Process and system for the preparation of hydroxylamine nitrate

Abstract

The application discloses a process and system for preparing hydroxylamine nitrate, wherein the process for preparing hydroxylamine nitrate comprises the following steps: obtaining modified nano-metal cation resin by loading nano-metal oxide on an acidic cation resin to form the modified nano-metal cation resin; and preparing hydroxylamine nitrate solution by filling the modified nano-metal cation resin into an ion exchange column, obtaining hydroxylamine hydrochloride solution, adding the hydroxylamine hydrochloride solution into the ion exchange column to adsorb the hydroxylamine hydrochloride by the modified nano-metal cation resin, removing the adsorbed chloride ions by water washing, and desorbing the hydroxylamine in the modified nano-metal cation resin by using nitric acid solution to obtain the hydroxylamine nitrate solution. The modified nano-metal cation resin is applied in the process for preparing hydroxylamine nitrate by ion exchange with hydroxylamine hydrochloride solution as raw material, so that the selection performance and adsorption performance of the cation resin can be effectively improved, and the adsorption capacity and conversion efficiency of the cation resin are effectively improved.

Description

Technical Field

[0001] This invention relates to the field of hydroxylamine nitrate preparation, and more specifically to a process and system for preparing hydroxylamine nitrate. Background Technology

[0002] In nuclear fuel reprocessing plants employing the PUREX process, plutonium separation and purification are achieved by reducing Pu(Ⅳ), which is easily extracted by TBP, to Pu(Ⅲ), which is less easily extracted, thus separating uranium and purifying plutonium. Hydroxylamine nitrate (HAN) is a salt-free organic reagent capable of reducing Pu(Ⅳ) to Pu(Ⅲ). It is characterized by reagent stability and simple reaction products and has been widely used in reprocessing plants.

[0003] Hydroxylamine nitrate is a monoclinic crystal with a melting point of 48°C, molecular formula NH₂OHNO₃, molecular weight of 98, and decomposes at 100°C. Solid HAN is highly hygroscopic, rapidly absorbing moisture from the air and deliquescing into a liquid. There are various methods for preparing HAN, which can be broadly classified into two categories based on the starting materials used: one uses nitric acid or nitrogen oxides as raw materials, undergoing a reduction reaction to produce HAN, such as the catalytic reduction method; the other uses free hydroxylamine or hydroxylamine salts (e.g., hydroxylamine sulfate) as raw materials, neutralizing them with nitric acid or replacing other acid radicals in the hydroxylamine salt with nitrate ions to obtain HAN, such as the ion exchange method.

[0004] The ion exchange method for preparing hydroxylamine nitrate has been successfully applied in a pilot plant. However, with increasing throughput and processing capacity, the requirements for the adsorption-desorption performance of the ion exchange resin and the production capacity of hydroxylamine nitrate are becoming increasingly stringent. The adsorption-desorption performance of the currently used ion exchange resin and the production capacity of hydroxylamine nitrate need further optimization. Therefore, optimizing the adsorption performance of the exchange resin and the hydroxylamine nitrate preparation process to address the issues of feed supply and stability after scale-up of the feeding system are urgent technical problems to be solved. Summary of the Invention

[0005] Therefore, the technical problem to be solved by the present invention is to overcome the defects in feeding stability caused by the scale-up of the feeding system, thereby providing a process and system for preparing hydroxylamine nitrate to solve the above problems.

[0006] A process for preparing hydroxylamine nitrate includes the following steps:

[0007] Obtaining modified nano-metal cation resin: Nano-metal oxides are loaded onto acidic cation resin to form modified nano-metal cation resin;

[0008] Preparation of hydroxylamine nitrate solution: Modified nano-metal cation exchange resin was filled into an ion exchange column to obtain hydroxylamine hydrochloride solution, which was then added to the ion exchange column. The modified nano-metal cation exchange resin adsorbed the hydroxylamine hydrochloride. The adsorbed chloride ions were removed by washing with water, and then the hydroxylamine in the modified nano-metal cation exchange resin was desorbed with nitric acid solution to obtain hydroxylamine nitrate solution.

[0009] The process of loading the nano-metal oxide onto the acidic cation exchange resin is as follows:

[0010] Resin pretreatment: Clean the acidic cation exchange resin by soaking it in a chloride ion solution, then rinse it with water again, and dry it for later use.

[0011] Reaction: Obtain a metal salt, mix it with a solvent to obtain a metal salt solution, mix the pretreated acidic cation exchange resin with the metal salt solution, add an alkaline solution to react with the metal salt to form a metal hydroxide, and heat and age to generate a metal oxide from the metal hydroxide.

[0012] The modified nano-metal cation resin was obtained by washing and drying.

[0013] The concentration of the metal salt solution is 1.75 g / 100 mL;

[0014] And / or, the solvent is an aqueous methanol solution or an aqueous ethanol solution;

[0015] And / or, the concentration of the alkaline solution is 2-2.5 mol / L;

[0016] And / or, the molar ratio between hydroxide ions and metals in the alkaline solution is 1.4 or higher;

[0017] The chloride-containing solution is a saturated NaCl solution or a hydrochloric acid solution, preferably a saturated NaCl solution. Sodium chloride can convert the acidic cation exchange resin into a sodium-form resin, which can better adsorb cations in water, and the resin does not release hydrogen ions during the reaction. Strong acids are not used during regeneration; using sodium chloride for regeneration is safer.

[0018] The reaction time is 30-60 minutes;

[0019] And / or, the heating aging temperature is 100°C and the heating aging time is 12 hours.

[0020] In the washing step, deionized water is used for washing;

[0021] And / or, the drying temperature is 60-80℃, and the drying time is 10-12h.

[0022] The nano-metal oxide includes at least one of MnO2, Fe3O4, SnO2, CeO2, and ZrO2; to form the nano-metal oxide, the metal salt should be at least one of Mn salt, Fe salt, Sn salt, Ce salt, and Zr salt, and the metal salt is more preferably a metal chloride salt or a metal nitrate.

[0023] And / or, the acidic cation exchange resin includes an ion exchange resin containing at least one of the following groups: sulfonic acid group (-SO3H), carboxylic acid group (-COOH), phosphoric acid group (-PO3H2) and phenolic group (-OH);

[0024] And / or, the concentration of the hydroxylamine hydrochloride solution is 2-2.5 mol / L;

[0025] And / or, the concentration of the nitric acid solution is 2-2.5 mol / L.

[0026] The acidic cation exchange resin is of type D001, D201, D301 or D400.

[0027] The system based on the above-described process for preparing hydroxylamine nitrate includes:

[0028] An ion exchange column filled with modified nano-metal cation exchange resin;

[0029] A hydroxylamine hydrochloride preparation tank is used to prepare hydroxylamine hydrochloride solution, and its outlet is connected to the inlet of the ion exchange column via a hydroxylamine hydrochloride metering pump.

[0030] The deionized water high-level tank has its outlet connected to the inlet of the ion exchange column for cleaning the ion exchange column.

[0031] The nitric acid preparation tank is used to prepare nitric acid solution, and its outlet is connected to the inlet of the ion exchange column via a nitric acid metering pump.

[0032] The neutralization tank, connected to the outlet of the ion exchange column, is used to hold the chloride ions removed during washing.

[0033] The outer surface of the ion exchange column is also provided with a jacket and a cooling water circulator installed on the jacket;

[0034] And / or, the nitric acid preparation tank is also connected to a nitric acid metering tank for holding analytical grade nitric acid.

[0035] The outlet of the deionized water high-level tank is also equipped with a deionized water metering pump.

[0036] An acid-base neutralization centrifugal pump is also installed at the outlet of the neutralization tank.

[0037] The pump head material of the hydroxylamine hydrochloride metering pump includes, but is not limited to, PVC hydraulic end, 316 hydraulic end, PVDF hydraulic end, black PP hydraulic end, and hydraulic ends applicable to the above metering pumps.

[0038] Preferably, the hydroxylamine hydrochloride metering pump adds the ion exchange column at a flow rate of 7-14 L / min, and / or the nitric acid metering pump adds the ion exchange column at a flow rate of 7-14 L / min.

[0039] Preferably, the process operating conditions are as follows: deionized water and hydroxylamine hydrochloride are added through the feed port and mechanically stirred for 5-20 minutes; the hydrochloric acid washed off is discharged into a neutralization tank and neutralized with 40-45% NaOH; when the resin volume in the ion exchange column is controlled at 950-1000L, the volume of the nitric acid solution for desorbing hydroxylamine is 1400-1450L; the equipment requires cooling, and 0.5-1MPa production water is circulated into the jacket for cooling, with the adsorption temperature at 40-50℃.

[0040] When desorption begins, the water flowing down should be drained first. Once hydroxylamine nitrate is detected by sampling, switch the valve, and the desorbed hydroxylamine nitrate will flow by gravity into the hydroxylamine nitrate storage tank. When the resin volume is controlled at 950-1000L, the desorbed hydroxylamine nitrate product will be approximately 750-800L, with a concentration of approximately 1.0-1.5mol / L.

[0041] The technical solution of this invention has the following advantages:

[0042] 1. This invention provides a process for preparing hydroxylamine nitrate, using hydroxylamine hydrochloride solution and nitric acid solution as raw materials. Ion exchange is performed through a modified nano-metal cation exchange resin. Even after scale-up of the feeding system, the process effectively maintains feeding stability and significantly improves the conversion rate of hydroxylamine nitrate, meeting the needs of large-scale post-processing plants. The modified nano-metal cation exchange resin refers to a process in which inorganic substances such as nano-sized metal particles, metal oxides, and hydroxides are loaded onto a cation exchange resin as modifiers. This modified nano-metal cation exchange resin is used in the process of generating hydroxylamine nitrate from hydroxylamine hydrochloride solution as a raw material. It effectively enhances the selectivity and adsorption performance of the cation exchange resin, thereby significantly improving its adsorption capacity and conversion efficiency.

[0043] 2. The system for preparing hydroxylamine nitrate provided by the present invention combines a hydroxylamine hydrochloride preparation tank, a deionized water high-level tank, a nitric acid preparation tank, and a neutralization tank. By alternately feeding and discharging materials through two or more sets of ion exchange columns, the system can effectively achieve the process requirements of automatic and continuous feeding of raw materials. Furthermore, the system can effectively perform quantitative operation by cooperating with a hydroxylamine hydrochloride metering pump and a nitric acid metering pump, and has the advantages of stability and speed. Attached Figure Description

[0044] To more clearly illustrate the specific embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the specific embodiments or the prior art will be briefly introduced below. Obviously, the drawings described below are some embodiments of the present invention. For those skilled in the art, other drawings can be obtained from these drawings without creative effort.

[0045] Figure 1 This is a schematic diagram of the system in Embodiment 1 of the present invention.

[0046] Figure label:

[0047] 1-Ion exchange column, 2-hydroxylamine hydrochloride preparation tank, 3-deionized water high-level tank, 4-nitric acid metering tank, 5-nitric acid preparation tank, 6-neutralization tank, 7-hydroxylamine hydrochloride metering pump, 8-deionized water metering pump, 9-nitric acid metering pump, 10-acid-base neutralization centrifugal pump, 11-cooling water circulator. Detailed Implementation

[0048] The following embodiments are provided to better understand the present invention and are not limited to the preferred embodiments described. They do not constitute a limitation on the content and scope of protection of the present invention. Any product that is the same as or similar to the present invention, derived by any person under the guidance of the present invention or by combining the features of the present invention with other prior art, falls within the protection scope of the present invention.

[0049] For experiments not specifically described in the examples, the procedures or conditions should be followed according to the conventional experimental procedures described in the literature in this field. Reagents or instruments whose manufacturers are not specified are all commercially available conventional reagent products.

[0050] Example 1

[0051] A system for preparing hydroxylamine nitrate, such as Figure 1 As shown, the system includes: an ion exchange column 1, a hydroxylamine hydrochloride preparation tank 2, a deionized water elevating tank 3, a nitric acid preparation tank 5, and a neutralization tank 6. The ion exchange column 1 is filled with modified nano-metal cation exchange resin. The hydroxylamine hydrochloride preparation tank 2 is used to prepare the hydroxylamine hydrochloride solution, and its outlet is connected to the inlet of the ion exchange column 1 via a hydroxylamine hydrochloride metering pump 7. The deionized water elevating tank 3 is used to clean the ion exchange column 1, and its outlet is connected to the inlet of the ion exchange column 1 via a deionized water metering pump 8. The nitric acid preparation tank 5 is used to prepare the nitric acid solution, and its outlet is connected to the inlet of the ion exchange column 1 via a nitric acid metering pump 9. The neutralization tank 6 is used to hold the chloride ions removed during washing in the ion exchange column 1, and its inlet is connected to the outlet of the ion exchange column 1. The aforementioned hydroxylamine hydrochloride metering pump and nitric acid metering pump work together to achieve effective quantitative operation, offering advantages of stability and speed.

[0052] Meanwhile, the number of ion exchange columns 1 in the above system is preferably set to at least two sets, and the at least two sets of ion exchange columns 1 are used alternately, which can effectively achieve the process requirements of automatic and continuous feeding of raw materials.

[0053] The process by which the above system achieves ion exchange is as follows:

[0054] Deionized water is added to hydroxylamine hydrochloride preparation tank 2, and solid hydroxylamine hydrochloride is added to hydroxylamine hydrochloride preparation tank 2 through the feed port. The mixture is mechanically stirred to prepare a hydroxylamine hydrochloride solution. The prepared hydroxylamine hydrochloride solution is then added to ion exchange column 1. After chloride ions and hydroxylamine are adsorbed by the exchange column, deionized water is added to ion exchange column 1 from deionized water high-level tank 3 via deionized water metering pump 8 to wash the adsorbed hydroxylamine and remove chloride ions (i.e., hydrochloric acid) from the exchange column. The washed hydrochloric acid is discharged into neutralization tank 6. A nitric acid solution is prepared in nitric acid preparation tank 5. Specifically, analytical grade nitric acid is added to nitric acid metering tank 4, and the analytical grade nitric acid and deionized water from nitric acid metering tank 4 are simultaneously added to nitric acid preparation tank 5 and mixed with mechanical stirring to obtain a nitric acid solution. Finally, the prepared nitric acid solution is added to ion exchange column 1 via nitric acid metering pump 9 to desorb the adsorbed hydroxylamine in ion exchange column 1, yielding hydroxylamine nitrate.

[0055] During the ion exchange process described above, deionized water and hydroxylamine hydrochloride are added to the hydroxylamine hydrochloride preparation tank 2 through the feed port, and the mechanical stirring time is 5-20 minutes; the concentration of the hydroxylamine hydrochloride solution in the hydroxylamine hydrochloride preparation tank 2 is 2-2.5 mol / L, and the concentration of the nitric acid solution in the nitric acid preparation tank 5 is 2-2.5 mol / L; the resin volume in the ion exchange column 1 is controlled to be 950-1000L, of which the volume of the nitric acid solution for desorbing hydroxylamine is 1400-1450L.

[0056] In the above process, the ion exchange column 1 needs to be cooled. Therefore, a jacket and a cooling water circulator 11 are provided on the outer surface of the ion exchange column 1 to cool the column by introducing 0.5-1MPa production water into the jacket to control the temperature during adsorption to 40-50℃.

[0057] The hydrochloric acid washed off is discharged into a neutralization tank. In order to better treat it, the hydrochloric acid washed off in the neutralization tank is neutralized with NaOH of a concentration of 40-45%. For example, the hydrochloric acid washed off can be mechanically stirred with 42% NaOH for 5 minutes. After sampling and analysis, if it is neutral, it is discharged into the indoor drainage ditch by acid-base neutralization centrifugal pump 10.

[0058] Specifically, in this embodiment, the process for preparing hydroxylamine nitrate is as follows:

[0059] The modified nano-metal cation resin was prepared as follows: 3.5 g of Mn(NO3)2·4H2O was weighed and transferred to a three-necked flask. 200 mL of a 1:1 mixture of water and methanol was added. The mixture was heated using a heating mantle or a constant-temperature water bath, maintaining a stable reaction temperature of 25 °C. 2 g of D001 resin was then added, along with 10 mL of a 2 mol / L NaOH solution. The mixture was reacted at room temperature with stirring for 30 min, followed by aging in a 100 °C oven for 24 h. The aged resin was filtered, washed with deionized water until neutral, and then baked at 60 °C for 10 h to obtain the modified nano-metal cation resin.

[0060] 962 L of modified nano-metal cation exchange resin was packed into an ion exchange column 1 with a diameter (D) = 750 mm and a height (H) = 4000 mm. A 2 mol / L hydroxylamine hydrochloride solution was prepared in a hydroxylamine hydrochloride preparation tank. Specifically, deionized water and solid hydroxylamine hydrochloride were added through pipelines and feed ports, and then mechanically stirred for 15 minutes to obtain the hydroxylamine hydrochloride solution. The prepared hydroxylamine hydrochloride solution was added to the ion exchange column via a hydroxylamine hydrochloride metering pump at a flow rate of 8 L / min, with a total addition volume of 700 L. After hydroxylamine was adsorbed by the exchange column, it was washed with 650 L of deionized water. Deionized water from a high-level deionized water tank was added to the ion exchange column via a metering pump at a flow rate of 8 L / min to wash away chloride ions. The washed hydrochloric acid was discharged through pipelines to a neutralization tank, neutralized with 42% NaOH, and then pumped out to the indoor drainage ditch. Finally, 1450 L of 2 mol / L nitric acid solution was added to the ion exchange column at a flow rate of 10 L / min, and 750 L of hydroxylamine nitrate solution was desorbed.

[0061] After testing and conversion of the hydroxylamine nitrate solution, the results showed that the conversion rate of hydroxylamine nitrate in this process was 95%.

[0062] Example 2

[0063] A process for preparing hydroxylamine nitrate, using the system for preparing hydroxylamine nitrate as described in Example 1, is as follows:

[0064] The modified nano-metal cation resin was prepared as follows: 3.5 g of Mn(NO3)2·4H2O was weighed and transferred to a three-necked flask. 200 mL of a 1:1 mixture of water and methanol was added. The mixture was heated using a heating mantle or a constant-temperature water bath, maintaining a stable reaction temperature of 25 °C. 2 g of D001 resin was then added, along with 10 mL of a 2 mol / L NaOH solution. The mixture was reacted at room temperature with stirring for 30 min, followed by aging in a 100 °C oven for 24 h. The aged resin was filtered, washed with deionized water until neutral, and then baked at 60 °C for 10 h to obtain the modified nano-metal cation resin.

[0065] 962 μg of modified nano-metal cation exchange resin was packed into ion exchange column 1 (D=750, H=4000). A 2 mol / L hydroxylamine hydrochloride solution was prepared in a hydroxylamine hydrochloride preparation tank. Specifically, deionized water and solid hydroxylamine hydrochloride were added via pipeline and feed port, followed by mechanical stirring for 15 minutes to obtain the hydroxylamine hydrochloride solution. The prepared hydroxylamine hydrochloride solution was added to the ion exchange column via a hydroxylamine hydrochloride metering pump at a flow rate of 14 L / min, reaching a total addition volume of 700 L. After hydroxylamine was adsorbed by the exchange column, it was washed with 650 L of deionized water. Deionized water from the deionized water elevating tank was added to the ion exchange column via a metering pump at a flow rate of 8 L / min to wash away chloride ions. The washed hydrochloric acid was discharged via pipeline to a neutralization tank, neutralized with 42% NaOH, and then pumped out to the indoor drainage ditch. Finally, 1450 L of 2.5 mol / L nitric acid solution was added to the ion exchange column at a flow rate of 14 L / min, and 750 L of hydroxylamine nitrate solution was desorbed.

[0066] After testing and conversion of the hydroxylamine nitrate solution, the results showed that the conversion rate of hydroxylamine nitrate in this process was 93%.

[0067] Example 3

[0068] The difference from Example 1 is that the heating aging time in the preparation of the modified nano-metal cation resin was changed to 6 hours, while the rest is the same as in Example 1.

[0069] After testing and conversion of the hydroxylamine nitrate solution, the results showed that the conversion rate of hydroxylamine nitrate in this process was 80%.

[0070] Example 4

[0071] The difference from Example 1 is that in the process of preparing the modified nano-metal cation resin, the nano-metal oxide is Fe3O4, that is, the raw material Mn(NO3)2·4H2O is replaced with Fe(NO3)3. At the same time, the acidic cation resin is D301 resin, and the rest is the same as in Example 1.

[0072] After testing and conversion of the hydroxylamine nitrate solution, the results showed that the conversion rate of hydroxylamine nitrate in this process was 83%.

[0073] Example 5

[0074] The difference from Example 1 is that in the process of preparing the modified nano-metal cation resin, the nano-metal oxide is SnO2, that is, the raw material Mn(NO3)2·4H2O is replaced with Sn(NO3)2. At the same time, the acidic cation resin is selected as D201 resin, and the rest is the same as in Example 1.

[0075] After testing and conversion of the hydroxylamine nitrate solution, the results showed that the conversion rate of hydroxylamine nitrate in this process was 77%.

[0076] Example 6

[0077] The difference from Example 1 is that the reaction time under room temperature stirring conditions was changed to 60 min, and then it was placed in a 100°C constant temperature oven for heating and aging for 12 h. Otherwise, it was the same as Example 1.

[0078] After testing and conversion of the hydroxylamine nitrate solution, the results showed that the conversion rate of hydroxylamine nitrate in this process was 91%.

[0079] Example 7

[0080] The difference from Example 1 is that the resin after filtration, separation, heating and aging was washed with deionized water until neutral, and then baked at 80°C instead of 60°C. Otherwise, it is the same as Example 1.

[0081] After testing and conversion of the hydroxylamine nitrate solution, the results showed that the conversion rate of hydroxylamine nitrate in this process was 90%.

[0082] Example 8

[0083] The difference from Example 1 is that the resin after filtration, separation, heating and aging, washing with deionized water until neutral, and baking for 10 hours is changed to 12 hours. Otherwise, it is the same as Example 1.

[0084] After testing and conversion of the hydroxylamine nitrate solution, the results showed that the conversion rate of hydroxylamine nitrate in this process was 90%.

[0085] Comparative Example 1

[0086] The difference from Example 1 is that in this example, the acidic cation exchange resin is not modified, and D001 resin is directly used to fill the ion exchange column 1.

[0087] After testing and conversion of the hydroxylamine nitrate solution, the results showed that the conversion rate of hydroxylamine nitrate in this process was 76%.

[0088] Comparative Example 2

[0089] The difference from Example 4 is that in this example, the acidic cation exchange resin is not modified, and D301 resin is directly used to fill the ion exchange column 1.

[0090] After testing and conversion of the hydroxylamine nitrate solution, the results showed that the conversion rate of hydroxylamine nitrate in this process was 70%.

[0091] Comparative Example 3

[0092] The difference from Example 4 is that in this example, the acidic cation exchange resin is not modified, and D201 resin is directly used to fill the ion exchange column 1.

[0093] After testing and conversion of the hydroxylamine nitrate solution, the results showed that the conversion rate of hydroxylamine nitrate in this process was 66%.

[0094] Obviously, the above embodiments are merely illustrative examples for clear explanation and are not intended to limit the implementation. Those skilled in the art will recognize that other variations or modifications can be made based on the above description. It is neither necessary nor possible to exhaustively list all possible implementations here. However, obvious variations or modifications derived therefrom are still within the scope of protection of this invention.

Claims

1. A process for preparing hydroxylamine nitrate, characterized in that, Includes the following steps: Obtaining modified nano-metal cation resin: Nano-metal oxides are loaded onto acidic cation resin to form modified nano-metal cation resin; Preparation of hydroxylamine nitrate solution: Modified nano-metal cation exchange resin was filled into an ion exchange column to obtain hydroxylamine hydrochloride solution, which was then added to the ion exchange column. The modified nano-metal cation exchange resin adsorbed the hydroxylamine hydrochloride. The adsorbed chloride ions were removed by washing with water, and then the hydroxylamine in the modified nano-metal cation exchange resin was desorbed with nitric acid solution to obtain hydroxylamine nitrate solution. The nano-metal oxide includes at least one of MnO2, Fe3O4, SnO2, CeO2, and ZrO2.

2. The process according to claim 1, characterized in that, The process of loading the nano-metal oxide onto the acidic cation exchange resin is as follows: Resin pretreatment: Clean the acidic cation exchange resin by soaking it in a chloride ion solution, then rinse it with water again, and dry it for later use. Reaction: Obtain a metal salt, mix it with a solvent to obtain a metal salt solution, mix the pretreated acidic cation exchange resin with the metal salt solution, add an alkaline solution to carry out the reaction, and heat to age. The modified nano-metal cation resin was obtained by washing and drying.

3. The process according to claim 2, characterized in that, The concentration of the metal salt solution is 1.75 g / 100 mL; And / or, the solvent is an aqueous methanol solution or an aqueous ethanol solution; And / or, the molar ratio between hydroxide ions and metals in the alkaline solution is 1.4 or higher; The chloride-containing solution is a saturated NaCl solution or a hydrochloric acid solution.

4. The process according to claim 2, characterized in that, The reaction time is 30-60 minutes; And / or, the heating aging temperature is 100°C, and the heating aging time is 6-12 hours.

5. The process according to claim 2, characterized in that, In the washing step, deionized water is used for washing; And / or, the drying temperature is 60-80℃, and the drying time is 10-12h.

6. The process according to any one of claims 1-5, characterized in that, The acidic cation exchange resin includes an ion exchange resin containing at least one of the following groups: sulfonic acid group, carboxylic acid group, phosphoric acid group, and phenolic group. And / or, the concentration of the hydroxylamine hydrochloride solution is 2-2.5 mol / L; And / or, the concentration of the nitric acid solution is 2-2.5 mol / L.

7. The process according to any one of claims 1-5, characterized in that, The acidic cation exchange resin is of type D001, D201, D301 or D400.

8. A system for preparing hydroxylamine nitrate based on the process according to any one of claims 1-7, characterized in that, include: Ion exchange column (1), which is filled with modified nano-metal cation resin; Hydroxylamine hydrochloride preparation tank (2) is used to prepare hydroxylamine hydrochloride solution, and its outlet is connected to the inlet of ion exchange column (1) through hydroxylamine hydrochloride metering pump (7); The deionized water high-level tank (3) has its outlet connected to the inlet of the ion exchange column (1) for cleaning the ion exchange column (1); The nitric acid preparation tank (5) is used to prepare nitric acid solution, and its outlet is connected to the inlet of the ion exchange column (1) through the nitric acid metering pump (9); The neutralization tank (6) is connected to the outlet of the ion exchange column (1) and is used to hold the chloride ions removed by washing.

9. The system according to claim 8, characterized in that, The outer surface of the ion exchange column (1) is also provided with a jacket and a cooling water circulator (11) provided on the jacket. And / or, the nitric acid preparation tank (5) is also connected to a nitric acid metering tank (4) for holding analytical grade nitric acid. And / or, the ion exchange columns (1) are at least two sets.

10. The system according to claim 8 or 9, characterized in that, The deionized water high-level tank (3) is also equipped with a deionized water metering pump (8) at its outlet. The neutralization tank (6) is also equipped with an acid-base neutralization centrifugal pump (10) at its outlet.

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