equipment for liquid materials, a static mixer is used for the mixer, a translucent PTFE tube with an inner diameter of 3 mm is used for the liquid material conveying pipeline, and a vacuum filtration device is used for solid-liquid separation of materials. The pipeline is immersed in a cold water bath for heat dissipation, and an ultrasonic generator is installed on the heat dissipation pipeline.

[0045] Using 95.0% potassium nitrite by mass and 98.0% muchloric acid by mass as raw materials, first weigh 200 grams of mucic acid and dissolve it in 400 grams of 95% alcohol for use. The volume is about 600ml; in addition, weigh 400g of potassium nitrite and dissolve it into 900g of ethanol water-soluble solution with a mass concentration of 45% for use. The volume of the potassium nitrite solution is about 1200ml.

[0046] Two peristaltic pumps are used to control the flow of the raw material solution and the nitrating agent...

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Abstract

The invention discloses a continuous preparation method of a trinitromalonaldehydic acid dipotassium salt. The continuous preparation method comprises the following steps of: conveying the alcoholic solution of mucobromic acid or mucochloric acid and a nitrating agent solution in parallel by using continuous conveying equipment and completing a reaction in a continuous reactor or a pipeline, performing ultrasonic dispersion treatment in the material conveying process, and carrying out the treatment processes such as solid-liquid separation, washing and drying on the generated product, thus obtaining the trinitromalonaldehydic acid dipotassium salt. Solvent distillation recovery is performed on the separated reaction mother liquor and thewashing liquid, and the distilled mother liquor is crystallized so that the by-product potassium bromide or potassium chloride can be separated out. The method is capable of improving the reaction efficiency, reducing the online handling capacity of materials and reducing or eliminating potential safety hazards probably caused by reaction heat release in the intermittent reaction process. Besides, the byproduct can be separated and utilized effectively; therefore, pollution on the environment can be avoided.

Description

Technical field [0001] The invention belongs to the synthesis technology of organic compounds, in particular to a preparation method of dipotassium trinitropropionate. Background technique [0002] In recent years, increasing the energy density of solid propellants and improving their environmental performance has become a research hotspot in the world. Dipotassium trinitropropionate is an important intermediate in the synthesis of energetic materials, which improves the synthesis efficiency of this compound. And process safety is very necessary. The traditional synthesis process is carried out by a batch process. Because a large amount of heat is released during the synthesis reaction of the compound, the material needs to be cooled to a lower temperature before the reaction. If the reaction temperature is out of control, the equipment system has a higher risk of explosion. In particular, the amount of materials being produced during industrial production is large, and the risk...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C205/44C07C201/10C01D3/10C01D3/04
Inventor 蔺向阳潘仁明李伯平杜震黄海丰杨军
Owner NANJING UNIV OF SCI & TECH
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