Extraction and recovery device and method for ammonium perchlorate in retired hydroxyl-terminated polybutadiene propellant

Through the combination of devices and methods, the efficient extraction and recycling of ammonium perchlorate in the decommissioned butyl hydroxy propellant is achieved, and the problems of environmental protection and resource waste are solved. The extraction rate is high and the extract can be recycled.

CN120479004APending Publication Date: 2025-08-15XIAN MODERN CHEM RES INST
View PDF 5 Cites 0 Cited by

Patent Information

Application Number
CN202510506584.8
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-04-22
Publication Date
2025-08-15

AI Technical Summary

Technical Problem

The treatment method of decommissioned hydroxypropants in the prior art leads to environmental pollution and waste of resources, and the recycling and reuse of ammonium perchlorate is difficult to achieve engineering.

Method used

The device consisting of a wet crusher, extraction kettle, disc filter, washing water storage tank, crystallization kettle and crystallization liquid filter is used to achieve the extraction and recovery of ammonium perchlorate through the steps of pulverization, extraction, and crystallization.

Benefits of technology

It realizes efficient extraction and recycling of ammonium perchlorate, solves environmental protection problems and resource waste, the extraction rate reaches more than 90%, and the extract can be recycled.

✦ Generated by Eureka AI based on patent content.

Smart Images

  • Figure CN120479004A_ABST
    Figure CN120479004A_ABST
Patent Text Reader

Abstract

The invention provides a device and a method for extracting and recovering ammonium perchlorate in a retired hydroxyl-terminated polybutadiene propellant, the device comprises a wet pulverizer, the discharge port of the wet pulverizer is connected with the feed port of an extraction kettle, and the discharge port of the extraction kettle is connected with the feed port of a disc filter through an extracted mixture metering pump. And a washing water outlet of the washing water storage tank is connected with a disc filter washing water inlet of the disc filter through a washing water metering pump. A disc filter filtrate outlet of the disc filter is connected with a liquid inlet of the extracted filtrate receiving tank, a liquid outlet of the extracted filtrate receiving tank is connected with a feeding hole of the crystallization kettle through the extracting solution metering pump, and a discharging hole of the crystallization kettle is connected with a feeding hole of the crystallization solution filter. The device provided by the invention solves the problems of environmental protection and resource waste caused by direct destruction of the solid decommissioned hydroxyl-terminated polybutadiene propellant at present, and provides a solution thought for recycling of components of the solid decommissioned hydroxyl-terminated polybutadiene propellant.
Need to check novelty before this filing date? Find Prior Art

Description

Technical Field

[0001] The invention belongs to the technical field of explosives and propellants, relates to retired HTPB propellants, and particularly relates to a device and method for extracting and recovering ammonium perchlorate in retired HTPB propellants. Background Art

[0002] At present, a large number of engines loaded with solid HTPB propellant are scrapped every year. The current mainstream treatment process is burning or blasting. If these treatment methods are adopted, waste gas (NO x , HCl, HCN, NH3 and Cl2) and solid waste residues. Pollutants spread with the atmosphere and water and pollute the environment. At the same time, burning the discarded solid retired HTPB propellant by incineration wastes potential energy and resources. Taking the destruction of 1,000 tons of conventional solid propellant as an example, open-air incineration will produce about 310 tons of solid dust and 900 tons of waste gas, including 202 tons of HCl gas, 270 tons of nitrogen oxide gas (based on NO2), and 428 tons of CO2 gas. Assuming that acid rain with a pH of 5.6 is formed, the total waste gas volume will reach 8.42×10 5 Ten thousand tons.

[0003] To improve the environmental, economic, and safety of decommissioned engine processing, it is necessary to extract, separate, and recover energetic components from solid propellants, specifically solid decommissioned HTPB propellants (HTPBs). Ammonium perchlorate is the primary energetic component in solid decommissioned HTPBs, accounting for over 50%, making its extraction and recovery crucial. Previous research has reported methods for extracting energetic components from spent ammunition, but these studies have primarily focused on laboratory-based process development, with limited research focused on scaling up ammonium perchlorate recovery processes from solid decommissioned HTPBs or developing engineering-based approaches. Summary of the Invention

[0004] In view of the shortcomings of the existing technology, the purpose of the present invention is to provide an extraction and recovery device and method for ammonium perchlorate in retired HTPB propellant, so as to solve the technical problem in the existing technology that it is difficult to achieve both the recovery and reuse of ammonium perchlorate in retired HTPB propellant and the engineering of the extraction and recovery of ammonium perchlorate in retired HTPB propellant.

[0005] In order to solve the above technical problems, the present invention adopts the following technical solutions:

[0006] A device for extracting and recovering ammonium perchlorate from retired HTPB propellant comprises a wet grinder, wherein the discharge port of the wet grinder is connected to the feed port of an extraction kettle, and the discharge port of the extraction kettle is connected to the feed port of a disc filter via an extraction mixture metering pump.

[0007] It also includes a washing water storage tank, and the washing water outlet of the washing water storage tank is connected to the disc filter washing water inlet of the disc filter through a washing water metering pump.

[0008] The filtrate outlet of the disc filter is connected to the liquid inlet of the extraction filtrate receiving tank, the liquid outlet of the extraction filtrate receiving tank is connected to the feed port of the crystallization kettle through the extraction liquid metering pump, and the discharge port of the crystallization kettle is connected to the feed port of the crystallization liquid filter.

[0009] The present invention also protects a method for extracting and recovering ammonium perchlorate from retired HTPB propellant, which is implemented using the above-mentioned device for extracting and recovering ammonium perchlorate from retired HTPB propellant.

[0010] Compared with the prior art, the present invention has the following technical effects:

[0011] (I) The device of the present invention uses solid retired HTPB propellant as the object, and uses an engineering approach to extract and recover ammonium perchlorate from solid retired HTPB propellant through crushing, extraction and crystallization, thereby solving the environmental problems and resource waste caused by the current direct destruction of solid retired HTPB propellant, and providing a solution for the recovery and reuse of components of solid retired HTPB propellant.

[0012] (II) The method of the present invention monitors the concentration of ammonium perchlorate in the extract by measuring the conductivity of the filtered liquid in the extract filtrate receiving tank, thereby enabling the recycling of the filtered liquid in the extract filtrate receiving tank, i.e., the extract.

[0013] (III) The method of the present invention can achieve an ammonium perchlorate extraction rate of more than 90% by controlling the pulverization particle size of the solid retired HTPB propellant in the wet pulverizer, and the extraction effect is relatively good.

[0014] (IV) The method of the present invention controls the extraction time of ammonium perchlorate in the extraction kettle to be greater than or equal to 25 minutes, thereby improving the extraction rate of ammonium perchlorate. BRIEF DESCRIPTION OF THE DRAWINGS

[0015] Figure 1 Schematic diagram of the overall structure of the device in the present invention.

[0016] The meanings of the various numbers in the figure are: 1-wet crusher, 2-extraction kettle, 3-extraction mixture metering pump, 4-disc filter, 5-washing water storage tank, 6-washing water metering pump, 7-extraction filtrate receiving tank, 8-extraction liquid metering pump, 9-crystallization kettle, 10-crystallization liquid filter, 11-crystallization filtrate receiving tank, 12-vacuum pump, 13-heating machine, 14-refrigeration machine, 15-propellant feeder, 16-tap water high-level tank, 17-pipeline, 18-valve, 19-circulation pump.

[0017] 401-disc filter feed port, 402-disc filter wash water inlet, 403-disc filter filtrate outlet.

[0018] The specific contents of the present invention are further described in detail below with reference to the accompanying drawings and embodiments. DETAILED DESCRIPTION

[0019] It should be noted that, unless otherwise specified, all equipment, instruments and components in the present invention are equipment, instruments and components known in the prior art. For example, the wet grinder adopts the known wet grinder, the heater adopts the known heater, and the flow meter adopts the known flow meter.

[0020] The various devices in the present invention are mainly connected through pipelines 17. Each pipeline 17 is provided with a valve 18 and a circulation pump 19 as needed, and is opened or closed according to process requirements.

[0021] In the present invention, the solid retired HTPB propellant refers to the solid HTPB propellant loaded in retired and scrapped engines.

[0022] In accordance with the above technical solution, specific embodiments of the present invention are given below. It should be noted that the present invention is not limited to the following specific embodiments, and all equivalent changes made on the basis of the technical solution of this application fall within the protection scope of the present invention.

[0023] Example 1:

[0024] This embodiment provides a device for extracting and recovering ammonium perchlorate from retired HTPB propellant. Figure 1 As shown, it includes a wet grinder 1, the discharge port of the wet grinder 1 is connected to the feed port of the extraction kettle 2, and the discharge port of the extraction kettle 2 is connected to the disc filter feed port 401 of the disc filter 4 through the extraction mixture metering pump 3.

[0025] like Figure 1 As shown, a washing water storage tank 5 is further included, and a washing water outlet of the washing water storage tank 5 is connected to the disc filter washing water inlet 402 of the disc filter 4 through a washing water metering pump 6 .

[0026] like Figure 1 As shown, the disc filter filtrate outlet 403 of the disc filter 4 is connected to the liquid inlet of the extraction filtrate receiving tank 7, the liquid outlet of the extraction filtrate receiving tank 7 is connected to the feed port of the crystallization kettle 9 through the extraction liquid metering pump 8, and the discharge port of the crystallization kettle 9 is connected to the feed port of the crystallization liquid filter 10.

[0027] In this embodiment, the wet pulverizer 1 pumps the pulverized solid-liquid mixture into the extraction kettle 2 .

[0028] In this embodiment, the extraction kettle 2 is made of stainless steel.

[0029] In this embodiment, the filter cake filtered by the disc filter 4 is collected in a solid residue box for standby use.

[0030] As a preferred method of this embodiment, Figure 1 As shown, the filtrate outlet of the crystallization liquid filter 10 is also connected to the liquid inlet of the crystallization filtrate receiving tank 11.

[0031] In this embodiment, the filter cake outlet of the crystallization liquid filter 10 is the recovered ammonium perchlorate, which is placed in an explosion-proof vacuum oven for standby use.

[0032] In this embodiment, ammonium perchlorate is obtained by cooling crystallization.

[0033] As a preferred method of this embodiment, Figure 1 As shown, the vacuum port of the crystallization filtrate receiving tank 11 is connected to the exhaust port of the vacuum pump 12.

[0034] like Figure 1 As shown, the vacuum port of the extraction filtrate receiving tank 7 is also connected to the exhaust port of the vacuum pump 12.

[0035] As a preferred method of this embodiment, Figure 1 As shown, the hot water inlet of the jacket of the extraction kettle 2 is connected to the liquid outlet of the heater 13 .

[0036] like Figure 1 As shown, the hot water outlet of the jacket of the extraction kettle 2 is connected to the liquid return port of the heater 13.

[0037] As a preferred method of this embodiment, Figure 1 As shown, the cold water inlet of the jacket of the crystallization kettle 9 is connected to the liquid outlet of the refrigerator 14.

[0038] like Figure 1 As shown, the jacket cold water outlet of the crystallization kettle 9 is connected to the liquid return port of the refrigerator 14.

[0039] As a preferred method of this embodiment, Figure 1 As shown, the jacket cold water inlet of the wet pulverizer 1 is connected to the liquid outlet of the refrigerator 14 ; the jacket cold water outlet of the wet pulverizer 1 is connected to the liquid return port of the refrigerator 14 .

[0040] like Figure 1 As shown, a propellant feeder 15 is further provided above the wet pulverizer 1 ; the discharge port of the propellant feeder 15 is connected to the feed port of the wet pulverizer 1 .

[0041] like Figure 1As shown, a tap water high level tank 16 is further provided above the wet pulverizer 1 ; the water outlet of the tap water high level tank 16 is connected to the water inlet of the wet pulverizer 1 .

[0042] In this embodiment, the wet pulverizer 1 can also perform internal circulation, and the wet pulverizer 1 adopts a commonly used wet pulverizer 1 known in the art.

[0043] As a preferred method of this embodiment, Figure 1 As shown, the liquid outlet of the extraction filtrate receiving tank 7 can also be connected to the water inlet of the tap water high-level tank 16 through the extraction liquid metering pump 8.

[0044] In this embodiment, the water inlet of the tap water high level tank 16 can also be connected to an external tap water pipe to provide a tap water source, and the external tap water pipe adopts a known and commonly used external tap water pipe.

[0045] Example 2:

[0046] This embodiment provides a method for extracting and recovering ammonium perchlorate from retired HTPB propellant. The method is implemented using the apparatus for extracting and recovering ammonium perchlorate from retired HTPB propellant in Example 1. The method specifically comprises the following steps:

[0047] Step 1: Open the valve of the water outlet of the tap water high-level tank 16, measure the tap water through the flow meter, and add it into the wet grinder 1 through multi-point feeding; start the propellant feeder 15, add the solid retired hydroxybutane propellant in the propellant feeder 15 into the wet grinder 1 and grind it. During the grinding process, the solid-liquid ratio is maintained at 1: (6 to 8).

[0048] In step 2, while the solid retired HTPB propellant is being crushed, the refrigerator 14 is started, and the valve of the cold water inlet of the jacket of the wet grinder 1 is opened to maintain the material temperature at 25±2°C during the crushing process of the solid retired HTPB propellant; the solid-liquid mixture obtained after the solid retired HTPB propellant is crushed is transported from the discharge port of the wet grinder 1 to the feed port of the extraction kettle 2.

[0049] Step 3: After the solid-liquid mixture is added, the valve of the hot water inlet of the jacket of the extraction kettle 2 is opened, and the heater 13 is started to ensure the material temperature during the extraction process, and the extraction time is ≥25 min and the stirring speed is ≥200 rpm.

[0050] Step 4: Open the valve of the discharge port of the extraction kettle 2, start the extraction mixture metering pump 3, and continuously add the extracted mixture to the disc filter 4. The disc filter 4 is in a continuous filtration mode, and the relationship between the feeding rate of the extracted mixture and the filtration rate of the disc filter 4 is 1: (1 to 1.5).

[0051] Step 5: Start the washing water metering pump 6 while filtering, and deliver the tap water in the washing water storage tank 5 to the rinsing area of the disc filter 4. The ratio of the rinsing water volume to the total amount of filtered material is 1:(3-5). After the filtration is completed, the filtered liquid enters the extraction filtrate receiving tank 7 for temporary storage, and the filter cake enters the solid residue box.

[0052] Step six, the conductivity of the liquid filtered in the extraction filtrate receiving tank 7 is detected by conductivity. If the conductivity of the liquid filtered in the extraction filtrate receiving tank 7 is less than the set value, when the next batch of solid retired HTPB propellant is crushed in the wet grinder 1, the extraction liquid metering pump 8 is started, and the filtered liquid in the extraction filtrate receiving tank 7 is returned to the tap water high-level tank 16 through the extraction liquid metering pump 8, and the filtered liquid in the extraction filtrate receiving tank 7 is used as a cooling medium to recycle the filtered liquid.

[0053] After being recycled many times, when the conductivity of the liquid filtered in the extraction filtrate receiving tank 7 is greater than or equal to the set value, the pipeline valve of the extraction liquid metering pump 8 is switched, and the liquid filtered in the extraction filtrate receiving tank 7 is added to the crystallization kettle 9 through the extraction liquid metering pump 8 for crystallization treatment.

[0054] Step seven, after all the liquid filtered in the extract filtrate receiving tank 7 is added to the crystallization kettle 9, the crystallization kettle 9 is started and stirred, the valve of the jacket cold water inlet of the crystallization kettle 9 is opened, and the temperature of the material in the crystallization kettle 9 is slowly reduced. The cooling rate range is 1 to 2 ° C / min, and the stirring speed is ≥ 200 rpm; after continuing to keep warm and stir for 30 minutes, the valve of the discharge port of the crystallization kettle 9 is opened to transport the crystallized material to the crystallization liquid filter 10.

[0055] Step eight, after all the crystallized materials are transported to the crystallization liquid filter 10, the valve of the vacuum port of the crystallization filtrate receiving tank 11 is opened to vacuumize, so that the vacuum degree in the crystallization filtrate receiving tank 11 is ≤

[0056] -0.09MPa, the crystallization mother liquor is pumped into the crystallization filtrate receiving tank 11; after all the crystallization mother liquor enters the crystallization filtrate receiving tank 11, the valve of the vacuum port of the crystallization filtrate receiving tank 11 is closed; the vacuum pump 12, the heater 13 and the refrigerator 14 are turned off, and the filter cake in the crystallization liquid filter 10 is the recovered ammonium perchlorate.

[0057] Step nine: collect the filter cake in the crystallization liquid filter 10 and place it in an explosion-proof vacuum oven. Control the temperature in the explosion-proof vacuum oven to be 60° C., the vacuum degree to be -0.09 MPa, and the drying time to be 5 to 6 hours, and finally obtain an ammonium perchlorate product with a purity greater than 99%.

[0058] In this embodiment, the multi-point feeding method means that the tap water can be divided into multiple water flows after entering the wet pulverizer 1 through the water inlet of the wet pulverizer 1.

[0059] In this embodiment, the liquid obtained by filtration includes a filtrate and a washing liquid.

[0060] In this embodiment, the liquid obtained by filtration in the extraction filtrate receiving tank is the extraction liquid.

[0061] In this embodiment, in step 1, the solid-liquid ratio is maintained at 1:7 during the pulverization process.

[0062] In this embodiment, in step 3, the extraction time is 25 min and the stirring speed is 200 rpm.

[0063] In this embodiment, in step 4, the ratio of the feeding speed of the extracted mixture to the filtering speed of the disc filter 4 is 1:1.25.

[0064] In this embodiment, in step five, the ratio of the amount of rinse water to the total amount of filtered material is 1:4.

[0065] In this embodiment, in step seven, the cooling rate is 1.5° C. / min and the stirring speed is 200 rpm.

[0066] In this embodiment, in step eight, the vacuum degree in the crystallization filtrate receiving tank 11 is -0.09 MPa.

[0067] In this embodiment, in step nine, the drying time is 5.5 hours.

[0068] As a preferred solution of this embodiment, in step 1, the particle size of the solid retired HTPB propellant after crushing is 0.5 to 1.5 mm.

[0069] In step 3, the material temperature during the extraction process is 50±5°C.

[0070] In step seven, the temperature of the material in the crystallization kettle 9 is reduced to less than or equal to 5°C.

[0071] In this embodiment, in step 1, the particle size of the solid retired HTPB propellant after crushing is 1 mm to ensure that the extraction rate of ammonium perchlorate is ≥90%.

[0072] In this embodiment, in step seven, the temperature of the material in the crystallization kettle 9 is reduced to 5°C.

[0073] As a preferred solution of this embodiment, in step six, the conductivity of the liquid obtained by filtration in the extraction filtrate receiving tank 7 is set to 105 ms / cm.

Claims

1. A device for extracting and recovering ammonium perchlorate from retired HTPB propellant, comprising a wet pulverizer (1), characterized in that: The discharge port of the wet pulverizer (1) is connected to the feed port of the extraction kettle (2), and the discharge port of the extraction kettle (2) is connected to the disc filter feed port (401) of the disc filter (4) through the extraction mixture metering pump (3); It also includes a washing water storage tank (5), the washing water outlet of the washing water storage tank (5) is connected to the disc filter washing water inlet (402) of the disc filter (4) through a washing water metering pump (6); The disc filter filtrate outlet (403) of the disc filter (4) is connected to the liquid inlet of the extraction filtrate receiving tank (7), the liquid outlet of the extraction filtrate receiving tank (7) is connected to the feed port of the crystallization kettle (9) through the extraction liquid metering pump (8), and the discharge port of the crystallization kettle (9) is connected to the feed port of the crystallization liquid filter (10).

2. The device for extracting and recovering ammonium perchlorate from retired HTPB propellant according to claim 1, wherein: The filtrate outlet of the crystallization liquid filter (10) is also connected to the liquid inlet of the crystallization filtrate receiving tank (11).

3. The device for extracting and recovering ammonium perchlorate from retired HTPB propellant according to claim 2, wherein: The vacuum port of the crystallization filtrate receiving tank (11) is connected to the air extraction port of the vacuum pump (12); The vacuum port of the extraction filtrate receiving tank (7) is also connected to the air extraction port of the vacuum pump (12).

4. The device for extracting and recovering ammonium perchlorate from retired HTPB propellant according to claim 1, wherein: The hot water inlet of the jacket of the extraction kettle (2) is connected to the liquid outlet of the heater (13); The hot water outlet of the jacket of the extraction kettle (2) is connected to the liquid return port of the heater (13).

5. The device for extracting and recovering ammonium perchlorate from retired HTPB propellant according to claim 1, wherein: The cold water inlet of the jacket of the crystallization kettle (9) is connected to the liquid outlet of the refrigerator (14); The cold water outlet of the jacket of the crystallization kettle (9) is connected to the liquid return port of the refrigerator (14).

6. The device for extracting and recovering ammonium perchlorate from retired HTPB propellant according to claim 5, characterized in that: The jacket cold water inlet of the wet pulverizer (1) is connected to the liquid outlet of the refrigerator (14); the jacket cold water outlet of the wet pulverizer (1) is connected to the liquid return port of the refrigerator (14); A propellant feeder (15) is further provided above the wet pulverizer (1); the discharge port of the propellant feeder (15) is connected to the feed port of the wet pulverizer (1); A tap water high level tank (16) is also provided above the wet pulverizer (1); the water outlet of the tap water high level tank (16) is connected to the water inlet of the wet pulverizer (1).

7. The device for extracting and recovering ammonium perchlorate from retired HTPB propellant according to claim 6, wherein: The liquid outlet of the extraction filtrate receiving tank (7) can also be connected to the water inlet of the tap water high-level tank (16) through the extraction liquid metering pump (8).

8. A method for extracting and recovering ammonium perchlorate from retired HTPB propellant, characterized in that: The method is implemented using the device for extracting and recovering ammonium perchlorate from retired HTPB propellant according to any one of claims 1 to 7; the method specifically comprises the following steps: Step 1: Open the valve of the water outlet of the tap water high-level tank (16), measure the tap water through a flow meter, and add the tap water into the wet grinder (1) through a multi-point feeding method; start the propellant feeder (15), add the solid retired HTPB propellant in the propellant feeder (15) into the wet grinder (1) and grind it, and keep the solid-liquid ratio at 1: (6-8) during the grinding process; Step 2: while the solid retired HTPB propellant is being pulverized, a refrigerator (14) is started, and the valve of the cold water inlet of the jacket of the wet pulverizer (1) is opened, so that the material temperature of the solid retired HTPB propellant is maintained at 25±2° C. during the pulverization process; the solid-liquid mixture obtained after the solid retired HTPB propellant is pulverized is transported from the discharge port of the wet pulverizer (1) to the feed port of the extraction kettle (2); Step 3: After the solid-liquid mixture is added, the valve of the hot water inlet of the jacket of the extraction kettle (2) is opened, and the heater (13) is started to ensure the material temperature during the extraction process, and the extraction time is ≥25 min and the stirring speed is ≥200 rpm; Step 4: Open the valve of the discharge port of the extraction kettle (2), start the extraction mixture metering pump (3), and continuously add the extracted mixture to the disc filter (4). The disc filter (4) is in a continuous filtration mode, and the relationship between the feeding speed of the extracted mixture and the filtration speed of the disc filter (4) is 1: (1 to 1.5); Step 5: while filtering, start the washing water metering pump (6) to deliver the tap water in the washing water storage tank (5) to the rinsing area of the disc filter (4). The ratio of the amount of rinsing water to the total amount of filtered material is 1:(3-5). After the filtration is completed, the filtered liquid enters the extraction filtrate receiving tank (7) for temporary storage, and the filter cake enters the transfer barrel; Step 6: Detecting the conductivity of the liquid obtained by filtration in the extraction filtrate receiving tank (7) by conductivity. If the conductivity of the liquid obtained by filtration in the extraction filtrate receiving tank (7) is less than the set value, when the next batch of solid retired HTPB propellant is pulverized in the wet pulverizer (1), the extraction liquid metering pump (8) is started, and the liquid obtained by filtration in the extraction filtrate receiving tank (7) is returned to the tap water high-level tank (16) through the extraction liquid metering pump (8). The liquid obtained by filtration in the extraction filtrate receiving tank (7) is used as a cooling medium to recycle the liquid obtained by filtration. After being recycled for multiple times, when the conductivity of the liquid filtered in the extraction filtrate receiving tank (7) is greater than or equal to a set value, the pipeline valve of the extraction liquid metering pump (8) is switched, and the liquid filtered in the extraction filtrate receiving tank (7) is added to the crystallization kettle (9) through the extraction liquid metering pump (8) for crystallization treatment; Step 7: After all the liquid obtained by filtration in the extraction filtrate receiving tank (7) is added to the crystallization kettle (9), the crystallization kettle (9) is started and stirred, the valve of the jacket cold water inlet of the crystallization kettle (9) is opened, and the temperature of the material in the crystallization kettle (9) is slowly reduced. The cooling rate range is 1 to 2°C / min, and the stirring speed is ≥200rpm; after continuing to keep warm and stir for 30 minutes, the valve of the discharge port of the crystallization kettle (9) is opened to transport the crystallized material to the crystallization liquid filter (10); Step eight, after all the crystallized materials are transported to the crystallization liquid filter (10), the valve of the vacuum port of the crystallization filtrate receiving tank (11) is opened to evacuate the vacuum so that the vacuum degree in the crystallization filtrate receiving tank (11) is ≤-0.09MPa, and the crystallization mother liquor is pumped into the crystallization filtrate receiving tank (11); after all the crystallization mother liquor enters the crystallization filtrate receiving tank (11), the valve of the vacuum port of the crystallization filtrate receiving tank (11) is closed; the vacuum pump (12), the heater (13) and the refrigerator (14) are turned off, and the filter cake in the crystallization liquid filter (10) is the recovered ammonium perchlorate; Step nine, collecting the filter cake in the crystallization liquid filter (10), placing it in an explosion-proof vacuum oven, controlling the temperature in the explosion-proof vacuum oven to 60° C., the vacuum degree to -0.09 MPa, and the drying time to 5 to 6 hours, and finally obtaining an ammonium perchlorate product with a purity greater than 99%.

9. The method for extracting and recovering ammonium perchlorate from retired HTPB propellant according to claim 8, wherein: In step 1, the solid retired HTPB propellant is crushed to a particle size of 0.5 to 1.5 mm; In step 3, the material temperature during the extraction process is 50±5°C; In step seven, the temperature of the material in the crystallization kettle (9) is reduced to less than or equal to 5°C.

10. The method for extracting and recovering ammonium perchlorate from retired HTPB propellant according to claim 9, wherein: In step six, the conductivity of the liquid filtered in the extraction filtrate receiving tank (7) is set to 105ms / cm.

Citation Information

Patent Citations

  • Production system for preparing nicotinamide fungicides

    CN219308403U

  • Treatment of solids with liquids

    GB1010321A

  • Apparatus and method for the disposal of waste solid rocket motors

    KR101122575B1

  • Method for leaching rare earth elements and critical minerals from organically associated materials

    US20220145421A1

  • Hydraulic waste propellant macerator and method of use

    US4662893A