Production process for efficient recovery of phosphoric acid fluorine resources by wet method

Abstract

The application discloses a kind of wet-process phosphoric acid fluorine resource efficient recovery production process, comprising the following steps: S1, the solid ammonium fluoride is added water, ammonium fluoride is uniformly mixed and stirred with water, and ammonium fluoride absorption liquid is prepared, ammonium fluoride absorption liquid is carried out in spray device high-efficiency atomization spray;S2, wet-process phosphoric acid reaction process flue gas is passed into to spray tower, so that flue gas and ammonium fluoride absorption liquid are fully reacted, so that hydrofluoric acid is obtained, and hydrofluoric acid falls to the storage tank at the bottom of spray tower with gravity;S3, the fluorine resource recovery process of the application is optimized, the fluorine in tail gas is absorbed by absorption liquid, and by spray tower assembly, spray assembly, application replacement assembly, limiting component, absorption liquid is realized in the process of spraying, when different hole numbers appear in the process of spray blockage, linkage adaptive adjustment is realized, while avoiding absorption liquid waste, absorption liquid and tail gas are uniformly contacted, tail gas is fully reacted with absorption liquid, and efficient recovery of fluorine resources is realized.

Description

Technical Field

[0001] This invention relates to the field of wet-process fluorine phosphate recovery technology, and in particular to a high-efficiency wet-process fluorine phosphate resource recovery production process. Background Technology

[0002] Wet-process phosphoric acid is an inorganic compound produced through a wet process. It is primarily used in fertilizer production and other industrial applications. The preparation of wet-process phosphoric acid typically uses phosphate rock as raw material, and involves a series of chemical reactions and processing steps to extract phosphoric acid. The main steps include: 1. Digestion of phosphate rock: The phosphate rock is mixed with a digestion solution such as dilute acid to dissolve the phosphoric acid. 2. Filtration and solid-liquid separation: The digestion solution is filtered to separate the solid phosphoric acid residue from the liquid. 3. Concentration and crystallization: The liquid phosphoric acid is concentrated to increase its concentration, and crystallization is carried out to obtain crystalline solid phosphoric acid. 4. Refining and drying: The crystallized phosphoric acid is further processed and refined to remove impurities and improve its purity. Finally, it is dried to obtain the final wet-process phosphoric acid product.

[0003] The above steps will generate fluorine-containing tail gas. In the existing technology, in order to absorb fluorine gas, a defluorination tank or a spray tower is generally selected to treat the tail gas and recover fluorine. However, in the process of using the existing technology, the contact between the tail gas and the absorption liquid is not complete. Especially in the process of spray tower treatment, once the spray port is blocked, it cannot be detected in time, which directly leads to the problem of reduced fluorine treatment efficiency in the tail gas. Therefore, a wet process for efficient recovery of fluorine phosphate resources is needed. Summary of the Invention

[0004] This invention provides a wet-process high-efficiency production process for recovering fluorine from phosphoric acid resources, in order to solve the problem of unsatisfactory fluorine treatment efficiency in existing tail gas treatment methods.

[0005] To solve the above problems, the present invention is achieved through the following technical solution: A high-efficiency wet-process production technology for the recovery of fluorine phosphate resources includes the following steps: S1. Add solid ammonium fluoride to water, mix and stir the ammonium fluoride and water evenly through a mixing vessel to prepare ammonium fluoride absorption solution, and add the ammonium fluoride absorption solution to the spraying device for efficient atomization spraying. S2. The flue gas from the wet phosphoric acid reaction process is introduced into the spray tower of the spray device to allow the flue gas to react fully with the ammonium fluoride absorbent to obtain hydrofluoric acid. The hydrofluoric acid falls into the storage tank at the bottom of the spray tower by gravity. S3. The hydrofluoric acid in the storage tank is diverted to the external storage tank, and ammonia gas is introduced into the storage tank. The hydrofluoric acid reacts with the ammonia gas to produce ammonium bifluoride. The crystal precipitation device pumps the raw material out of the storage tank and performs crystallization treatment. Then, it is concentrated and evaporated to obtain ammonium bifluoride crystals, thus completing the absorption of fluorine in the wet phosphoric acid reaction process.

[0006] As a preferred technical solution, the spraying device in S1 includes a spraying tower assembly, a spraying assembly, an application replacement assembly, and a limiting assembly.

[0007] As a preferred technical solution, the spray tower assembly includes a spray tower body, a high-pressure pump disposed on one side of the spray tower body, a water supply pipe connected to the output end of the high-pressure pump, a water collection sleeve disposed within the spray tower body, and an annular groove formed inside the spray tower body.

[0008] As a preferred technical solution, the spray assembly includes a water distribution pipe connected to the water collection sleeve, an atomizing spray head connected to the front end of the water distribution pipe, a telescopic rod connected to the side of the atomizing spray head, a spare spray frame connected to the front end of the telescopic rod, and a drive pipe connected to the side end of the water supply pipe.

[0009] As a preferred technical solution, the water collection sleeve is connected to three water distribution pipes respectively; each water distribution pipe is equipped with an atomizing spray head, telescopic rod and spare spray frame with the same structure at its front end.

[0010] As a preferred technical solution, the water collecting sleeve is fitted with the drive pipe, and the drive pipe rotates along the water collecting sleeve; The side wall of the drive tube has several water inlet holes, which are connected to the water collection sleeve.

[0011] As a preferred technical solution, the application replacement component includes a short plate fixed in the annular groove, a first electric telescopic rod disposed on one side inside the annular groove, a second electric telescopic rod disposed in the groove opening on the bottom surface of the annular groove, a spare atomizing nozzle disposed at the top of the second electric telescopic rod, an infrared ray emitter disposed on one side of the spare atomizing nozzle, and an infrared ray receiver disposed on the other side of the spare atomizing nozzle. There are three electric telescopic poles, and the three electric telescopic poles are arranged in a ring.

[0012] As a preferred technical solution, the limiting component includes concave side plates fixed on both sides of the spare atomizing nozzle, an electric rotating shaft disposed in the concave side plates, and a rectangular plate connected to the electric rotating shaft.

[0013] As a preferred technical solution, the limiting component further includes a concave mounting frame disposed within the spare spray frame, a rotating shaft disposed within the concave mounting frame, a cover plate connected to the rotating shaft, and a circular opening formed on the bottom surface of the spare spray frame.

[0014] As a preferred technical solution, the spray nozzle of the drive pipe is directly opposite the distributed water distribution pipes, and the water jet from the drive pipe directly impacts and pushes the corresponding water distribution pipes.

[0015] The above-mentioned technical solution provides a high-efficiency wet-process phosphoric acid fluoride resource recovery production process, including the following steps: S1, adding solid ammonium fluoride to water, mixing and stirring the ammonium fluoride and water evenly through a mixing vessel to prepare an ammonium fluoride absorbent solution, and adding the ammonium fluoride absorbent solution to a spraying device for high-efficiency atomized spraying; S2, introducing the flue gas from the wet-process phosphoric acid reaction into the spraying tower of the spraying device, allowing the flue gas to fully react with the ammonium fluoride absorbent solution to obtain hydrofluoric acid, which falls to the storage tank at the bottom of the spraying tower by gravity; S3, guiding the hydrofluoric acid in the storage tank to an external storage tank, and introducing ammonia gas into the storage tank, where the hydrofluoric acid reacts with the ammonia gas to obtain ammonium bifluoride, covering the storage tank with a crystal precipitation device, and then concentrating and evaporating the ammonium bifluoride to obtain ammonium bifluoride crystals, thus completing the fluoride absorption during the wet-process phosphoric acid reaction.

[0016] Advantages of this invention: The fluorine resource recovery process is optimized by absorbing fluorine in the exhaust gas with an absorbent. Through the spray tower components, spray components, application replacement components, and limit components, the absorbent is dynamically adjusted according to the occurrence of spray blockage at different hole numbers during the spraying process. This avoids waste of absorbent while ensuring uniform contact between absorbent and exhaust gas, ensuring that the exhaust gas fully reacts with the absorbent, and achieving efficient recovery of fluorine resources. When a single spray hole becomes blocked, the pressure inside the pipe increases. At this time, the absorbent liquid is discharged through the drive pipe. The absorbent liquid impacts the corresponding water distribution pipe, thereby pushing the water collection sleeve to rotate along the drive pipe, achieving uniform spraying. When two or three spray holes become blocked, the impact force of the absorbent gradually increases, and the rotation speed of the water collection jacket gradually increases. Under the action of inertia, the spare spray frame is thrown out, triggering the replacement structure and realizing the automatic replacement of the spray structure. In this way, the automatic switching and linkage reaction are achieved according to the number of blocked holes, ensuring the uniform spray reaction of the absorbent and realizing the efficient recovery of fluorine. Attached Figure Description

[0017] To more clearly illustrate the technical solutions of the embodiments of the present invention, the present invention will be described in detail below with reference to the accompanying drawings and detailed embodiments. Obviously, the drawings described below are only some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort. Wherein: Figure 1 This is a flowchart of the wet-process high-efficiency recovery production process of fluorine phosphate resources in this invention; Figure 2 This is a structural diagram of the spray tower assembly in the wet-process high-efficiency recovery production process of fluorine phosphate resources of the present invention; Figure 3 This is a structural diagram of the spraying component in the wet-process high-efficiency recovery production process of fluorine phosphate resources of the present invention; Figure 4 This is a structural diagram of the replacement component used in the wet-process fluorine phosphate resource high-efficiency recovery production process of the present invention; Figure 5 This is a structural diagram of the limiting component in the wet-process fluorine phosphate resource high-efficiency recovery production process of the present invention; Figure 6 This is an internal structural diagram of the spare spray frame in the wet-process high-efficiency recovery production process of fluorine phosphate resources of the present invention; Figure 7 This is a schematic diagram of the fitting structure between the water collection jacket and the water conveying pipeline in the wet-process high-efficiency recovery production process of fluorine phosphate of the present invention. In the diagram: 11-Spray tower body; 12-High-pressure pump; 13-Water supply pipe; 14-Water collection jacket; 15-Annular groove; 21-Water distribution pipe; 22-Atomizing spray head; 23-Telescopic rod; 24-Spare spray frame; 25-Drive pipe; 31-Short plate; 32-First electric telescopic rod; 33-Second electric telescopic rod; 34-Spare atomizing spray head; 35-Infrared ray emitter; 36-Infrared ray receiver; 41-Concave side plate; 42-Electric rotating shaft; 43-Rectangular plate; 44-Concave mounting frame; 45-Rotating shaft; 46-Cover plate; 47-Circular opening. Detailed Implementation

[0018] To overcome the above deficiencies, this invention provides a wet-process high-efficiency recovery production process for fluorine phosphate resources to solve the problems mentioned in the background art.

[0019] To make the technical means, creative features, objectives and effects of this invention easier to understand, the invention will be further described below with reference to specific embodiments. Example 1

[0020] This invention provides a high-efficiency wet-process fluorine phosphate resource recovery production process, optimizing the fluorine resource recovery process. It utilizes an absorbent to absorb fluorine from the tail gas, and through a spray tower assembly, spray components, application replacement components, and limiting components, the absorbent is dynamically adjusted during spraying based on the occurrence of spray blockage at different hole numbers. This avoids waste of absorbent while ensuring uniform contact between the absorbent and the tail gas, guaranteeing sufficient reaction between the tail gas and the absorbent, thus achieving high-efficiency fluorine resource recovery.

[0021] Figures 1 to 7 The diagram shown is an overall structural schematic of one embodiment of the wet-process fluorine phosphate resource high-efficiency recovery production process of the present invention. Please refer to [link / reference]. Figures 1-7 ; The efficient wet-process production technology for recovering fluorine from phosphate resources includes the following steps: S1: First, add water to solid ammonium fluoride and mix and stir the ammonium fluoride and water evenly through a mixing vessel to prepare ammonium fluoride absorption solution. Then, perform high-efficiency atomization spraying of the ammonium fluoride absorption solution in a spraying device. The spraying device specifically includes a spraying tower assembly, spraying components, application replacement components, and limit components; The spray tower assembly includes a spray tower body 11, a high-pressure pump 12 located on one side of the spray tower body 11, a water supply pipe 13 connected to the output end of the high-pressure pump 12, a water collection sleeve 14 located inside the spray tower body 11, and an annular groove 15 formed inside the spray tower body 11. The spray assembly includes a water distribution pipe 21 connected to the water collection sleeve 14, an atomizing spray head 22 connected to the front end of the water distribution pipe 21, a telescopic rod 23 connected to the side of the atomizing spray head 22, a spare spray frame 24 connected to the front end of the telescopic rod 23, and a drive pipe 25 connected to the side end of the water supply pipe 13. The water collecting sleeve 14 is fitted with the drive pipe 25, and the drive pipe 25 rotates along the water collecting sleeve 14; The drive tube 25 has several water inlet holes on its side wall, and the distributed water inlet holes are connected to the water collection sleeve 14. The application replacement components include a short plate 31 fixed in the annular groove 15, a first electric telescopic rod 32 disposed on one side inside the annular groove 15, a second electric telescopic rod 33 disposed in the groove opening on the bottom surface of the annular groove 15, a spare atomizing nozzle 34 disposed at the top of the second electric telescopic rod 33, an infrared ray emitter 35 disposed on one side of the spare atomizing nozzle 34, and an infrared ray receiver 36 disposed on the other side of the spare atomizing nozzle 34. The limiting assembly includes concave side plates 41 fixed on both sides of the spare atomizing nozzle 34, an electric rotating shaft 42 disposed in the concave side plates 41, and a rectangular plate 43 connected to the electric rotating shaft 42. The limiting assembly also includes a concave mounting frame 44 disposed in the spare spray frame 24, a rotating shaft 45 disposed in the concave mounting frame 44, a cover plate 46 connected to the rotating shaft 45, and a circular opening 47 opened on the bottom surface of the spare spray frame 24. During the use of the spraying device, the ammonium fluoride absorbent is transported by the high-pressure pump 12 and delivered to the water collection jacket 14. Finally, it is sprayed out through three distributed atomizing spray nozzles 22, thus allowing the exhaust gas to enter the main body 11 of the spraying tower. At this time, the ammonium fluoride absorbent will come into full contact with the exhaust gas and directly absorb the fluorine gas. When one of the atomizing spray heads 22 becomes clogged, the pressure inside the water supply pipe 13 gradually increases. At this time, the ammonium fluoride absorbent liquid is sprayed out through the drive pipe 25. The sprayed ammonium fluoride absorbent liquid pushes the water distribution pipe 21, causing the water distribution pipe 21 to rotate on the surface of the water supply pipe 13 through the water collection sleeve 14. In this way, when clogged, the rotational spray is directly activated to achieve uniform spraying of the ammonium fluoride absorbent liquid and ensure that the ammonium fluoride absorbent liquid is in full contact with the exhaust gas. When two or three atomizing spray heads 22 become blocked, the pressure in the water supply pipe 13 continues to increase. At this time, the rotation speed of the water distribution pipe 21 increases, directly throwing the spare spray frame 24 into the annular groove 15. The spare spray frame 24 is blocked by the short plate 31. At this time, the second electric telescopic rod 33 pushes the spare atomizing spray head 34 upward. The spare atomizing spray head 34 pushes the cover plate 46, and the cover plate 46 rotates through the rotating shaft 45. The cover plate 46 is pushed open, directly pushing the spare atomizing spray head 34 into the spare spray frame 24. The rectangular plate 43 is extended and limited by the electric rotating shaft 42, and the spare atomizing spray head 34 leaves the infrared ray emission area. When the infrared emitter 35 is in the region of the infrared ray receiver 36, the infrared rays emitted by the infrared ray emitter 35 are received by the infrared ray receiver 36. At this time, the three distributed first electric telescopic rods 32 are simultaneously extended. One of the first electric telescopic rods 32 pushes the spare spray frame 24 back to its original position, and the other two first electric telescopic rods 32 push the corresponding blocked atomizing spray head 22 to reset. In this way, when the spare spray frame 24 is replaced and the pressure is normally released, when the spray is rotated, the other two blocked atomizing spray heads 22 will not be thrown out, so as to ensure uniform rotation and ensure that the ammonium fluoride absorbent liquid is in full contact with the exhaust gas.

[0022] By setting the short plate 31, when the spare spray frame 24 is thrown out but does not fully enter the annular groove 15, it will not touch the short plate 31. When the spare spray frame 24 contacts the short plate 31, the spare spray frame 24 is directly limited and at this time the spray frame 24 is located in the annular groove 15.

[0023] S2: The flue gas from the wet phosphoric acid reaction process is introduced into the spray tower to allow the flue gas to fully react with the ammonium fluoride absorbent, thus obtaining hydrofluoric acid. The hydrofluoric acid falls into the storage tank at the bottom of the spray tower by gravity. S3: The hydrofluoric acid in the storage tank is diverted to the external storage tank, and ammonia gas is introduced into the storage tank. At this time, the hydrofluoric acid reacts with the ammonia gas to produce ammonium bifluoride. The crystal precipitation device pumps the raw material out of the storage tank and performs crystallization treatment. Then, it is concentrated and evaporated to obtain ammonium bifluoride crystals, thus completing the absorption of fluorine in the wet process of phosphoric acid reaction.

[0024] The foregoing has shown and described the basic principles, main features, and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited to the above embodiments. The embodiments and descriptions in the specification are merely illustrative of the principles of the invention. Various changes and modifications can be made to the invention without departing from its spirit and scope, and all such changes and modifications fall within the scope of the present invention as claimed. The scope of protection of this invention is defined by the appended claims and their equivalents.

Claims

1. A spraying device, characterized in that, The spraying device includes a spraying tower assembly, a spraying component, an application replacement component, and a limiting component; the spraying tower assembly includes a spraying tower body, a high-pressure pump disposed on one side of the spraying tower body, a water supply pipe connected to the output end of the high-pressure pump, a water collection sleeve disposed inside the spraying tower body, and an annular groove formed inside the spraying tower body. The spray assembly includes a water distribution pipe connected to the water collection sleeve, an atomizing spray head connected to the front end of the water distribution pipe, a telescopic rod connected to the side of the atomizing spray head, a spare spray frame connected to the front end of the telescopic rod, and a drive pipe connected to the side end of the water supply pipe; the water collection sleeve and the drive pipe are fitted together, and the drive pipe rotates along the water collection sleeve. The application replacement component includes a short plate fixed in the annular groove, a first electric telescopic rod disposed on one side inside the annular groove, a second electric telescopic rod disposed in the groove opening on the bottom surface of the annular groove, a spare atomizing nozzle disposed at the top of the second electric telescopic rod, an infrared ray emitter disposed on one side of the spare atomizing nozzle, and an infrared ray receiver disposed on the other side of the spare atomizing nozzle. The limiting component includes concave side plates fixed on both sides of the spare atomizing nozzle, an electric rotating shaft disposed within the concave side plates, and a rectangular plate connected to the electric rotating shaft.

2. The spraying device as described in claim 1, characterized in that: The water collection sleeve is connected to three water distribution pipes respectively; each water distribution pipe is equipped with an atomizing spray head, telescopic rod and spare spray frame with the same structure at the front end.

3. The spraying device as described in any one of claims 1 and 2, characterized in that: The side wall of the drive tube has several water inlet holes, which are connected to the water collection sleeve.

4. The spraying device as described in claim 1, characterized in that: in, There are three first electric telescopic poles, and the three first electric telescopic poles are distributed in a ring.

5. The spraying device as described in claim 1, characterized in that: The limiting component also includes a concave mounting frame disposed within the spare spray frame, a rotating shaft disposed within the concave mounting frame, a cover plate connected to the rotating shaft, and a circular opening formed on the bottom surface of the spare spray frame.

6. The spraying device as described in claim 1, characterized in that: The nozzle of the drive pipe is directly opposite the distributed water distribution pipes, and the water jet from the drive pipe directly impacts and pushes the opposite water distribution pipes.

Images