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Method for electrochemical synthesis of HMX

An electrochemical and mixed solution technology, which is applied in the synthesis of Oktokin and the field of electrochemical synthesis of HMX, can solve the problem of low yield and achieve the effect of simple operation and low cost

Active Publication Date: 2022-04-15
XIAN MODERN CHEM RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Although there are many ways to synthesize HMX using DPT as a raw material, the yields are relatively low, and the product needs to undergo post-washing, recrystallization and other treatments to meet the requirements of the national military standard for purity, acidity and crystal form, so the yield of HMX is increased. is the main problem to be solved at present

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] This example discloses a preparation method of 3,7-dinitro-1,3,5,7-tetraazabicyclo[3.3.1]nonane (DPT):

[0028] At -5-0°C, add 5g of urea in batches to 11.5mL of 95% fuming nitric acid and 10.5mL of 20% fuming sulfuric acid solution, and stir at 0-5°C for 60min after the addition is complete. Then pour into 30g of ice water for hydrolysis for 90 minutes, and add 40.8mL of 37% formaldehyde solution dropwise at a temperature not exceeding 20°C. Then heat to 40°C, stir for 40 minutes, and cool down. Neutralize with 25% ammonia water at 20-25°C to pH 7.5, stirred at 20°C for 60min, filtered, washed with water, and dried at room temperature to obtain 11.84g of 3,7-dinitro-1,3,5,7-tetraazabicyclo[3.3.1]nonane white Solid, 65.2% yield.

Embodiment 2

[0030] At -20°C, mix 2.6g of ammonium nitrate and 25.8g of fuming nitric acid solution to obtain a fuming nitric acid solution of ammonium nitrate, add 0.9g of dinitrogen tetroxide to the fuming nitric acid solution of ammonium nitrate, dissolve, and divide Add 2.0g of the DPT of Example 1 in batches, after the addition, react for 10min, then slowly add 7ml of deionized water dropwise to the system, the deionized water drop rate is 2-5s per drop, to keep the system temperature below -15°C, after the addition is complete The mixed solution was electrolyzed in a two-electrode two-chamber electrolyzer, the electrolysis time was 1 h, the electrolysis temperature was 8°C, and the electrolysis voltage was 3.5V.

[0031] The solution after electrolysis was poured into ice water to precipitate, filtered, washed, and dried to obtain 1.99 g of HMX white solid, with a yield of 74.2%.

Embodiment 3

[0033] At -25°C, mix 2.6g of ammonium nitrate and 25.8g of fuming nitric acid solution to obtain a fuming nitric acid solution of ammonium nitrate, add 0.7g of sodium nitrite to the fuming nitric acid solution of ammonium nitrate, dissolve it, and then batch Add 2.0g of DPT from Example 1, after the addition, react for 10min, slowly add 7ml of water dropwise to the system, the deionized water drop rate is 2-5s per drop, to keep the system temperature below -15°C, after the addition is completed, place it on the Carry out electrolysis in two-chamber electrolyzer, electrolysis time, temperature, voltage are equal to embodiment 2.

[0034] The dissolved solution after electrolysis was poured into ice water to precipitate, filtered, washed and dried to obtain 2.00 g of HMX as a white solid with a yield of 74.6%.

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Abstract

The invention discloses a method for electrochemical synthesis of HMX, which specifically comprises the following steps: mixing nitrogen tetroxide or sodium nitrite with ammonium nitrate, fuming nitric acid and DPT at-25 to-15 DEG C, reacting for 5-10 minutes, then adding deionized water, and ensuring that the system temperature is-25 to-15 DEG C in the deionized water adding process to obtain a mixed solution; carrying out electrolysis in a two-pole two-chamber electrolytic bath by taking the mixed solution as an electrolyte; and separating out, filtering, washing and drying the electrolyzed solution to obtain HMX. According to the method, DPT is used as a raw material and mixed with fuming nitric acid, ammonium nitrate and dinitrogen tetroxide, then HMX is obtained through an electrolysis method, the preparation method is easy and convenient to operate and low in cost, and the yield of the final product can reach 75.1%; and the obtained product does not need post-treatment and can directly meet the requirements of national military standards.

Description

technical field [0001] The invention belongs to the technical field of propellant and explosive synthesis, in particular to the synthesis of Octogen (HMX), in particular to a method for electrochemically synthesizing HMX. Background technique [0002] Octojin (HMX) is the high-energy explosive with the best comprehensive performance used in the military today. It has high density, high energy and excellent thermal stability, and has broad application prospects in my country's national defense construction. [0003] With 3,7-dinitro-1,3,5,7-tetraazabicyclo[3.3.1]nonane (DPT) at present, there are many studies on the synthesis of Octogen as raw material, for example: Li Quanliang et al. "Research on DPT Preparation of HMX", "Energetic Materials", Volume 15, Issue 5, 509-510, 2007, discloses a method for preparing HMX using DPT as a raw material. Using DPT as raw material, using fuming nitric acid, ammonium nitrate and magnesium oxide solution as nitrating agent for nitration ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25B3/05C25B3/07C25B3/09C07D487/08
CPCC25B3/05C25B3/07C25B3/09C07D487/08
Inventor 陈志强郭涛李洪丽姜俊郑晓东邱少君贺虎林姚冰洁石强秦明娜唐望王子俊陈劭力吕英迪葛忠学
Owner XIAN MODERN CHEM RES INST
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