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Method and device for recycling ethanol in production of hexanitrostilbene

A technology of hexanitrobibenzyl and ethanol, which is applied in the field of ethanol in the production of hexanitrobibenzyl recovered by pervaporation method, which can solve the problem of easy introduction of the third component into the product, large amount of the third component, and large equipment footprint and other problems, to achieve the effect of improving energy utilization, saving reagent consumption, and reducing equipment footprint

Active Publication Date: 2016-01-06
JIANGSU NINE HEAVEN HIGH TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, the ethanol recovery method in the production of hexanitrobibenzyl mostly adopts extraction and rectification with salt addition, and ethylene glycol is generally used as the extraction agent, and extraction and rectification with salt addition is a double-tower process, which consumes a lot of steam and occupies a large area of ​​equipment. The environmental pollution is serious, and the product is easy to introduce the third component, resulting in low product purity, large amount of third component and high recycling cost

Method used

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  • Method and device for recycling ethanol in production of hexanitrostilbene

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Embodiment 1

[0040] The method of ethanol recovery in the production of hexanitrobibenzyl, the equipment used is such as figure 1 As shown, the operation process includes the following steps: the mother liquor from the hexanitrobibenzyl oxidative coupling reaction section is firstly filtered in the filter press 2, the filtrate then enters the feed liquid tank 3, and finally enters the crystallization tank 4 for crystallization, and the upper mother liquor (The water content is about 20wt%) is sent to the distillation pot 5 for concentration, and the distilled ethanol is collected in the intermediate tank 6. The volume of the mother liquor is reduced to about 25% during the distillation process, and the water content of the intermediate tank 6 is an ethanol solution of 15wt%. The material liquid in the intermediate tank 6 is delivered to the preheater 7 with a controlled flow rate of 900kg / h. The material liquid is preheated to 80°C by the product steam, and then it is heated in the evaporato...

Embodiment 2

[0046] The method of ethanol recovery in the production of hexanitrobibenzyl, the equipment used is such as figure 1 As shown, the operation process includes the following steps: the mother liquor obtained from the hexanitrobibenzyl oxidative coupling reaction section is firstly filtered in the filter press 2, the filtrate then enters the feed liquid tank 3, and finally enters the crystallization tank 4 for crystallization, the upper mother liquor (The water content is about 20wt%) is sent to the distillation pot 5 for concentration, and the distilled ethanol is collected in the intermediate tank 6. During the distillation process, the volume of the concentrated liquid is reduced to about 10%, 15%, 20%, 25%, 30%, and 35% respectively. (Mass percentage), an ethanol solution with a water content of 12 wt% in the intermediate tank 6. The flow rate in the intermediate tank 6 is controlled to 1200kg / h and sent to the preheater 7, the material liquid is preheated to 75°C by the produ...

Embodiment 3

[0052] The method of ethanol recovery in the production of hexanitrobibenzyl, the equipment used is such as figure 1 As shown, the operation process includes the following steps: the mother liquor obtained from the hexanitrobibenzyl oxidative coupling reaction section is firstly filtered in the filter press 2, the filtrate then enters the feed liquid tank 3, and finally enters the crystallization tank 4 for crystallization, the upper mother liquor (The water content is about 15wt%) is sent to the distillation pot 5 for concentration, and the distilled ethanol is collected in the intermediate tank 6. The intermediate tank 6 contains an ethanol solution with a water content of 10wt%. The ethanol in the intermediate tank 6 is transferred to the preheater 7 with a controlled flow rate of 1000kg / h. The material liquid is preheated to 85°C by the product steam, and then it is heated in the evaporator 8. The material liquid is heated to 110°C to steam The form enters into 15 NaA molec...

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Abstract

The invention relates to a method and a device for recycling ethanol in the production of hexanitrostilbene. According to the method, a mother liquid obtained in an oxidative coupling reaction section of hexanitrostilbene is filtered and crystallized, wherein ethanol serving as filtrate and crystallization liquid waste is fed to a distillation still, and products obtained from the top of the distillation still enter an intermediate tank; after being evaporated, an ethanol solution recycled through distillation is added into a pervaporation membrane separation unit to be dehydrated, high-purity ethanol is obtained from a material liquid side of the pervaporation membrane separation unit and is taken as a solvent to be returned to the oxidative coupling reaction section of hexanitrostilbene for cycle use; a permeation side of the pervaporation membrane separation unit is connected with a vacuum system, water and little ethanol in the solution in the material liquid side penetrate through a pervaporation membrane, and penetrating liquid is further returned to the distillation still after being condensed. According to the method, no other waste except water is emitted in the recycling process, the recovery rate is high, the technical process is simple, the utilization rate of energy is high, and no third component is added.

Description

Technical field [0001] The invention relates to a method and device for recovering ethanol in the production of hexanitrobibenzyl, in particular to a method and device for recovering ethanol from the production of hexanitrobibenzyl by a pervaporation method, and belongs to the application field of pervaporation membranes. Background technique [0002] Hexanitrobibenzyl is dipicrylethane with a melting point of 212°C and a light yellow powder. It is an important raw material for the two-step synthesis of heat-resistant explosive hexanitrostilbene. [0003] In the hexanitrobibenzyl oxidative coupling reaction section, the raw material TNT is first dissolved in ethanol, and then sodium hypochlorite is added. After the oxidative coupling reaction, the material liquid is filtered, washed, and crystallized to obtain the hexanitrobibenzyl product. In the above process, ethanol forms a solution with water and other trace components. If the ethanol is not recovered, it will not be recycled...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C31/08C07C29/76C07C29/80
CPCC07C29/76C07C29/80C07C31/08Y02P20/50
Inventor 纪祖焕张传恒孔维芳
Owner JIANGSU NINE HEAVEN HIGH TECH
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