Method for preparing ethyl nitrate by continuously nitrifying nitric acid steam

A technology of ethyl nitrate and nitric acid, which is applied in the preparation of nitrate esters, organic chemistry, etc., can solve the problems of not being used as military explosives, and achieve the effects of shortening the residence time, shortening the residence time, and reducing the chance of death

Active Publication Date: 2012-07-04
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, it has not been used as a military explosive due to its volatilization and liquid

Method used

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  • Method for preparing ethyl nitrate by continuously nitrifying nitric acid steam
  • Method for preparing ethyl nitrate by continuously nitrifying nitric acid steam
  • Method for preparing ethyl nitrate by continuously nitrifying nitric acid steam

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] Add protective agent and water to the 500ml reactor with oil bath heating device, the total addition is 160ml (about 185g) of nitrating agent, and the mass percentage content of three parts of nitrating agent is: HNO 3 75%, H 2 O is 15%, and protecting agent is 10%; Wherein, the mass percentage of protecting agent is urea 70%, dicyandiamide is 20%, and melamine is 10%;

[0042] First add 13g of urea, 3.7g of dicyandiamide, and 2g of melamine into the reactor system, add 28ml of water, make it completely dissolved, and then add 38g of 68% nitric acid, completely mix with this protective agent, and wait until the temperature of the system rises to 60 2mol absolute ethanol (92g) and 100g of 68% nitric acid were slowly added dropwise at °C, the temperature was raised to 90°C and reflux was started for 5 minutes. While refluxing, the product is initially distilled out. The upper layer of the crude product obtained at a distillation temperature of 90°C is unreacted ethanol, ...

Embodiment 2

[0046] Add protective agent and water to the 1000ml reactor with oil bath heating device, the total addition amount is 300ml (about 3500g) of nitrating agent, and the mass percentage content of three parts of nitrating agent is: HNO 3 75%, H 2 O is 15%, and protecting agent is 10%; Wherein, the mass percentage of protecting agent is urea 50%, and dicyandiamide is 50%;

[0047] In the reactor, first add protective agent and water, then add a little nitric acid participating in the reaction; slowly add 55mol absolute ethanol (2630g) dropwise when the temperature of the system rises to 60°C, heat up to 88°C and begin to reflux for 10 minutes, when the temperature rises to Stop reflux at 91°C. Control the drop rate of ethanol and nitric acid. At this time, the product is initially distilled while refluxing. The distillation temperature of the system is maintained at 90 ° C. The upper layer of the obtained crude product is unreacted ethanol, and the lower layer is crude ester and ...

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Abstract

The invention discloses a method for preparing ethyl nitrate by continuously nitrifying nitric acid steam, which belongs to the field of energetic materials. The method comprises the steps of preparing a nitrifying agent, heating the nitrifying agent to 40-60 DEG C, adding dropwise ethanol and nitric acid, and separating liquid after the addition, wherein ethyl nitrate is positioned in the lower layer; and finally washing, drying and rectifying the ethyl nitrate to obtain pure ethyl nitrate. The method changes the traditional nitrifying method for preparing the ethyl nitrate, effectively uses the steam produced by nitrifying under the protection of carbonyl groups, enables products to be moved out fast, controls the feeding speed and the product production in order, shortens the residence time of nitrate in a heating environment, slows the production of nitrous acid products, and improves the safety of production and preparation processes.

Description

technical field [0001] The invention relates to a method for preparing ethyl nitrate by continuous nitration of nitric acid vapor, belonging to the field of energetic materials. Background technique [0002] Alkyl monohydric alcohol nitrates can be used as auxiliary fuel for liquid rocket engines, or as the main fuel for fuel air explosives; [0003] Alcohol nitrate is a colorless transparent liquid with good fluidity, slightly soluble in water (increased solubility with increasing temperature) and miscible with ethanol, benzene, acetone and other organic solvents. There is a sweet ester smell (but excessive inhalation is harmful, the toxicity is similar to nitroglycerin causing headaches, but the action is faster than nitroglycerin and the duration is shorter) Boiling point: 88.7 degrees does not decompose and is volatile when boiling, heat of combustion: 322kc / mol, in the open Under the conditions, it burns rapidly and produces a green flame with NOx odor. Confined space...

Claims

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Application Information

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IPC IPC(8): C07C203/04C07C201/02
Inventor 刘吉平杨荣华王虎王晓君范宝忠
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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