A method for synthesizing energetic ion compounds by bipolar membrane electrodialysis filtration and electroreaction
Through bipolar membrane electrodialysis filtration and power-up reaction method, the synthesis process of energy-containing ionic compounds is simplified, the problems of complex steps, high cost and environmental pollution in the prior art are solved, and high purity and low cost industrial production are achieved.
Patent Information
- Application Number
- CN202310365080.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-04-07
- Publication Date
- 2024-12-31
- Estimated Expiration
- 2043-04-07
AI Technical Summary
The existing ionic compounds synthesis methods have complex steps, high production costs, large reaction risk coefficients, and a large amount of solid or liquid waste, which seriously pollutes the environment and limits its industrial application.
The bipolar membrane electrodialysis filtration and electricity-adding reaction method is adopted. The high-purity synthesis of energy-containing ionic compounds is achieved by performing electrodialysis filtration and membrane filtration in aqueous solution, avoiding the use of organic solvents and drying and dehydration process, and simplifying the reaction steps.
The synthesis of high-purity energy-containing ionic compounds is achieved, which reduces production costs, avoids environmental pollution, and is suitable for large-scale industrial production.
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Figure CN116282412B_ABST
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of energetic ion compound synthesis and application, and in particular relates to a method for synthesizing energetic ion compounds through bipolar membrane electrodialysis filtration and electrical reaction. Background Art
[0002] Energetic ion compounds usually refer to compounds with a nitrogen content of more than 20%. Energetic ion compounds generally have high heat of formation and contain strong oxidizing or explosive groups. Such substances are prone to rapid decomposition, combustion or explosion. The decomposition product is clean nitrogen, so it is also called "green energetic materials" and is widely used in explosives, propellants, gunpowder and detonators.
[0003] The structure and substituent types of energetic compounds usually contain one or more NN single bonds or OO bonds, and the structure has a high decomposition activity. The representative group is hydrazine, and other groups include amino, nitro and dinitramide. Common energetic compounds include ammonium dinitramide (ADN), hydrazine nitroformate (HNF), etc.
[0004] At present, the inorganic method for synthesizing ADN mainly involves nitration of aminosulfonates with nitric and sulfuric acid mixed acids, and neutralization with ammonia water or potassium hydroxide to prepare ADN. The purification of ADN mainly uses physical methods and organic solvent methods. C. Vorde et al. provided a method for preparing KDN by reacting FOX12 with potassium hydroxide in patent US2008226533, and preparing ADN by exchanging KDN with ammonium sulfate ions. The preparation of ADN was achieved in two steps, but the method was complicated and a large amount of organic solvents were used in the experiment, which was not suitable for large-scale industrial production. Patent CN113336241B uses column chromatography to prepare and separate ADN, but the amount of column chromatography solvent is large and the concentration of the feed solution is low.
[0005] At present, the synthesis steps of energetic ion compounds are long, the salt conversion and desalination process is complicated, the production cost is high, the reaction risk factor is high, it is not conducive to industrial scale-up, and a large amount of solid or liquid waste is generated, which seriously pollutes the environment. Therefore, the synthesis method of energetic ion compounds has always restricted their preparation and application. Summary of the invention
[0006] The present invention aims at the technical problems existing in the synthesis of energetic ion compounds and proposes a method for synthesizing energetic ion compounds by bipolar membrane electrodialysis filtration plus electrical reaction, which is simple in method, easy to operate and applicable to industrial production.
[0007] In order to achieve the above object, the technical solution adopted by the present invention is: a method for synthesizing energetic ion compounds by bipolar membrane electrodialysis filtration and electrical reaction, characterized in that it comprises the following steps:
[0008] a. Firstly, a negative ion energetic compound containing metal ions is prepared into an aqueous solution to be reacted;
[0009] b. subjecting the prepared aqueous solution to an electrolysis reaction through a bipolar membrane electrodialysis filtration system to obtain a free acid solution and a base;
[0010] c. separating the free acid solution and the base, and adding a reaction amount of ammonia water or hydrazine to the free acid solution according to the potential balance and ion balance ratio to obtain an aqueous solution of an energetic compound ammonium salt or hydrazine salt;
[0011] d. Concentrating the obtained aqueous solution of the energetic compound ammonium salt or hydrazine salt through a membrane filtration system and concentrating under reduced pressure to obtain a concentrated solution;
[0012] e. Crystallize, filter and dry the concentrated solution of the energetic compound ammonium salt or hydrazine salt to obtain a high-purity energetic ion compound.
[0013] Preferably, in step a, the mass concentration of the aqueous solution of the negative ion energetic compound containing metal ions is between 1% and 15%.
[0014] Preferably, in step b, the temperature of the electrical reaction is 0°C to 15°C.
[0015] Preferably, in step b, the power-on voltage is 16V to 20V, and the charging current is 3A to 4A.
[0016] Preferably, in step b, the end point of the electrochemical reaction is when the metal ion concentration in the salt chamber is less than 10 mM.
[0017] Preferably, in step b, the end point of the charging reaction is when the concentration of energetic anions in the salt chamber is less than 10 mM.
[0018] The method for synthesizing energetic ion compounds by bipolar membrane electrodialysis filtration plus electrical reaction according to claim 1 is characterized in that, in the step c, the amount of ammonia water or hydrazine used is 1.1 to 1.2 times the amount of free acid substance, calculated as the amount of ammonia or hydrazine.
[0019] Preferably, in step d, the membrane in the membrane filtration system is a polyamide reverse osmosis membrane or a semi-aromatic polyamide reverse osmosis membrane.
[0020] Preferably, in step d, the filtration pressure of the membrane filtration system is 1.0 MPa to 6.0 MPa.
[0021] Preferably, in the step d, the concentration of the ammonium salt or hydrazine salt of the energetic compound after reduced pressure concentration is ≤50%.
[0022] Compared with the prior art, the advantages and positive effects of the present invention are:
[0023] 1. The present invention provides a method for synthesizing energetic ion compounds by bipolar membrane electrodialysis filtration and electrical reaction, which utilizes potential difference to realize the transfer and removal of metal ions by bipolar membrane-cationic membrane electrodialysis filtration and electrical reaction; or realizes the transfer of negative ion energetic compounds by bipolar membrane-negative membrane electrodialysis filtration and electrical reaction, and finally realizes the synthesis of negative ion energetic compound ammonium salt or hydrazine salt and the removal of metal ions, avoiding the use of organic solvents, avoiding the drying and dehydration of energetic compounds, avoiding the yield loss caused by repeated transfer of solid materials and the danger of operation. At the same time, the energetic ion compounds are separated and concentrated by membrane filtration and concentration, which effectively avoids the problems of high energy consumption, easy decomposition, and easy explosion generated in the conventional concentration process.
[0024] 2. The present invention utilizes bipolar membrane electrodialysis and membrane filtration to realize the synthesis of ammonium salt or hydrazine salt of energetic ion compounds. The reaction steps are simple, and the synthesis and post-treatment are all carried out under aqueous conditions, thereby avoiding the use of organic solvents, avoiding drying and dehydration in the intermediate process of post-treatment of energetic compounds, and avoiding yield loss and operational hazards caused by repeated transfer of solid materials. It has created a new method for the synthesis of energetic ion compounds and broadened the new application direction of energetic ion compounds. BRIEF DESCRIPTION OF THE DRAWINGS
[0025] In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the following briefly introduces the drawings required for use in the description of the embodiments. Obviously, the drawings described below are some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without creative work.
[0026] Figure 1 This is the schematic diagram of the electrification reaction of bipolar membrane-cationic membrane electrodialysis filtration;
[0027] Figure 2 This is the schematic diagram of the electrification reaction of bipolar membrane-anion membrane electrodialysis filtration. DETAILED DESCRIPTION
[0028] In order to more clearly understand the above-mentioned purpose, features and advantages of the present invention, the present invention is further described below in conjunction with the accompanying drawings and embodiments. It should be noted that the embodiments of the present application and the features in the embodiments can be combined with each other without conflict.
[0029] In the following description, many specific details are set forth to facilitate a full understanding of the present invention. However, the present invention may also be implemented in other ways than those described herein. Therefore, the present invention is not limited to the specific embodiments of the following disclosure.
[0030] First, the equipment of the bipolar membrane electrodialysis filtration system used in the embodiment is EDBC-17, and the equipment used in the membrane filtration system is a high-pressure flat membrane test machine TYLG-19. Among them, the bipolar membrane electrodialysis filtration system is divided into a bipolar membrane-cationic membrane electrodialysis filtration system and a bipolar membrane-anionic membrane electrodialysis filtration system. If the bipolar membrane-cationic membrane electrodialysis filtration system is selected, the metal ions in the reaction liquid are transferred to the adjacent compartment through the charged cation membrane, and the bipolar membrane completes the hydrolysis to produce OH- and metal ions to form a base; the bipolar membrane hydrolyzes and supplements H+ to form a free acid with anion energetic compounds, and the charged reaction is terminated when the metal ion concentration in the salt chamber is less than 10mM.
[0031] If a bipolar membrane-anion membrane electrodialysis filtration system is selected, the negative ion energetic compounds in the reaction liquid are transferred to the adjacent compartment through the charged anion membrane, and the bipolar membrane hydrolyzes to produce H+ and the negative ion energetic compounds to form free acid; the bipolar membrane hydrolyzes to supplement OH- and forms a base with metal ions; the charged reaction ends when the concentration of energetic negative ions in the salt chamber is less than 10mM, and the charged reaction is terminated.
[0032] The negative ion energetic compounds containing metal ions are furan, imidazole, triazole, tetrazine, tetrazole and their condensed ring derivatives.
[0033] Example 1: A method for synthesizing energetic compounds by bipolar membrane-cationic membrane electrodialysis filtration plus electrical reaction: First, the energetic compound containing metal ions is prepared into an aqueous solution with a mass fraction of 2% for standby use.
[0034] Adjust the voltage of the powered reaction device EDBC-17 of the bipolar membrane-cationic membrane electrodialysis filtration system to 16V and 3A respectively, and set it aside.
[0035] Install the reverse osmosis membrane into the high-pressure flat membrane testing machine TYLG-19, test the pure water flux at 0.4MPa and 25℃, drain the pure water and set aside.
[0036] Then, the prepared aqueous solution was added to the prepared bipolar membrane electrodialysis filtration system, the temperature was controlled at 5°C, and the bipolar membrane electrodialysis filtration charging reaction was started. + The bipolar membrane replenishes OH by moving from the positive electrode to the negative electrode and into the alkaline chamber. - Enter the alkali room and meet M + Forming MOH lye; bipolar membrane replenishes H + , and A- to form free acid until the pH of the liquid is reduced, then 1.1 to 1.2 times the amount of HA free acid substance is added to the liquid, and finally the acid-base neutralization is carried out to obtain NH 4 A reaction solution.
[0037] The above reaction is completed NH 4A reaction solution is added into the membrane filtration concentration system, and the low temperature circulation cooling device is turned on to control the filtration temperature to 10℃. The low temperature of 10℃ can ensure the NH 4 A is stable, and the pressure regulating valve is adjusted to control the filtration pressure to 4MPa. The pressure of 4MPa can ensure that the filtration flux requirements are met. 4 After the A compound is concentrated by membrane, it is further concentrated under reduced pressure to collect the 4 A's concentrate is 0.026L.
[0038] The collected 0.026L high-purity NH 4 Solution A was further concentrated and crystallized at 4°C to obtain 99.9% pure NH 4 Product A: 3.6 g, total molar yield: 93.2%.
[0039] Example 2, a method for synthesizing energetic compounds by bipolar membrane-cationic membrane electrodialysis filtration plus electrical reaction: First, the energetic compound containing metal ions is prepared into a 5% by mass aqueous solution for standby use.
[0040] Adjust the voltage of the powered reaction device EDBC-17 of the bipolar membrane-cationic membrane electrodialysis filtration system to 18V and 4A respectively, and set it aside.
[0041] Install the reverse osmosis membrane into the high-pressure flat membrane testing machine TYLG-19, test the pure water flux at 0.4MPa and 25℃, drain the pure water and set aside.
[0042] Then, the prepared aqueous solution is added to the prepared bipolar membrane-cationic membrane electrodialysis filtration system, the temperature is controlled at 10°C, and the bipolar membrane electrodialysis filtration charging reaction is started. The metal ion M+ moves toward the negative electrode through the cation membrane into the alkaline chamber, and the bipolar membrane replenishes OH - Enter the alkali room and meet M + Forming MOH lye; bipolar membrane replenishes H + , and A- to form free acid until the pH of the liquid is reduced, then 1.1 to 1.2 times the amount of HA free acid substance is added to the liquid, and finally the acid-base neutralization is carried out to obtain NH 4 A reaction solution.
[0043] The above reaction is completed NH 4 A reaction solution is added into the membrane filtration concentration system, and the low temperature circulation cooling device is turned on to control the filtration temperature to 10℃. The low temperature of 10℃ can ensure the NH 4 A is stable, and the pressure regulating valve is adjusted to control the filtration pressure to 4MPa. The pressure of 4MPa can ensure that the filtration flux requirements are met. 4 After low temperature concentration of compound A, further vacuum concentration was performed to collect the 4A's concentrate is 0.046L.
[0044] The collected 0.046L high-purity NH 4 Solution A was further concentrated and crystallized at 4°C to obtain 99.9% pure NH 4 Product A was 7.8 g, with a total molar yield of 94.5%.
[0045] Example 3: A method for synthesizing energetic compounds by bipolar membrane-cationic membrane electrodialysis filtration plus electrical reaction: First, the energetic compound containing metal ions is prepared into an aqueous solution with a mass fraction of 10% for standby use.
[0046] Adjust the voltage of the powered reaction device EDBC-17 of the bipolar membrane-cationic membrane electrodialysis filtration system to 16V and 4A respectively, and set it aside.
[0047] Install the reverse osmosis membrane into the high-pressure flat membrane testing machine TYLG-19, test the pure water flux at 0.4MPa and 25℃, drain the pure water and set aside.
[0048] Then, the prepared aqueous solution was added to the prepared bipolar membrane-cationic membrane electrodialysis filtration system, the temperature was controlled at 5°C, and the bipolar membrane electrodialysis filtration charging reaction was started. The metal ion M+ moved toward the negative electrode through the cation membrane into the alkaline chamber, and the bipolar membrane supplemented OH - Enter the alkali room and meet M + Forming MOH lye; bipolar membrane replenishes H + , and A - The free acid is formed until the pH of the feed solution decreases, and then 1.1 to 1.2 times the amount of HA free acid substance is added to the feed solution, and finally the acid-base neutralization is performed to obtain NH 4 A reaction solution.
[0049] The above reaction is completed NH 4 A reaction solution is added into the membrane filtration concentration system, and the low temperature circulation cooling device is turned on to control the filtration temperature to 10℃. The low temperature of 10℃ can ensure the NH 4 A is stable, and the pressure regulating valve is adjusted to control the filtration pressure to 4MPa. The pressure of 4MPa can ensure that the filtration flux requirements are met. 4 After low temperature concentration of compound A, further vacuum concentration was performed to collect the 4 A concentrate 0.065L.
[0050] The collected 0.065L high-purity NH 4 Solution A was further concentrated and crystallized at 4°C to obtain 99.9% pure NH 4 Product A: 15.6 g, total molar yield: 96.6%.
[0051] Example 4, a method for synthesizing energetic compounds by bipolar membrane-cationic membrane electrodialysis filtration plus electrical reaction: First, the energetic compound containing metal ions is prepared into an aqueous solution with a mass fraction of 15% for standby use.
[0052] Adjust the voltage of the powered reaction device EDBC-17 of the bipolar membrane-cationic membrane electrodialysis filtration system to 20V and 4A respectively, and set it aside.
[0053] Install the reverse osmosis membrane into the high-pressure flat membrane testing machine TYLG-19, test the pure water flux at 0.4MPa and 25℃, drain the pure water and set aside.
[0054] Then, the prepared aqueous solution is added to the prepared bipolar membrane-cationic membrane electrodialysis filtration system, the temperature is controlled at 5°C, and the bipolar membrane electrodialysis filtration charging reaction is started. The metal ion M+ moves toward the negative electrode through the cation membrane into the alkaline chamber, and the bipolar membrane replenishes OH- into the alkaline chamber and reacts with M + Forming MOH lye; bipolar membrane replenishes H + , and A- to form free acid until the pH of the liquid is reduced, then 1.1 to 1.2 times the amount of HA free acid substance is added to the liquid, and finally the acid-base neutralization is carried out to obtain NH 4 A reaction solution.
[0055] The above reaction is completed NH 4 A reaction solution is added into the membrane filtration concentration system, and the low temperature circulation cooling device is turned on to control the filtration temperature to 10℃. The low temperature of 10℃ can ensure the NH 4 A is stable, and the pressure regulating valve is adjusted to control the filtration pressure to 4MPa. The pressure of 4MPa can ensure that the filtration flux requirements are met. 4 After the A compound is concentrated by membrane, it is further concentrated under reduced pressure to collect the 4 A's concentrate is 0.093L.
[0056] The collected 0.093L high-purity NH 4 Solution A was further concentrated and crystallized at 4°C to obtain 99.9% pure NH 4 Product A: 23.7 g, total molar yield: 97.8%.
[0057] Example 5, a new technology for synthesizing energetic compounds by bipolar membrane-anionic membrane electrodialysis filtration plus electrical reaction: First, the energetic compound containing metal ions is prepared into a 3% by mass aqueous solution for standby use.
[0058] Adjust the voltage of the powered reaction device EDBC-17 of the bipolar membrane-anionic membrane electrodialysis filtration system to 20V and 4A respectively, and set it aside.
[0059] Install the reverse osmosis membrane into the high-pressure flat membrane testing machine TYLG-19, test the pure water flux at 0.4MPa and 25℃, drain the pure water and set aside.
[0060] Then, the prepared aqueous solution was added to the prepared bipolar membrane-anion membrane electrodialysis filtration system, the temperature was controlled at 5°C, and the bipolar membrane electrodialysis filtration charging reaction was started. The negative ion energetic compound A- moved toward the positive electrode through the anion membrane into the acid chamber, and the bipolar membrane supplemented H + , and A- forms a free acid, and 1.1 to 1.2 times the amount of HA free acid is added to the acid chamber, and finally the acid-base neutralization is carried out to obtain NH 4 A reaction solution.
[0061] The above reaction is completed NH 4 A reaction solution is added into the membrane filtration concentration system, and the low temperature circulation cooling device is turned on to control the filtration temperature to 10℃. The low temperature of 10℃ can ensure the NH 4 A is stable, and the pressure regulating valve is adjusted to control the filtration pressure to 4MPa. The pressure of 4MPa can ensure that the filtration flux requirements are met. 4 After the A compound is concentrated by membrane, it is further concentrated under reduced pressure to collect the 4 A's concentrate is 0.034L.
[0062] The collected 0.034L high-purity NH 4 Solution A was further concentrated and crystallized at 4°C to obtain 99.9% pure NH 4 Product A: 4.8 g, total molar yield: 94.6%.
[0063] Example 6 A method for synthesizing energetic compounds by bipolar membrane-anionic membrane electrodialysis filtration plus electrical reaction: First, the energetic compound containing metal ions is prepared into a 5% by mass aqueous solution for standby use.
[0064] Adjust the voltage of the powered reaction device EDBC-17 of the bipolar membrane-anionic membrane electrodialysis filtration system to 16V and 4A respectively, and set it aside.
[0065] Install the reverse osmosis membrane into the high-pressure flat membrane testing machine TYLG-19, test the pure water flux at 0.4MPa and 25℃, drain the pure water and set aside.
[0066] Then, the prepared aqueous solution was added to the prepared bipolar membrane-anion electrodialysis filtration system, the temperature was controlled at 10°C, and the bipolar membrane electrodialysis filtration charging reaction was started, and the anion-containing energetic compound A - The bipolar membrane replenishes H by moving from the cathode to the anode and into the acid chamber. + , and A -To form free acid, add 1.1 to 1.2 times the amount of ammonia as the free acid of HA into the acid chamber, and finally neutralize with acid and alkali to obtain NH 4 A reaction solution.
[0067] The above reaction is completed NH 4 A reaction solution is added into the membrane filtration concentration system, and the low temperature circulation cooling device is turned on to control the filtration temperature to 10℃. The low temperature of 10℃ can ensure the NH 4 A is stable, and the pressure regulating valve is adjusted to control the filtration pressure to 4MPa. The pressure of 4MPa can ensure that the filtration flux requirements are met. 4 After the A compound is concentrated by membrane, it is further concentrated under reduced pressure to collect the 4 A's concentrate is 0.042L.
[0068] The collected 0.042L high-purity NH 4 Solution A was further concentrated and crystallized at 4°C to obtain 99.9% pure NH 4 Product A was 8.1 g, with a total molar yield of 95.5%.
[0069] Example 7 A method for synthesizing energetic compounds by bipolar membrane-anionic membrane electrodialysis filtration and electrical reaction
[0070] Firstly, the energetic compound containing metal ions is prepared into a 10% by mass aqueous solution for standby use.
[0071] Adjust the voltage of the powered reaction device EDBC-17 of the bipolar membrane-anionic membrane electrodialysis filtration system to 16V and 4A respectively, and set it aside.
[0072] Install the reverse osmosis membrane into the high-pressure flat membrane testing machine TYLG-19, test the pure water flux at 0.4MPa and 25℃, drain the pure water and set aside.
[0073] Then, the prepared aqueous solution was added to the prepared bipolar membrane-anion electrodialysis filtration system, the temperature was controlled at 5°C, and the bipolar membrane electrodialysis filtration charging reaction was started, and the anion-containing energetic compound A - The bipolar membrane replenishes H by moving from the cathode to the anode and into the acid chamber. + , and A - To form free acid, add 1.1 to 1.2 times the amount of ammonia as the free acid of HA into the acid chamber, and finally neutralize with acid and base to obtain NH 4 A reaction solution.
[0074] The above reaction is completed NH 4 A reaction solution is added into the membrane filtration concentration system, and the low temperature circulation cooling device is turned on to control the filtration temperature to 10℃. The low temperature of 10℃ can ensure the NH 4A is stable, and the pressure regulating valve is adjusted to control the filtration pressure to 4MPa. The pressure of 4MPa can ensure that the filtration flux requirements are met. 4 After the A compound is concentrated by membrane, it is further concentrated under reduced pressure to collect the 4 A's concentrate is 0.062L.
[0075] The collected 0.062L high-purity NH 4 Solution A was further concentrated and crystallized at 4°C to obtain 99.9% pure NH 4 Product A: 16.3 g, total molar yield: 96.1%.
[0076] Example 8 A method for synthesizing energetic compounds by bipolar membrane-anionic membrane electrodialysis filtration plus electrical reaction: First, the energetic compound containing metal ions is prepared into an aqueous solution with a mass fraction of 15% for standby use.
[0077] Adjust the voltage of the powered reaction device EDBC-17 of the bipolar membrane-anionic membrane electrodialysis filtration system to 16V and 4A respectively, and set it aside.
[0078] Install the reverse osmosis membrane into the high-pressure flat membrane testing machine TYLG-19, test the pure water flux at 0.4MPa and 25℃, drain the pure water and set aside.
[0079] Then, the prepared aqueous solution was added to the prepared bipolar membrane-anion electrodialysis filtration system, the temperature was controlled at 5°C, and the bipolar membrane electrodialysis filtration charging reaction was started, and the anion-containing energetic compound A - The bipolar membrane replenishes H by moving from the cathode to the anode and into the acid chamber. + , and A - To form free acid, add 1.1 to 1.2 times the amount of ammonia as the free acid of HA into the acid chamber, and finally neutralize with acid and base to obtain NH 4 A reaction solution.
[0080] The above reaction is completed NH 4 A reaction solution is added to the membrane filtration concentration system 2, and the low temperature circulation cooling device is turned on to control the filtration temperature to 10°C. The low temperature of 10°C can ensure that NH 4 A is stable, and the pressure regulating valve is adjusted to control the filtration pressure to 4MPa. The pressure of 4MPa can ensure that the filtration flux requirements are met. 4 After the A compound is concentrated by membrane, it is further concentrated under reduced pressure to collect the 4 A's concentrate is 0.087L.
[0081] The collected 0.087L high-purity NH 4 Solution A was further concentrated and crystallized at 4°C to obtain 99.9% pure NH4 Product A: 24.8 g, total molar yield: 97.5%.
[0082] The results of the above examples show that the method provided by the present invention avoids the use of organic solvents, avoids drying and dehydration of energetic compounds, avoids yield loss and operational hazards caused by repeated transfer of solid materials, while ensuring yield and purity, and is suitable for large-scale promotion and use.
[0083] The above description is only a preferred embodiment of the present invention and does not limit the present invention in other forms. Any technician familiar with the profession may use the technical content disclosed above to change or modify it into an equivalent embodiment with equivalent changes and apply it to other fields. However, any simple modification, equivalent change and modification made to the above embodiment based on the technical essence of the present invention without departing from the content of the technical solution of the present invention still falls within the protection scope of the technical solution of the present invention.
Claims
1. A method for synthesizing energetic ion compounds by bipolar membrane electrodialysis filtration and electroreaction, characterized in that: The following steps are involved: a. Firstly, a negative ion energetic compound containing metal ions is prepared into an aqueous solution to be reacted; b. subjecting the prepared aqueous solution to an electrolytic reaction through a bipolar membrane electrodialysis filtration system to obtain a free acid solution and a base; c. separating the free acid solution and the base, and adding a reaction amount of ammonia water or hydrazine to the free acid solution according to the potential balance and ion balance ratio to obtain an aqueous solution of an energetic compound ammonium salt or hydrazine salt; d. Concentrating the obtained aqueous solution of the energetic compound ammonium salt or hydrazine salt through a membrane filtration system and concentrating under reduced pressure to obtain a concentrated solution; e. Crystallize, filter and dry the concentrated solution of the energetic compound ammonium salt or hydrazine salt to obtain a high-purity energetic ion compound. Wherein, in the step a, the mass concentration of the aqueous solution of the negative ion energetic compound containing metal ions is between 1% and 15%, in the step b, the temperature of the electrochemical reaction is 0°C to 15°C, in the step b, the electrochemical voltage is 16V to 20V, and the charging current is 3A to 4A. In the step b, the electrochemical reaction ends when the metal ion concentration in the salt chamber is less than 10mM. In the step b, the electrochemical reaction ends when the energetic negative ion concentration in the salt chamber is less than 10mM. In the step c, the amount of ammonia water or hydrazine used is 1.1 to 1.2 times the amount of free acid substance in terms of the amount of ammonia or hydrazine. In the step d, the membrane in the membrane filtration system is a polyamide reverse osmosis membrane or a semi-aromatic polyamide reverse osmosis membrane. In the step d, the filtration pressure of the membrane filtration system is 1.0MPa to 6.0MPa. In the step d, the concentration of the ammonium salt or hydrazine salt of the energetic compound after reduced pressure concentration is ≤50%.
