A temperature-controllable rapid extraction device and process for ammonium dinitramide

Abstract

The present invention relates to a temperature-controlled rapid extraction device and process for ammonium dinitramide, comprising a plurality of cylinders connected sequentially from top to bottom, each of which is provided with a temperature-controlled jacket on the outside. The upper side of the uppermost cylinder is connected to a pressure control line, a sample supply line, and a water supply line. Filter assemblies are provided between adjacent cylinders. A flange hemisphere is connected to the lower side of the lowermost cylinder, and a filter assembly is also provided between the lowermost cylinder and the flange hemisphere. An output line with a liquid outlet valve is provided on the lower side of the flange hemisphere. Each cylinder is filled with activated carbon. The device of the present invention has a simple structure, is easy to install and disassemble, and is easy to scale up. The extraction and elution processes are carried out under temperature and pressure control conditions, and activated carbon of different particle sizes can be used for filling as needed. The overall operation is simple, efficient, and fast, making it particularly suitable for the industrial production of ammonium dinitramide.

Description

Technical Field

[0001] The invention relates to the technical field of ammonium dinitramide production, in particular to a temperature-controllable rapid extraction device and process for ammonium dinitramide. Background Art

[0002] Ammonium dinitramide (ADN) is a new high-energy oxidizer. Its molecule is halogen-free, its combustion products are clean and pollution-free, and its oxygen balance is high (+25.81%). Using ADN as a replacement for ammonium perchlorate can increase the specific impulse of propellants and reduce their signature. It can be used in both small surface-to-air missiles and boosters for intercontinental ballistic missiles, making it one of the most promising high-energy components in solid propellants. Furthermore, ADN, used in liquid monopropellants, offers advantages such as low toxicity, high energy content, and excellent safety, making it a promising alternative to the highly toxic hydrazine monopropellant.

[0003] At present, the synthesis of ammonium dinitramide mainly adopts the inorganic mixed acid method, which uses aminosulfonate as the starting raw material and fuming nitric acid and concentrated sulfuric acid as the nitrating reagents. It can be divided into an ion exchange process route and an adsorption extraction process route. The ion exchange process route refers to converting the nitration product dinitramide acid (HDN) into potassium dinitramide (KDN) or guanyl urea dinitramide (GUDN), and then obtaining ammonium dinitramide through an ion exchange reaction. The adsorption extraction process refers to the direct generation of ammonium dinitramide from the nitration product dinitramide acid (HDN) by ammoniation, and then separating it from the inorganic salt by-product by adsorption extraction. The ion exchange method is cumbersome to operate, has a low yield, and requires a large amount of organic solvents, resulting in high production costs; the chromatographic purification method has fewer process steps, a high yield of adsorption extraction operation, high product purity, low production costs, and is easy to achieve industrial production. The specific reaction for the synthesis of ammonium dinitramide is shown below:

[0004] NH2SO3K→mixed acid nitration→HN(NO2)2+NH3→NH4N(NO2)2+NH4NO3+(NH4)2SO4.

[0005] At present, the adsorption extraction of ammonium dinitramide generally uses activated carbon as an adsorbent, as described in the method disclosed in patent US5976483. In addition, related research has also been carried out in China (Liu Qian et al., Research on the Inorganic Synthesis and Separation and Purification of ADN, Energetic Materials, 2006(14), 5, 358-360; Liu Haizhou et al., Research on the Separation and Purification Process of ADN Synthesized by Mixed Acid Method, Chemical Propellants and Polymer Materials, 2009(7), 5, 47-49; Pan Yongfei et al., Separation and Purification of ADN by Activated Carbon Adsorption, Journal of Explosives and Propellants, 2017(40), 4, 61-65). However, these are all laboratory-level studies. Some studies believe that the activated carbon adsorption method has low separation efficiency and produces a large amount of salt-containing wastewater. For every kg of ammonium dinitramide produced, 500 kg of industrial wastewater will be generated. In addition, the process operation is time-consuming, requiring 2 to 3 working days (Pan Yongfei et al., Thermodynamic and Kinetic Study on the Adsorption of ADN by Resin DX, Journal of Explosives and Propellants, 2018(41), 4, 382-387). It is difficult to apply it to the industrial production of ammonium dinitramide. Summary of the Invention

[0006] The present invention aims to provide a temperature-controlled rapid extraction device and process for ammonium dinitramide. The device has a simple structure, is easy to install and disassemble, and is easy to scale up. The extraction and elution processes are carried out under temperature and pressure control conditions, and activated carbon of different particle sizes can be used for filling as needed. The overall operation is simple, efficient, and fast, and the device is suitable for the industrial production of ammonium dinitramide.

[0007] The object of the present invention is achieved through the following technical solutions:

[0008] A temperature-controllable rapid extraction device for ammonium dinitramide comprises a plurality of cylinders connected in sequence from top to bottom, wherein a temperature-control jacket is provided on the outside of each cylinder, a pressure control pipeline, a sample supply pipeline and a water supply pipeline are connected to the upper side of the uppermost cylinder, a filter assembly is provided between adjacent cylinders, a flange hemisphere is connected to the lower side of the lowermost cylinder, a filter assembly is provided between the lowermost cylinder and the flange hemisphere, an output pipeline with a liquid outlet valve is provided on the lower side of the flange hemisphere, and each cylinder is filled with activated carbon.

[0009] A sealing plate connecting flange is provided on the upper side of the uppermost cylinder and is connected to a sealing plate. Adjacent cylinders are fixedly connected through the cylinder connecting flange. The lowermost cylinder is installed on a support, and the support is provided with a support connecting flange. The lower side of the lowermost cylinder is fixedly connected to the support connecting flange, and the flange hemisphere is arranged in the support.

[0010] The pressure control pipeline, sample supply pipeline and water supply pipeline are installed on the sealing plate, and filter components are provided in the inner holes of adjacent cylinder connecting flanges and the inner holes of the lowermost cylinder connecting flange and the support connecting flange.

[0011] The filter assembly includes a screen and a porous filter plate, and the screen is arranged on the upper side of the porous filter plate.

[0012] The temperature control jacket is provided with a temperature control jacket medium inlet at the lower end and a temperature control jacket medium outlet at the upper end. In two adjacent temperature control jackets, the temperature control jacket medium inlets and the temperature control jacket medium outlets belonging to different temperature control jackets are connected through a pipeline with a connecting valve, and the temperature control jacket medium inlet of the lowermost temperature control jacket and the temperature control jacket medium outlet of the uppermost temperature control jacket are respectively connected to a temperature control device through a pipeline.

[0013] The sample supply pipeline and the water supply pipeline are both provided with a delivery pump and a flow meter, and the pressure control pipeline is provided with a safety control valve.

[0014] A process for the temperature-controlled rapid extraction device of ammonium dinitramide comprises the following steps:

[0015] Step 1, preparing an ammonium dinitramide saline solution;

[0016] Step 2: Assemble the flange hemisphere, pressure control pipe, sample supply pipe, water supply pipe and each cylinder to form an integral device column, and fill activated carbon into each cylinder during installation;

[0017] Step 3: Adjust the temperature and internal pressure of the column of the integrated device, input the saline solution of ammonium dinitramide prepared in step 1 into the column of the integrated device through the sample feeding pipeline, and input the extraction water into the column of the integrated device through the water supply pipeline for extraction;

[0018] Step 4: After the extraction operation is completed, the temperature and internal pressure of the entire device column are readjusted, and the elution water is input into the entire device column through the water supply pipeline for elution operation.

[0019] In step 2, activated carbon filling is performed in one of the following two ways:

[0020] Method 1: The whole device column is divided into two layers, the particle size of the upper layer of activated carbon is larger than that of the lower layer, and the two layers are the same height;

[0021] Method 2: The overall device column is divided into two layers, the particle size of the upper layer activated carbon is larger than that of the lower layer activated carbon, and the height of the upper layer is twice the height of the lower layer.

[0022] The particle size of the activated carbon filled in the column of the integral device is 40-140 meshes, wherein the particle size of the upper layer activated carbon is 80-140 meshes, and the particle size of the lower layer activated carbon is 40-80 meshes.

[0023] The temperature control range of the extraction operation of the column of the overall device is 0-10°C, the temperature control range of the elution operation is 30-50°C, and the pressure control range of the extraction operation and elution operation is 0-1.0kg.

[0024] The advantages and positive effects of the present invention are:

[0025] 1. The device of the present invention adopts a segmented design in which multiple cylinders are connected. The number of cylinders can be designed according to needs, which is convenient for installation and disassembly, as well as for loading and removing activated carbon, and is also easy to scale up the device.

[0026] 2. The present invention uses a variety of activated carbons of different particle sizes to fill the column of the overall device. The activated carbon with small particle size and strong adsorption is filled in the upper part of the column of the overall device, and the activated carbon with large particle size and weak adsorption is filled in the lower part of the column of the overall device. That is, the particle size of the activated carbon in the column of the overall device is arranged in a stepped manner, from small to large from top to bottom. Activated carbon with small particle size (large mesh number) has strong adsorption capacity, and the difference in its adsorption capacity for ammonium dinitramide and inorganic salts (relative to activated carbon with large particle size) becomes larger, which is beneficial for extraction; activated carbon with large particle size (small mesh number) has weaker adsorption capacity for ammonium dinitramide (relative to activated carbon with small adsorption capacity), which is beneficial for elution. This filling method takes into account both extraction and elution, is particularly beneficial for elution, and reduces the amount of elution water used.

[0027] 3. The device of the present invention can achieve temperature control through the temperature control jacket, and can achieve pressure control through the pressure control pipeline. Appropriately increasing the pressure and lowering the temperature of the device during the extraction operation can accelerate the extraction process, enhance the extraction and separation effect, reduce the amount of extraction solvent used, reduce the amount of salt-containing wastewater generated, and significantly shorten the extraction process operation time; appropriately increasing the pressure and raising the temperature of the device during the elution operation can weaken adsorption, accelerate the elution process, reduce the amount of elution water used, and significantly shorten the elution process operation time.

[0028] 4. The extraction and elution operations of the present invention can achieve satisfactory results using only room temperature water, without the need for cold water extraction and hot water elution, thus simplifying the process operation. BRIEF DESCRIPTION OF THE DRAWINGS

[0029] Figure 1 Schematic diagram of the structure of the device of the present invention.

[0030] Among them, 1 is the pressure control pipeline; 2 is the sample feeding pipeline; 3 is the water supply pipeline; 4 is the medium outlet of the temperature control jacket; 5 is the sealing plate connecting flange; 6 is the temperature control jacket; 7 is the medium inlet of the temperature control jacket; 8 is the cylinder; 9 is the cylinder connecting flange; 10 is the screen; 11 is the porous filter plate; 12 is the support connecting flange; 13 is the support; 14 is the liquid outlet valve, and 15 is the flange hemisphere. DETAILED DESCRIPTION

[0031] The present invention will be further described below in conjunction with the accompanying drawings.

[0032] like Figure 1 As shown, the device of the present invention includes a plurality of cylinders 8 connected in sequence from top to bottom, and a temperature control jacket 6 is provided on the outside of each cylinder 8. The upper side of the uppermost cylinder 8 is connected to a pressure control pipeline 1, a sample supply pipeline 2 and a water supply pipeline 3. A filter assembly is provided between adjacent cylinders 8. The lower side of the lowermost cylinder 8 is connected to a flange hemisphere 15, and a filter assembly is also provided between the lowermost cylinder 8 and the flange hemisphere 15. An output pipeline with a liquid outlet valve 14 is provided on the lower side of the flange hemisphere 15, and each cylinder 8 is filled with activated carbon.

[0033] like Figure 1 As shown, a sealing plate connecting flange 5 is provided on the upper side of the uppermost cylinder 8 and is connected to a sealing plate, and the pressure control pipeline 1, the sample loading pipeline 2 and the water supply pipeline 3 are installed on the sealing plate, and a sealing gasket and other structures can be arranged between the sealing plate connecting flange 5 and the sealing plate to ensure the sealing of the upper end of the entire device, and the adjacent cylinders 8 are fixedly connected through the cylinder connecting flange 9, and the filter assembly is provided in the inner hole of the cylinder connecting flange 9, and a sealing gasket and other structures can be arranged between the adjacent cylinder connecting flanges 9 to ensure the sealing of the device, the lowermost cylinder 8 is installed on a support 13, and a support connecting flange 12 is provided on the support 13, the lower side cylinder connecting flange 9 of the lowermost cylinder 8 is fixedly connected to the support connecting flange 12, the flange hemisphere 15 is provided in the support 13, and the inner holes of the lowermost cylinder connecting flange 9 and the support connecting flange 12 are also provided with a filter assembly, and a sealing gasket and other structures can be arranged between the lowermost cylinder connecting flange 9 and the support connecting flange 12 to ensure the sealing of the device.

[0034] like Figure 1 As shown, the filter assembly includes a screen 10 and a porous filter plate 11, and the screen 10 is arranged on the upper side of the porous filter plate 11. The function of the porous filter plate 11 is to provide physical support. Under the premise of ensuring physical support, some holes (about 5 mm in diameter) are distributed on the porous filter plate 11 for the passage of chromatography liquid and eluent. The function of the screen 10 is to intercept the activated carbon to ensure that the activated carbon in each cylinder 8 will not fall into the next layer, and to ensure the passage of chromatography liquid and eluent.

[0035] like Figure 1As shown, the temperature control jacket 6 is provided with a temperature control jacket medium inlet 7 at the lower end and a temperature control jacket medium outlet 4 at the upper end, wherein the temperature control medium (water or gas, etc.) enters the cavity inside the temperature control jacket 6 from the temperature control jacket medium inlet 7 and exchanges heat with the cylinder 8 to achieve temperature control, and then is output from the temperature control jacket medium outlet 4. Each temperature control jacket 6 can adopt a series mode, and in two adjacent temperature control jackets 6, the temperature control jacket medium inlet 7 and the temperature control jacket medium outlet 4 belonging to different temperature control jackets 6 are connected by a pipeline with a connecting valve, and the temperature control jacket medium inlet 7 of the lowermost temperature control jacket 6 and the temperature control jacket medium outlet 4 of the uppermost temperature control jacket 6 are respectively connected to a temperature control device through a pipeline to achieve temperature regulation of the temperature control medium. The cylinder 8 can be provided with a temperature sensor or other components as needed to monitor the temperature inside the cylinder in real time and feed back to the temperature control device for timely adjustment. The temperature control device and temperature sensor are well known in the art and are commercially available products. The extraction operation temperature control range of the process of the present invention is 0-10 DEG C, and the elution operation temperature control range is 30-50 DEG C.

[0036] like Figure 1 As shown, the upper side of the uppermost cylinder 8 is connected to a pressure control line 1, a sample line 2, and a water line 3, wherein the sample line 2 is used to add an aqueous solution containing inorganic salt ammonium dinitramide to be extracted into the device, and the water line 3 is used to add extraction water or elution water into the device. The pressure control line 1 is used to control the pressure in the device during the extraction and elution operations. The sample line 2 and the water line 3 are both equipped with a delivery pump and a flow meter to control the flow rate. The pressure control line 1 is provided with a safety control valve. When the installation control valve is opened, the pressure control line 1 can be exhausted or inflated to adjust the pressure. In addition, a pressure sensor can be provided in each cylinder 8 as needed to monitor the pressure in the cylinder 8 in real time and feedback to the device system to control the opening or closing of the safety control valve to achieve pressure regulation. The pressure control range of the extraction and elution operation process of the present invention is 0-1.0 kg. The flow meter, safety control valve, and pressure sensor are all commercially available products.

[0037] The working principle of the present invention is:

[0038] The preparation of the ammonium dinitramide saline solution of the present invention is as follows:

[0039] Prepare a mixed acid solution with 20.0 kg of fuming nitric acid and 6.1 kg of concentrated sulfuric acid, then cool to below -40°C. Add 4.2 kg of potassium sulfamate in batches to the mixed acid. Once all of the solution has been added, continue the reaction at -40°C for half an hour. Slowly pour the nitration reaction solution into a mixture of 18 kg of crushed ice and 2 kg of water, then neutralize and dilute the solution with ammonia until the solution is neutral or slightly alkaline.

[0040] The device of the present invention is constructed as follows:

[0041] First, install the flange hemisphere 15 on the support 13, then place the porous sieve plate 11 and the screen 10 on the support connecting flange 12, and then install the cylinder 8. After each cylinder 8 is installed, fill the cylinder 8 with activated carbon, and then place the porous sieve plate 11 and the screen 10 on the upper end of the cylinder 8 until all cylinders 8 are installed. Then install the sealing plate on the upper side of the uppermost cylinder 8 and install the sample pipeline 2, the water pipeline 3 and the pressure control pipeline 1. The temperature control jackets 6 on the outside of each cylinder 8 are connected in series in sequence through pipelines with connecting valves, and the temperature control jacket medium inlet 7 of the lowermost temperature control jacket 6 and the temperature control jacket medium outlet 4 of the uppermost temperature control jacket 6 are respectively connected to a temperature control device through pipelines, so that the temperature control device and the inside of each temperature control jacket 6 form a closed loop, and the heat exchange medium is driven to flow by a circulating pump arranged on the closed loop to achieve the purpose of controlling the temperature of the device.

[0042] During the construction of the above device, activated carbon filling can be carried out in two ways:

[0043] Method 1: The whole device column is divided into two layers, the upper layer of activated carbon is 120 mesh, and the lower layer of activated carbon is 40 mesh. The height of the two layers is the same, both 60 cm;

[0044] Method 2: The overall device column is divided into two layers, the upper layer activated carbon is 120 mesh, the lower layer activated carbon is 40 mesh, the upper layer height is twice the lower layer height, that is, the upper layer is 80 cm and the lower layer is 40 cm.

[0045] The mesh size of the sieve 10 in the filter assembly is set according to the specific filling method, and it is only necessary to ensure that the activated carbon in each cylinder 8 does not fall into the next layer.

[0046] Several examples and comparative examples are listed below to further illustrate the present invention.

[0047] Example 1

[0048] The column of the integrated device was loaded using method 1. A saline solution containing 2.7 kg of ammonium dinitramide was added to the column of the integrated device, pressurized to 0.5 kg, and the temperature was controlled at 5°C. After complete adsorption, room temperature water was added to start the extraction operation. The extract was detected by ultraviolet spectroscopy until the ultraviolet absorption peaks of the inorganic salts (ammonium sulfate and ammonium nitrate) disappeared. A total of 165 kg of saline wastewater was collected. The pressure was increased to 0.8 kg, the temperature was controlled at 40°C, room temperature water was added, and the eluent was detected by ultraviolet spectroscopy. Elution was terminated when the concentration of ammonium dinitramide in the eluent was less than 0.05%. A total of 270 liters of eluent was collected. After concentration, the product purity was determined by ion chromatography to be 99.7%, with a yield of 98.2%. The entire operation took approximately 7 hours.

[0049] Example 2

[0050] The column of the integrated device was loaded using method 2. A saline solution containing 2.7 kg of ammonium dinitramide was added to the column of the integrated device, pressurized to 0.6 kg, and the temperature was controlled at 5°C. After complete adsorption, room temperature water was added and the extraction operation began. The extract was detected by ultraviolet spectroscopy until the ultraviolet absorption peaks of the inorganic salts (ammonium sulfate and ammonium nitrate) disappeared. A total of 155 kg of saline wastewater was collected. The pressure was increased to 1.0 kg, the temperature was controlled at 50°C, room temperature water was added, and the eluent was detected by ultraviolet spectroscopy. Elution was terminated when the concentration of ammonium dinitramide in the eluent was less than 0.05%. A total of 240 liters of eluent was collected. After concentration, the product purity was determined by ion chromatography to be 99.8%, with a yield of 98.9%. The entire operation took approximately 6 hours.

[0051] Example 3

[0052] The column of the integrated device was loaded using method 1. A saline solution containing 2.4 kg of ammonium dinitramide was added to the column of the integrated device, pressurized to 0.8 kg, and the temperature was controlled at 10°C. After complete adsorption, room temperature water was added to start the extraction operation. The extract was detected by ultraviolet spectroscopy until the ultraviolet absorption peaks of the inorganic salts (ammonium sulfate and ammonium nitrate) disappeared. A total of 137 kg of saline wastewater was collected. The pressure was increased to 0.6 kg, the temperature was controlled at 30°C, room temperature water was added, and the eluent was detected by ultraviolet spectroscopy. Elution was terminated when the concentration of ammonium dinitramide in the eluent was less than 0.05%. A total of 190 liters of eluent was collected. After concentration, the product purity was determined by ion chromatography to be 99.6% and the yield was 97.3%. The entire operation took approximately 8 hours.

[0053] Example 4

[0054] The column of the overall device is filled using method 2. A saline solution containing 2.9 kg of ammonium dinitramide is added to the column of the overall device, pressurized to 0.3 kg, and the temperature is controlled at 1°C. After complete adsorption, room temperature water is added and the extraction operation begins. The extract is detected by ultraviolet spectroscopy until the ultraviolet absorption peaks of the inorganic salts (ammonium sulfate and ammonium nitrate) disappear. A total of 190 kg of saline wastewater is collected. The pressure is increased to 0.4 kg, the temperature is controlled at 50°C, room temperature water is added, and the eluent is detected by ultraviolet spectroscopy. Elution is terminated when the concentration of ammonium dinitramide in the eluent is less than 0.05%. A total of 310 liters of eluent are collected. After concentration, the product purity is determined by ion chromatography to be 99.5%, with a yield of 98.2%. The entire operation takes about 12 hours.

[0055] Comparative Example 1

[0056] The column of the integrated device was loaded using method 1. A saline solution containing 2.4 kg of ammonium dinitramide was added to the column without pressurization or temperature control. After complete adsorption, room temperature water (approximately 20°C) was added to begin the extraction process. The extract was monitored by ultraviolet spectroscopy until the UV absorption peaks of the inorganic salts (ammonium sulfate and ammonium nitrate) disappeared. A total of 152 kg of saline wastewater was collected. Room temperature water (approximately 20°C) was added, and the eluate was monitored by ultraviolet spectroscopy. Elution was terminated when the concentration of ammonium dinitramide in the eluate was less than 0.05%. A total of 330 liters of eluate was collected. After concentration, the product purity was determined by ion chromatography to be 99.4%, with a yield of 96.1%. The entire process took approximately 22 hours.

[0057] Comparative Example 2

[0058] The entire column of the device is filled with 120-mesh activated carbon. A saline solution containing 2.7 kg of ammonium dinitramide is added to the column of the device, pressurized to 0.3 kg, and the temperature is controlled at 1°C. After complete adsorption, room temperature water is added and the extraction operation begins. The extract is detected by ultraviolet spectroscopy until the ultraviolet absorption peaks of the inorganic salts (ammonium sulfate and ammonium nitrate) disappear. A total of 210 kg of saline wastewater is collected. The pressure is increased to 0.4 kg, the temperature is controlled at 50°C, room temperature water is added, and the eluent is detected by ultraviolet spectroscopy. Elution is terminated when the concentration of ammonium dinitramide in the eluent is less than 0.05%. A total of 340 liters of eluent are collected. After concentration, the product purity is determined by ion chromatography to be 99.7%, with a yield of 97.9%. The entire operation takes approximately 15 hours.

Claims

1. A temperature-controlled rapid extraction device for ammonium dinitramide, characterized in that: The invention comprises a plurality of cylinders (8) connected in sequence from top to bottom, and a temperature control jacket (6) is provided on the outside of each cylinder (8), a pressure control pipeline (1), a sample supply pipeline (2) and a water supply pipeline (3) are connected to the upper side of the uppermost cylinder (8), a filter assembly is provided between adjacent cylinders (8), a flange hemisphere (15) is connected to the lower side of the lowermost cylinder (8), and a filter assembly is provided between the lowermost cylinder (8) and the flange hemisphere (15), an output pipeline with a liquid outlet valve (14) is provided on the lower side of the flange hemisphere (15), and each cylinder (8) is filled with activated carbon; The upper side of the uppermost cylinder (8) is provided with a sealing plate connecting flange (5) connected to a sealing plate, and adjacent cylinders (8) are fixedly connected via cylinder connecting flanges (9). The lowermost cylinder (8) is mounted on a support (13), and the support (13) is provided with a support connecting flange (12). The lower side cylinder connecting flange (9) of the lowermost cylinder (8) is fixedly connected to the support connecting flange (12), and the flange hemisphere (15) is provided in the support (13); The pressure control pipeline (1), the sample supply pipeline (2) and the water supply pipeline (3) are installed on the sealing plate, and the inner holes of the adjacent cylinder connection flanges (9) and the inner holes of the lowermost cylinder connection flange (9) and the support connection flange (12) are all provided with filter components; The filter assembly comprises a screen (10) and a porous filter plate (11), and the screen (10) is arranged on the upper side of the porous filter plate (11); The temperature control jacket (6) is provided with a temperature control jacket medium inlet (7) at the lower end and a temperature control jacket medium outlet (4) at the upper end. In two adjacent temperature control jackets (6), the temperature control jacket medium inlets (7) and the temperature control jacket medium outlets (4) belonging to different temperature control jackets (6) are connected via a pipeline with a connecting valve. The temperature control jacket medium inlet (7) of the lowermost temperature control jacket (6) and the temperature control jacket medium outlet (4) of the uppermost temperature control jacket (6) are respectively connected to a temperature control device via a pipeline. The flange hemisphere (15), the pressure control line (1), the sample line (2), the water line (3) and the cylinders (8) are assembled to form an integral device column. During installation, activated carbon is filled into each cylinder (8). The activated carbon filling is performed in one of the following two ways: Method 1: The whole device column is divided into two layers, the particle size of the upper layer of activated carbon is smaller than that of the lower layer, and the two layers are the same height; Method 2: The overall device column is divided into two layers, the particle size of the upper layer activated carbon is smaller than that of the lower layer activated carbon, and the height of the upper layer is twice the height of the lower layer.

2. The temperature-controlled rapid extraction device for ammonium dinitramide according to claim 1, wherein: The sample supply pipeline (2) and the water supply pipeline (3) are both provided with a delivery pump and a flow meter, and the pressure control pipeline (1) is provided with a safety control valve.

3. A process for the temperature-controlled rapid extraction device of ammonium dinitramide according to claim 1, characterized in that: The steps include: Step 1, preparing an ammonium dinitramide saline solution; Step 2: Assemble the flange hemisphere (15), the pressure control pipeline (1), the sample supply pipeline (2), the water supply pipeline (3) and each cylinder (8) to form an integral device column, and fill activated carbon into each cylinder (8) during installation; Step 3: Adjust the temperature and internal pressure of the column of the whole device, input the saline solution of ammonium dinitramide prepared in step 1 into the column of the whole device through the sample feeding pipe (2), and input the extraction water into the column of the whole device through the water feeding pipe (3) to perform the extraction operation; Step 4: After the extraction operation is completed, the temperature and internal pressure of the entire device column are readjusted, and the elution water is input into the entire device column through the water supply pipe (3) for elution operation.

4. The process of the temperature-controlled rapid extraction device of ammonium dinitramide according to claim 3, wherein: In step 2, activated carbon filling is performed in one of the following two ways: Method 1: The whole device column is divided into two layers, the particle size of the upper layer of activated carbon is smaller than that of the lower layer, and the two layers are the same height; Method 2: The overall device column is divided into two layers, the particle size of the upper layer activated carbon is smaller than that of the lower layer activated carbon, and the height of the upper layer is twice the height of the lower layer.

5. The process of the temperature-controlled rapid extraction device of ammonium dinitramide according to claim 4, characterized in that: The particle size of the activated carbon filled in the column of the integral device is 40-140 meshes, wherein the particle size of the upper layer activated carbon is 80-140 meshes, and the particle size of the lower layer activated carbon is 40-80 meshes.

6. The process of the temperature-controlled rapid extraction device of ammonium dinitramide according to claim 3, characterized in that: The temperature control range of the extraction operation of the column of the overall device is 0-10°C, the temperature control range of the elution operation is 30-50°C, and the pressure control range of the extraction operation and elution operation is 0-1.0kg.

Images