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Preparation method of 2-fluoro-2, 2-dinitroethanol

A technology of dinitroethanol and dinitroacetylurea, which is applied in the field of energetic material preparation, can solve problems such as inability to apply engineering, achieve cheap and easy-to-obtain experimental operations, overcome expensive raw materials, and achieve high yields

Inactive Publication Date: 2019-06-18
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0014] The present invention overcomes the deficiencies of the prior art and provides a method for preparing 2-fluoro-2,2-dinitroethanol, which can efficiently and safely prepare the energetic compound 2-fluoro-2,2-dinitroethanol at low cost. Dinitroethanol overcomes the defect that the prior art cannot be applied in engineering

Method used

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  • Preparation method of 2-fluoro-2, 2-dinitroethanol
  • Preparation method of 2-fluoro-2, 2-dinitroethanol

Examples

Experimental program
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Effect test

Embodiment 1

[0035] (1) Preparation of dinitromethane methane salt

[0036] Measure 60ml of 95%-98% concentrated sulfuric acid and add it to a 250mL three-neck flask with a thermometer, control the temperature at 0-10°C, add 12.8g of barbituric acid in batches, and wait for the barbituric acid Add 10 mL of fuming nitric acid when it is almost dissolved, control the temperature below 25°C, slowly add it dropwise to the above solution, after the drop is complete, heat up to 45°C, the solution is white viscous liquid, continue to stir for 4 hours, there is a large amount of white powder After the reaction, it was cooled, filtered with suction, washed with trifluoroacetic acid (2 mL×5), and placed in a fume hood to air-dry overnight to obtain 20.60 g of a white powder solid with a yield of 92%.

[0037] Add 5g of compound 1 to a 100mL monoclinic flask, add 10mL of water, and stir at room temperature for 2 hours. During this period, a large number of bubbles are found, the solution is yellow, a...

Embodiment 2

[0046] (1) Preparation of dinitromethane methane salt

[0047] Measure 60mL of 95%-98% concentrated sulfuric acid and add it to a 250ml three-neck flask with a thermometer, control the temperature at 0-10°C, add 12.8g of barbituric acid in batches, and wait for the barbituric acid Add 10 ml of fuming nitric acid when it is almost dissolved, control the temperature below 25°C, slowly add it dropwise to the above solution, after the drop is complete, heat up to 45°C, the solution is white viscous liquid, continue to stir for 4 hours, there is a large amount of white powder After the reaction, it was cooled, filtered with suction, washed with trifluoroacetic acid (2 mL×5), and placed in a fume hood to air-dry overnight to obtain 20.60 g of a white powder solid with a yield of 92%.

[0048] Add 5g of compound 1 to a 100mL monoclinic flask, add 15mL of water, and stir at room temperature for 2 hours. During this period, a large amount of bubbles are found, the solution is yellow, a...

Embodiment 3

[0056] (1) Preparation of dinitromethane methane salt

[0057] Measure 60mL of 95%-98% concentrated sulfuric acid and add it to a 250mL three-neck flask with a thermometer, control the temperature at 0-10°C, add 12.8g of barbituric acid in batches, and wait for the barbituric acid Add 10 mL of fuming nitric acid when it is almost dissolved, control the temperature below 25°C, slowly add it dropwise to the above solution, after the drop is complete, heat up to 45°C, the solution is white viscous liquid, continue to stir for 4 hours, there is a large amount of white powder After the reaction, it was cooled, filtered with suction, washed with trifluoroacetic acid (2 mL×5), and placed in a fume hood to air-dry overnight to obtain 20.60 g of a white powder solid with a yield of 92%.

[0058] Add 5g of compound 1 to a 100mL monoclinic flask, add 5ml of water, and stir at room temperature for 2 hours. During this period, a large number of bubbles are found, the solution is yellow, an...

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Abstract

The invention discloses a preparation method of 2-fluoro-2, 2-dinitroethanol. The method includes: taking barbituric acid as the raw material, adopting concentrated sulfuric acid and fuming nitric acid as the nitrating agent, and conducting nitration and hydrolysis to obtain gem-dinitroacetylurea, then further performing hydrolysis in an alkaline aqueous solution of KOH to reach a yield of 87% andobtain an intermediate dinitromethane potassium salt, then carrying out addition reaction with a 37% formaldehyde solution under an alkaline condition to obtain 2, 2-dinitroethanol potassium salt, and finally using a selective fluorination reagent 1-chloromethyl-4-fluoro-1, 4-diazoniabicyclo2.2.2 octane bis(tetrafluoroboric acid)salt to acquire 2-fluoro-2, 2-dinitroethanol at room temperature with a yield up to 86%. The synthesis method overcomes the shortcomings of the existing technology. The preparation method has the characteristics of high production efficiency, low material cost, maturity and stability, safety and reliability, simple and easily operable synthesis steps, and simple process, and has engineering application prospects.

Description

technical field [0001] The invention relates to the field of energetic material preparation, and more specifically, the invention relates to a preparation method of an energetic compound 2-fluoro-2,2-dinitroethanol. Background technique [0002] 2-Fluoro-2,2-dinitroethanol is an important energetic compound. It is not only used as an energetic component of propellants and explosives, but also the main component for preparing most fluorodinitro energetic compounds. Intermediates, so it appears that the status of fluorodinitroethanol is particularly important. Adolph at the U.S. Naval Laboratory in the late 1960s [28] A method for preparing fluorine-containing FDNE was reported, and the main process used was the reduction of fluorotrinitromethane. The method is to prepare fluorodinitroethanol by reducing fluorotrinitromethane with hydrogen peroxide in the presence of formaldehyde under alkaline conditions. This reaction is a strong exothermic reaction, and the reaction formu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C201/12C07C205/26C07C205/15C07C205/02C07D239/60C07C273/18C07C275/50
Inventor 程广斌王伟霞熊华林杨红伟
Owner NANJING UNIV OF SCI & TECH
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