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Preparation method for methylnitrate

A technology of methyl nitrate and nitric acid, which is applied in the field of preparation of methyl nitrate, can solve problems such as hindering the application of methyl nitrate, high environmental and process requirements, etc., and achieve the effects of reducing retention time, improving safety, and increasing yield

Active Publication Date: 2012-07-11
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Due to its high volatility and low boiling point, methyl nitrate has high requirements on the environment and technology in the actual application process, which hinders the further application of methyl nitrate in reality. During World War II, Germany once Use Myrol, a mixture of methanol and methyl nitrate, to equip rocket fuel, but because of the dangers in the filling process, Germany later abandoned the use of Myrol and further practical applications

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  • Preparation method for methylnitrate
  • Preparation method for methylnitrate
  • Preparation method for methylnitrate

Examples

Experimental program
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Effect test

Embodiment 1

[0026] In a 500ml three-necked flask heated by an oil bath, add 20g of urea and 5g of ammonium nitrate, add 100ml of distilled water to make them completely dissolve, and then add 30ml of 68% nitric acid in the reaction flask. When the temperature of the reaction bottle was raised to 55° C., 32 g of methanol was added dropwise, and 70 ml of 68% nitric acid was added dropwise. After reflux to 89°C, after 30 minutes, the distillation device was opened, and the crude product and water were brought out by the nitric acid vapor, which were separated rapidly. The lower layer was the product, and the upper layer was water and mixed acid. Collect until there is no effluent. Wash the collected product with water to neutrality, wash twice with 300ml of 0.05% sodium carbonate, wash twice with 500ml of water each time, obtain the crude methanol nitrate after separation, dry with dry magnesium sulfate for 36h, filter 76 g of methanol nitrate was obtained. The yield was 98.7%.

[0027] T...

Embodiment 2

[0029] In a 500ml three-necked flask heated by an oil bath, add 15g of urea and 5g of dicyandiamide, add 80ml of distilled water to dissolve it completely, then add 50ml of 68% nitric acid into the reaction flask, and mix well. When the temperature of the reaction flask was raised to 55° C., 48 g of methanol was added dropwise, and simultaneously, 50 ml of 68% nitric acid was added dropwise. Reflux to 85°C for 45 minutes, turn on the distillation device, and control the crude product and water brought out by the nitric acid vapor at 95°C, and separate quickly. The lower layer is the product, and the upper layer is water and mixed acid. Collect until there is no effluent.

[0030] Wash the collected product with water until it is neutral, then wash it twice with 1000ml of 0.05% sodium carbonate, and wash it three times with 500ml of water each time. After separation, the crude methanol nitrate is obtained, dried with dry magnesium sulfate for 36h, and filtered 111 g of methano...

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Abstract

The invention relates to a preparation method for methylnitrate and belongs to the technical field of energetic materials. The preparation method comprises the following steps: dissolving a protective agent into distilled water, adding into a three-necked bottle and then adding nitric acid; adding methanol and nitric acid dropwise and performing nitration reaction; after the reaction is finished, separating the liquid, wherein the lower layer is nitric acid ester; washing and drying the nitric acid ester to obtain a coarse product; rectifying to obtain a coarse product nitric acid ester; and rectifying and collecting a product with the boiling point of 64.5 to 66 DEG C to obtain the methylnitrate with the purity of 99.80 percent. By the method, the preparation safety is improved; the nitration yield of the product is high and can reach 97 percent; side reaction is not generated; waste water is little; and environmental pollution can not be caused.

Description

technical field [0001] The invention relates to a preparation method of methyl nitrate, belonging to the technical field of energetic materials. Background technique [0002] Methyl nitrate, also known as methanol nitrate, can be used as auxiliary fuel for liquid rocket engines or as the main fuel for fuel air explosives. [0003] Methyl nitrate is also known as methanol nitrate, methyl nitrate, and its molecular formula is CH 3 ONO 2 , the molecular weight is 77.04, the relative density (water=1) is 1.21, and the boiling point is 65.5°C. Transparent oily liquid with slight aroma, slightly soluble in water, miscible with alcohols and ethers. [0004] The general condition for preparing methyl nitrate is to carry out nitration treatment on methanol for 20 to 40 minutes with the nitration solution of concentrated nitric acid or nitric acid mixed acid (40:60) containing urea nitrate and ammonium nitrate below 18°C ​​(requiring the specific gravity of concentrated nitric acid...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C203/04C07C201/02
Inventor 刘吉平杨荣华范宝忠
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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