Washing, filtering and drying integrated device and easily spontaneous combustion material production device

Abstract

The utility model belongs to the field of filtering and drying equipment, and particularly relates to a washing, filtering and drying integrated device and an easily spontaneous combustion material production device. The washing, filtering and drying integrated device comprises a washing, filtering and drying kettle, the washing, filtering and drying kettle comprises a kettle body, a washing solvent inlet and a washing waste liquid outlet are formed in the kettle body, and a stirring mechanism and a filtering mechanism are arranged in the kettle body. The kettle body is connected with a hot gas pipeline and a cold gas pipeline; the hot gas pipeline is used for introducing hot gas into the kettle body so as to blow and dry a material to be dried; the cold gas pipeline is used for introducing cold gas into the kettle body so as to cool the dried material; and a gas exhaust port for exhausting the hot gas and the cold gas during blowing drying and cooling is also arranged. According to the utility model, the spontaneous combustion of the high-activity material easy to spontaneously ignite during drying, discharging, transferring, packaging and other post-processing can be avoided, so that the production and processing safety of the material is improved.

Description

Technical Field

[0001] The utility model belongs to the field of filtering and drying equipment, and in particular relates to a washing, filtering and drying integrated device and a device for producing spontaneously combustible materials. Background Art

[0002] Sodium aluminum hydride (LiAlH4) is a strong reducing agent widely used in organic synthesis reactions. It is also an excellent solid hydrogen storage medium, used for the efficient and safe storage and transportation of hydrogen.

[0003] The Chinese invention patent with authorization announcement number CN 116573613 B, which was authorized on September 19, 2023, discloses a method for synthesizing sodium aluminum hydride using a single substance, wherein a mechanical mixture of metallic aluminum, metallic sodium and a solvent is subjected to a high-temperature and high-pressure reaction by introducing hydrogen into an autoclave to obtain a sodium aluminum hydride solution or a sodium aluminum hydride suspension, and large particles are removed from the obtained sodium aluminum hydride solution or suspension, and the solvent is removed from the filtrate to obtain powdered sodium aluminum hydride.

[0004] A Chinese invention patent with authorization announcement number CN 101531338 B, published on December 1, 2010, discloses a method for preparing sodium aluminum hydride. The method uses liquid sodium, solid aluminum, and hydrogen as reaction raw materials, triethylaluminum and titanium as catalysts, and toluene as solvent. A sodium aluminum hydride suspension is obtained through a high-temperature and high-pressure reaction. The suspension is then allowed to settle, the supernatant is discharged, and the suspension is dried to obtain a powdered sodium aluminum hydride solid.

[0005] As can be seen from the above production process of sodium aluminum hydride, it requires steps such as slurry filtration, solvent washing, and drying to ultimately produce powdered sodium aluminum hydride solid. Powdered sodium aluminum hydride solid is a hazardous chemical that is prone to spontaneous combustion and will spontaneously ignite within approximately one minute after contact with air. Powdered sodium aluminum hydride also decomposes at high temperatures to produce flammable and explosive gases such as hydrogen. These characteristics dictate that during the production of sodium aluminum hydride, transfer between process steps should be minimized to avoid contact with moisture, air, and other substances, thereby improving industrial production safety.

[0006] The Chinese utility model patent with an authorization announcement date of April 2, 2021 and an authorization announcement number of CN 212854846 U discloses a multifunctional filter with a dust removal device, including a kettle body consisting of a cylinder and a cylinder cover, a stirring mechanism is installed above the top center of the cylinder cover, a feed port is provided on the cylinder cover, a filtering mechanism is provided at the bottom of the cylinder, and a water outlet is provided at the center of the bottom of the cylinder. The slurry to be treated can enter the cylinder through the feed port, and the water filtered by the filtering mechanism is discharged through the water outlet. When solvent washing is required, the feed port can be used as the inlet of the washing solvent, and the water outlet is used as the outlet of the washing waste liquid, thereby realizing the filtering and washing functions. In addition, in order to achieve drying after washing, side heating coils and bottom heating coils are respectively provided on the side and bottom of the cylinder to achieve drying of the material.

[0007] When drying hazardous chemicals that are prone to spontaneous combustion, such as sodium aluminum hydride, the above-mentioned drying method using heating coils on the sides and bottom of the cylinder uses heat conduction to achieve heating and drying, and the overall drying efficiency is low. At the same time, the material may decompose due to heat during the drying process to produce flammable and explosive substances such as H2. The accumulation of flammable and explosive substances will pose a major safety hazard to the drying process and subsequent material transportation, packaging and other processes. Utility Model Content

[0008] The first purpose of the utility model is to provide an integrated washing, filtering and drying device to solve the problem that the existing device is dangerous when producing flammable materials such as sodium aluminum hydride.

[0009] The second purpose of the present invention is to provide a device for producing materials prone to spontaneous combustion, so as to solve the problem that flammable materials such as sodium aluminum hydride are prone to spontaneous combustion in the air.

[0010] In order to achieve the above first purpose, the technical solution adopted by the utility model is:

[0011] A washing, filtering and drying integrated device comprises a washing, filtering and drying kettle, the washing, filtering and drying kettle comprising a kettle body, the kettle body being provided with a washing solvent inlet and a washing waste liquid outlet, the kettle body being provided with a stirring mechanism and a filtering mechanism, the kettle body being connected to a hot gas pipeline for introducing hot gas into the kettle body to purge and dry the material to be dried, and a cold gas pipeline for introducing cold gas into the kettle body to cool the dried material, and further provided with a gas outlet for discharging the hot gas and cold gas during the purge drying and cooling.

[0012] The utility model is an improved invention. After slurry of inflammable materials such as sodium aluminum hydride is filtered and washed, hot gas is used for blowing and drying. The hot gas directly carries the free solvent and is discharged from the gas outlet, so the drying efficiency is high. During the above gas discharge process, new hot gas is continuously used to realize gas replacement, so as to update the inert gas atmosphere in the kettle body, and inflammable and explosive substances that may be generated by thermal decomposition of the material are discharged in time to avoid accumulation, thereby improving the safety of the atmosphere environment. After the blowing and drying is completed, cold gas is used for timely cooling to avoid spontaneous combustion of highly active and self-igniting materials due to excessive temperature during post-processing such as discharging, transportation, and packaging, thereby improving the safety of the production and processing of such materials.

[0013] Preferably, the gas outlet is connected to a gas-solid separation device, and the gas-solid separation device is provided with a filter element for intercepting solid materials, and a gas outlet for discharging gas after gas-solid separation.

[0014] Further preferably, the gas outlet is connected to a condenser via a condensation pipeline, and the condenser is connected to a solvent recovery tank.

[0015] More preferably, the washing waste liquid outlet is connected to a mother liquor discharge pipeline, and the mother liquor discharge pipeline is connected to the condensation pipeline through a drying tail gas pipeline; a first valve is provided on the mother liquor discharge pipeline, and a second valve is provided on the drying tail gas pipeline.

[0016] Preferably, the gas outlet is connected to a backflush mechanism.

[0017] Further preferably, the backflush mechanism includes a first backflush pipeline connected to the gas outlet and a second backflush pipeline connected to the first backflush pipeline, one of the first backflush pipeline and the second backflush pipeline is used to pass hot gas, and the other is used to pass cold gas.

[0018] Preferably, the kettle body is connected to a slurry inlet pipeline to be treated, the washing solvent inlet is connected to a solvent inlet pipeline, and a flushing pipeline is connected between the slurry inlet pipeline to be treated and the solvent inlet pipeline.

[0019] Preferably, the kettle body is provided with a jacket, and the jacket is provided with a medium inlet for introducing a heat medium or a coolant, and a medium outlet for discharging the heat medium or the coolant.

[0020] In order to achieve the above second purpose, the technical solution adopted by the present utility model is:

[0021] A device for producing spontaneously combustible materials comprises the above-mentioned integrated washing, filtering and drying device, wherein the integrated washing, filtering and drying device comprises a washing, filtering and drying kettle having a discharge port connected to a tablet press.

[0022] After filtering, washing and drying the slurry of flammable materials such as sodium aluminum hydride, a powdered sodium aluminum hydride solid is obtained. The powdered sodium aluminum hydride solid is directly tableted by using the self-igniting material production device of the utility model, which can effectively improve the extremely unstable property of sodium aluminum hydride in the air and extend the self-ignition time from about 1 minute to more than 1 hour, thereby effectively improving the safety of flammable materials such as sodium aluminum hydride in storage and transportation, and greatly reducing the safety risks of production, transportation and application enterprises.

[0023] Preferably, a powder silo is connected between the discharge port and the tablet press. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] Figure 1 This is a schematic structural diagram of the integrated washing, filtering and drying device according to Example 1 of the present utility model;

[0025] Figure 2 This is a schematic structural diagram of a device for producing spontaneously combustible materials according to Example 2 of the present utility model;

[0026] Among them, 1-washing, filtering and drying kettle; 2-condenser; 3-solvent recovery tank; 4-hot gas pipeline; 5-cold gas pipeline; 6-gas inlet; 7-exhaust port; 8-gas outlet; 9-exhaust pipeline; 10-gas-solid separation device; 11-first backflush pipeline; 12-second backflush pipeline; 13-condensation pipeline; 14-tail gas outlet pipeline; 15-nitrogen inlet pipeline; 16-solvent outflow pipeline; 17-slurry inlet; 18-washing solvent inlet; 19-washing waste liquid outlet; 20-slurry injection pipeline; 21-washing solvent injection pipeline; 22-mother liquor discharge pipeline; 23-drying tail gas pipeline; 24-first valve; 25-second valve; 26-flushing pipeline; 27-thermal oil feed pipeline; 28-thermal oil discharge pipeline; 29-stirring mechanism; 30-discharge port; 31-powder silo; 32-tablet press. DETAILED DESCRIPTION

[0027] The technical concept of the utility model is to ensure that slurry filtration, washing and drying are completed in the same equipment, and to use hot gas to purge and dry in combination with cold gas for cooling, so as to avoid the accumulation of heat and flammable and explosive substances in the drying process, which may cause safety risks to various production links of materials such as sodium aluminum hydride.

[0028] Furthermore, by setting up a condensation pipeline and a drying tail gas pipeline, the drying efficiency of the material can be further improved and the solvent can be recycled.

[0029] The above-mentioned integrated washing, filtering and drying device can be further combined with a tablet press to directly produce tablet products, which can suppress the spontaneous combustion of substances such as sodium aluminum hydride to a large extent and improve the production, storage and transportation of such substances.

[0030] The implementation process of the present utility model is described in detail below with reference to specific embodiments.

[0031] 1. Specific embodiments of the integrated washing, filtering and drying device of the present utility model

[0032] Example 1

[0033] The washing, filtering and drying integrated device of this embodiment is described by taking the solid-liquid separation, washing and drying of sodium aluminum hydride slurry as an example. Figure 1 As shown, it includes a washing, filtering and drying kettle 1, a condenser 2 and a solvent recovery tank 3.

[0034] The washing, filtering, and drying kettle 1 is an integrated solid-liquid separation, washing, and drying facility for sodium aluminum hydride slurry. It comprises a kettle body with a sealed inner cavity, to which are connected a hot gas line 4 and a cold gas line 5. The hot gas line 4 and the cold gas line 5 are used to introduce hot gas or cold gas, respectively, into the kettle body for hot gas purge drying and post-purge cooling. Stirring is simultaneously activated during the gas purge process. For flammable materials such as sodium aluminum hydride, inert gases such as nitrogen should be used for both hot and cold gases. The hot gas temperature is 90-95°C and the pressure is 0.4-0.6 MPa, while the cold gas temperature is 0-25°C and the pressure is 0.4-0.6 MPa.

[0035] The hot gas pipeline 4 and the cold gas pipeline 5 are both connected to the gas inlet 6 provided on the kettle body. Specifically, the cold gas pipeline 5 is directly connected to the gas inlet 6, and the hot gas pipeline 4 is connected to the cold gas pipeline 5. This can reduce the opening of the kettle body and simplify the structure of the kettle body. The kettle body is also provided with an exhaust port 7 and a gas outlet 8. The exhaust port 7 is connected to the exhaust pipeline 9 so that the air in the kettle can be discharged by nitrogen before the slurry enters the kettle body, thereby creating an inert gas atmosphere. The gas outlet 8 is used to discharge the hot gas and cold gas introduced during the drying and subsequent cooling of the slurry to maintain the pressure balance in the kettle. The comprehensive treatment method of hot gas drying and cooling is essentially to use inert gas contact to achieve heat transfer and remove heat and volatile components, which not only improves the treatment efficiency, but also realizes the washing, drying and cooling of the materials in the kettle body, reduces the risk of spontaneous combustion and explosion of the materials during the above-mentioned treatment and subsequent discharge, transportation and packaging processes, and maximizes the safety of sodium aluminum hydride production.

[0036] The gas outlet 8 is connected to a gas-solid separation device 10 and a backflush mechanism to perform gas-solid separation on the gas-solid mixture produced during the hot and cold gas purges. The gas-solid separation device 10 has a filter element. The backflush mechanism backflushes after the filter element is clogged with solid powder, returning the powder to the kettle. The backflush mechanism includes a first backflush line 11 and a second backflush line 12 connected to the gas-solid separation device 10. Specifically, the first backflush line 11 is directly connected to the gas-solid separation device 10, and the second backflush line 12 is connected to the first backflush line 11. The first backflush line 11 is used to pass cold gas, and the second backflush line 12 is used to pass hot gas.

[0037] The gas-solid separation device 10 is connected to the condenser 2 via the condensation pipeline 13, and the condenser 2 is connected to the solvent recovery tank 3. In this way, after the gas components flowing out of the gas-solid separation device 10 are condensed by the condenser 2, the volatile solvent components in the gas components can be condensed, and then enter the solvent recovery tank 3 for recovery, and the non-condensable gas in the gas components is discharged through the tail gas outlet pipeline 14 at the upper end of the solvent recovery tank 3. The upper end of the solvent recovery tank 3 is also provided with a nitrogen inlet pipeline 15, and the nitrogen inlet pipeline 15 introduces nitrogen into the solvent recovery tank 3, thereby placing the solvent recovery tank 3 in a slightly positive pressure state to prevent outside air from entering. The lower end of the solvent recovery tank 3 is connected to a solvent outflow pipeline 16.

[0038] The upper end of the kettle body is provided with a slurry inlet 17 and a washing solvent inlet 18, and the lower end of the kettle body is provided with a washing waste liquid outlet 19. The slurry inlet 17 is connected to the slurry injection pipeline 20, the washing solvent inlet 18 is connected to the washing solvent injection pipeline 21, and the washing waste liquid outlet 19 is connected to the mother liquor discharge pipeline 22 (the washing waste liquid can be used as a solvent for the production of sodium aluminum hydride and recycled as a mother liquor). A drying tail gas pipeline 23 is also connected between the mother liquor discharge pipeline 22 and the condensation pipeline 13. The mother liquor discharge pipeline 22 and the drying tail gas pipeline 23 are respectively provided with a first valve 24 and a second valve 25. During the washing stage, the first valve 24 is opened and the second valve 25 is closed to discharge the mother liquor; during the drying and cooling stage, the first valve 24 is closed and the second valve 25 is opened to allow the gas to enter the drying tail gas pipeline 23, the condenser 2 and the solvent recovery tank 3, so as to achieve condensation and recovery of the solvent in the gas components. During the hot gas drying and cold gas cooling processes, the provision of gas outlet 8 and drying tail gas pipeline 23 allows the gas to flow out of the kettle along both upper and lower paths. The upper path passes through gas outlet 8 and gas-solid separation device 10, while the lower path passes through the filtration mechanism and washing waste liquid outlet 19. Both paths pass through condenser 2 before entering solvent recovery tank 3. This arrangement further improves drying and cooling efficiency, significantly enhancing material production efficiency under closed and inert atmosphere conditions.

[0039] A flushing line 26 is also connected between the slurry injection line 20 and the washing solvent injection line 21. The flushing line 26 can flush the sodium aluminum hydride slurry remaining in the slurry injection line 20 to ensure that the slurry injection line 20 is clean.

[0040] The kettle is equipped with a jacket, connected to a thermal oil feed line 27 and a thermal oil discharge line 28. During the hot gas drying phase, hot thermal oil is introduced through these lines to assist in drying. During the cooling phase, cold thermal oil is introduced through these lines to assist in cooling. The jacket structure and the corresponding introduction of heat and coolant further improve drying and cooling efficiency.

[0041] The kettle is equipped with a stirring mechanism 29 and a filtering mechanism. The stirring mechanism 29 stirs the material and the washing solvent to promote more efficient washing. The filtering mechanism is located at the bottom of the kettle and separates the liquid (or gas) and solid by using filter cloth and filter plates. The stirring mechanism 29 and the filtering mechanism are both conventional structural designs in the field and will not be described in detail here.

[0042] A discharge port 30 is provided at the lower end of the kettle body. After drying and cooling, powdered material is obtained, which can be directly discharged from the discharge port in conjunction with the stirring mechanism 29.

[0043] The production process of the above-mentioned washing, filtering and drying integrated device is as follows:

[0044] Liquid sodium, solid aluminum, and hydrogen are used as the reaction materials, triethylaluminum is used as the catalyst, and toluene is used as the solvent. A sodium aluminum hydride slurry is produced after a high-temperature, high-pressure reaction. The sodium aluminum hydride slurry is filtered, washed, and dried in the integrated washing, filtration, and drying device, minimizing the possibility of the sodium aluminum hydride coming into contact with air. Toluene is used as the washing solvent.

[0045] Nitrogen is injected into the washing, filtering, and drying kettle 1 through the gas inlet 6 for gas replacement, and the replaced gas is discharged from the exhaust port 7. The sodium aluminum hydride slurry enters the washing, filtering, and drying kettle 1 through the slurry injection pipe for filtration, and the filtrate flows out through the mother liquor discharge line 22. Then, a solvent is injected into the washing, filtering, and drying kettle 1 through the washing solvent injection line 21 for washing. Washing can be performed twice or more. The initial liquid phase separation components of the sodium aluminum hydride slurry and the liquid phase separation components after washing can be discharged as mother liquor through the mother liquor discharge line 22. The impurities contained in the mother liquor are mainly catalysts and can be directly reused in the synthesis step.

[0046] After washing is completed, hot nitrogen is introduced into the washing, filtering, and drying kettle 1 for purge drying. Simultaneously, the valves on the jacket's thermal oil feed and discharge lines are opened. The airflow generated during the purge drying process is split into two paths. One path passes through the gas-solid separation unit 10 at the top for gas-solid separation. The gas components are condensed in the condenser 2 and then enter the solvent recovery tank 3. Non-condensable gases in the solvent recovery tank 3 are discharged through the tail gas outlet line 14. The other path passes through the filter cake and filter plates below, then passes through the drying tail gas line 23 and condenses again in the condenser 2 before flowing into the solvent recovery tank 3. During the purge drying process, powdered sodium aluminum hydride can clog the filter element of the gas-solid separation unit 10, reducing gas-solid separation efficiency. Hot nitrogen is then introduced through the backflush line to backflush the powdered sodium aluminum hydride back into the washing, filtering, and drying kettle 1, ensuring the separation efficiency of the gas-solid separation unit 10. After purge drying, cold nitrogen is introduced into the washing, filtering, and drying kettle 1 to cool it down. Simultaneously, the jacket is switched to cold thermal oil. During the cooling process of the cold nitrogen, the backflush line can also be used to introduce cold nitrogen for backflush, so as to clean the filter element of the gas-solid separation device 10 and improve the gas-solid separation efficiency.

[0047] After cooling is completed (cooling to below 40° C.), powdered sodium aluminum hydride is obtained, which can be subsequently sealed and packaged in an existing manner to obtain a finished product.

[0048] 2. Specific embodiments of the device for producing spontaneously combustible materials of the present invention

[0049] Example 2

[0050] The utility model of the production device of easily self-igniting materials, such as Figure 2 As shown, it includes a washing, filtering and drying integrated device, a powder silo 31 and a tablet press 32.

[0051] The implementation of the integrated washing, filtering, and drying device is the same as that of Example 1, comprising a washing, filtering, and drying kettle 1 having a discharge port 30 at its lower end, which is sequentially connected to a powder silo 31 and a tablet press 32 via connecting pipelines. Powdered sodium aluminum hydride produced by the washing, filtering, and drying kettle 1 is temporarily stored in the powder silo 31. The powdered sodium aluminum hydride in the powder silo 31 is then pressed into sodium aluminum hydride tablets in the tablet press 32. The tablets are then sealed in bags (or barrels) by a packaging machine and can be stored or transported as finished products.

[0052] In this example, powdered sodium aluminum hydride was pressed into dense sheets approximately 10 mm x 5 mm. Spontaneous combustion experiments showed that powdered sodium aluminum hydride spontaneously combusted within about one minute upon contact with air. However, after being pressed into sheets using the production apparatus of the present invention, the spontaneous combustion time was extended to over one hour.

[0053] Using this production device, the entire sodium aluminum hydride production process is isolated from operators and can be automated, greatly improving the safety of sodium aluminum hydride production and preventing production accidents. Furthermore, the extended spontaneous combustion time of sodium aluminum hydride is also very beneficial for the storage and transportation of sodium aluminum hydride solids, greatly expanding the application scenarios of sodium aluminum hydride solids.

Claims

1. A washing, filtering and drying integrated device, comprising a washing, filtering and drying kettle, wherein the washing, filtering and drying kettle comprises a kettle body, wherein the kettle body is provided with a washing solvent inlet and a washing waste liquid outlet, and wherein the kettle body is provided with a stirring mechanism and a filtering mechanism, wherein: The kettle body is connected to a hot gas pipeline for introducing hot gas into the kettle body to purge and dry the material to be dried, and a cold gas pipeline for introducing cold gas into the kettle body to cool the dried material. A gas exhaust port is also provided to discharge the hot gas and cold gas during the purge drying and cooling.

2. The integrated washing, filtering and drying device according to claim 1, characterized in that: The gas outlet is connected to a gas-solid separation device, and the gas-solid separation device is provided with a filter element for intercepting solid materials and a gas outlet for discharging gas after gas-solid separation.

3. The integrated washing, filtering and drying device according to claim 2, characterized in that: The gas outlet is connected to a condenser through a condensation pipeline, and the condenser is connected to a solvent recovery tank.

4. The integrated washing, filtering and drying device according to claim 3, characterized in that: The washing waste liquid outlet is connected to a mother liquid discharge pipeline, and the mother liquid discharge pipeline is connected to the condensation pipeline through a drying tail gas pipeline; a first valve is provided on the mother liquid discharge pipeline, and a second valve is provided on the drying tail gas pipeline.

5. The integrated washing, filtering and drying device according to claim 2, wherein: The gas outlet is connected to a backflush mechanism.

6. The integrated washing, filtering and drying device according to claim 5, characterized in that: The backflush mechanism includes a first backflush pipeline connected to the gas outlet and a second backflush pipeline connected to the first backflush pipeline. One of the first backflush pipeline and the second backflush pipeline is used to pass hot gas, and the other is used to pass cold gas.

7. The integrated washing, filtering and drying device according to claim 1, wherein: The kettle body is connected to a pipeline for inletting slurry to be processed, the washing solvent inlet is connected to a solvent inlet pipeline, and a flushing pipeline is connected between the pipeline for inletting slurry to be processed and the solvent inlet pipeline.

8. The integrated washing, filtering and drying device according to claim 1, wherein: The kettle body is provided with a jacket, and the jacket is provided with a medium inlet for introducing a heat medium or a coolant, and a medium outlet for discharging the heat medium or the coolant.

9. A device for producing spontaneously combustible materials, comprising the integrated washing, filtering and drying device according to any one of claims 1 to 8, wherein the integrated washing, filtering and drying device comprises a washing, filtering and drying kettle having a discharge port, wherein: The discharge port is connected with a tablet press.

10. The device for producing spontaneously combustible materials according to claim 9, characterized in that: A powder silo is also connected between the discharge port and the tablet press.

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