Wet-process phosphoric acid purification equipment, regeneration method and use method
By using resin columns in wet phosphoric acid purification equipment for adsorption and decolorization, and using rapid regeneration methods, the problems of high equipment maintenance costs, long regeneration cycles and product pollution are solved, and the effects of cost reduction and pollution avoidance are achieved.
Patent Information
- Application Number
- CN202510444195.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-04-10
- Publication Date
- 2025-06-27
AI Technical Summary
The existing wet phosphoric acid purification equipment has high maintenance costs, long regeneration cycles, and the products are susceptible to sodium ions contamination.
The resin column is used as the adsorption medium, and the adsorption of the resin column is used for adsorption and decolorization, and the resin column is quickly regenerated by water washing, steam washing, cold water cooling and compressed air blow-drying.
Reduces production costs, simplifies maintenance processes, avoids sodium ion contamination of products, and improves the recovery of organic matter.
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Figure CN120204770A_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of phosphoric acid production, and more specifically, to a wet-process phosphoric acid purification device, a regeneration method and a usage method thereof. Background Art
[0002] In the purification phosphoric acid obtained by the stripping process of the wet-process purification phosphoric acid technology prepared by the solvent extraction method, due to the presence of a small amount of solvent and other organic substances, the appearance is brownish-yellow, and it is necessary to carry out analysis and decolorization treatment. On the one hand, the extractant (methyl isobutyl ketone, abbreviated as MIBK) is recovered, and on the other hand, the organic matter is removed to make the product chromaticity meet the standard.
[0003] The existing process first uses a graphite rectification column to analyze the purified phosphoric acid to separate and recover most of the organic solvents (i.e., extractants) in the acid, and then uses the adsorption of activated carbon in the decolorization tower to remove the remaining organic substances in the phosphoric acid. This process has high equipment investment costs for graphite towers, consumes a large amount of steam during operation, and the inspection, repair and maintenance of graphite equipment are complex. At the same time, the activated carbon regeneration operation process of the decolorization tower is long, the regeneration cycle is long, and sodium hydroxide is required during regeneration, resulting in problems such as the product being easily contaminated by sodium ions. In addition, the equipment maintenance cost of this process is high.
[0004] In summary, how to solve the problems of high maintenance cost, long regeneration cycle of wet-process phosphoric acid purification equipment and sodium ion pollution of products is an urgent problem to be solved by those skilled in the art at present. Summary of the Invention
[0005] In view of this, the purpose of the present invention is to provide a wet-process phosphoric acid purification device that uses a resin column as an adsorption medium, and uses the adsorption of the resin column to adsorb and decolorize the product, and regenerates the resin column by flushing, which is simple to maintain, has a low usage cost, and during the regeneration process, sodium hydroxide is not required, avoiding sodium ion pollution of the product.
[0006] Another object of the present invention is to provide a regeneration method applied to the above wet-process phosphoric acid purification device. Through water washing and steam washing, the organic matter in the resin column is quickly precipitated, and cold water cooling and compressed air drying are used to achieve the rapid regeneration of the resin column.
[0007] Another object of the present invention is to provide a usage method applied to the above wet-process phosphoric acid purification device. The resin columns in multiple adsorption tanks are regenerated in turn to avoid equipment shutdown, and the adsorption tanks in the non-regeneration state can be used in series to achieve multi-stage adsorption of raw materials and ensure the purification effect of raw materials.
[0008] In order to achieve the above object, the present invention provides the following technical solutions:
[0009] A wet-process phosphoric acid purification device, comprising:
[0010] Adsorption tank, with a raw material discharge port and a flushing agent filling port provided at its top, and a raw material filling port and a flushing agent discharge port provided at its bottom. A resin column is filled in the adsorption tank for adsorbing organic substances in the raw material;
[0011] Heat exchanger, connected in series to the flushing agent discharge port for cooling the discharged material at the flushing agent discharge port.
[0012] Preferably, there are N adsorption tanks, N≥3, N is a positive integer, and the N adsorption tanks are arranged in a form of annular series connection, and a first stop valve is provided in the series pipeline;
[0013] The raw material filling ports of all the adsorption tanks are communicated with the main raw material filling pipeline, and a second stop valve is provided between the raw material filling port and the main raw material filling pipeline;
[0014] The raw material discharge ports of all the adsorption tanks are communicated with a buffer tank for storing the produced raw material, and a third stop valve is provided between the raw material discharge port and the buffer tank.
[0015] Preferably, the flushing agent discharge ports of all the adsorption tanks are communicated with the heat exchanger, and a fourth stop valve is provided between the flushing agent discharge port and the heat exchanger;
[0016] The flushing agent filling ports of all the adsorption tanks are communicated with a flushing pipeline for supplying the flushing agent, and a stop valve is provided between the flushing agent filling port and the flushing pipeline.
[0017] Preferably, the flushing agent filling port includes a gas filling port and a flushing liquid filling port;
[0018] The gas filling ports of all the adsorption tanks are respectively communicated with the main gas pipeline for gas source supply, and a fifth stop valve is provided between the gas filling port and the main gas pipeline;
[0019] The flushing liquid filling ports of all the adsorption tanks are communicated with the main flushing liquid pipeline for supplying the flushing liquid, and a sixth stop valve is provided between the flushing liquid filling port and the main flushing liquid pipeline.
[0020] Preferably, the flushing agent filling port is respectively communicated with the main gas pipeline for gas source supply and the main flushing liquid pipeline for supplying the flushing liquid through a reversing valve.
[0021] Preferably, the inlet end of the main gas pipeline is communicated with the steam pipeline and the compressed air pipeline in parallel, and a seventh stop valve is provided between the main gas pipeline and the steam pipeline and the compressed air pipeline respectively.
[0022] Preferably, the inlet end of the main flushing liquid pipeline is connected to the cold water pipeline and the hot water pipeline in parallel, and eighth stop valves are arranged between the main flushing liquid pipeline and the cold water pipeline and the hot water pipeline respectively.
[0023] Preferably, a phase separation tank is arranged at the outlet end of the heat exchanger for phase separation of the discharge from the heat exchanger.
[0024] A method for equipment regeneration, applied to the wet-process phosphoric acid purification equipment described in any one of the above, includes the following steps:
[0025] Control the raw material filling port and the raw material discharge port to be closed, control the flushing material filling port to fill with hot water, wash the resin column, and the wastewater is discharged through the flushing material discharge port;
[0026] Control the flushing material filling port to fill with high-temperature steam, scour the resin column, and the waste gas is discharged through the flushing material discharge port;
[0027] Control the flushing material filling port to fill with cold water, wash the resin column, and the wastewater is discharged through the flushing material discharge port;
[0028] Control the flushing material filling port to fill with compressed air, dry the resin column, and the waste gas is discharged through the flushing material discharge port;
[0029] Control the wastewater or the waste gas discharged from the flushing material discharge port to enter the heat exchanger, cool the wastewater, and condense the waste gas.
[0030] A usage method, applied to the wet-process phosphoric acid purification equipment described in any one of the above, includes the following steps:
[0031] Control the raw material filling port and the raw material discharge port of the Yth adsorption tank to be closed, and control the flushing material filling port of the adsorption tank to inject flushing material, and control the flushing material discharge port of the adsorption tank to discharge flushing waste for regenerating the resin column in the adsorption tank, where Y≤N;
[0032] Control the raw material filling port of the Zth adsorption tank to fill with raw material, and control the raw material discharge port of the Xth adsorption tank to discharge raw material; when Y<N, X + 1 = Y = Z - 1; when Y = N, X + 1 = Y, Z = 1; when Y = 1, X = N, Z = Y + 1.
[0033] The wet-process phosphoric acid purification equipment provided by the present invention, compared with the prior art, has at least the following beneficial effects:
[0034] Using a resin column as the adsorption material, the pores in the resin column are used to adsorb the organic substances in phosphoric acid, thereby achieving separation and decolorization. Moreover, the resin column can be regenerated, which can effectively reduce the production cost. In addition, compared with the traditional purification method of a graphite rectification column, sodium hydroxide is not required during the regeneration of the resin column, so the product is prevented from being contaminated by sodium ions.
[0035] At the same time, a flushing material filling port and a flushing material discharge port are integrated in the adsorption tank, which can flush and regenerate the resin column. In addition, a heat exchanger structure is added, which can cool and collect the organic substances flushed out, improve the recovery rate of the organic substances, and reduce emissions.
[0036] The equipment regeneration method provided by the present invention is applied to the above wet-process phosphoric acid purification equipment. The resin column is rinsed with hot water to remove the raw materials on the surface of the resin column, and the resin column is preliminarily heated to promote the precipitation of internal organic substances. Then, steam scouring is used to heat the resin column for the second time to promote the rapid precipitation of internal organic substances, which are discharged with the steam flow. Subsequently, the resin column is cooled with cold water and dried with compressed air to realize the regeneration of the resin column.
[0037] The usage method provided by the present invention is applied to the above wet-process phosphoric acid purification equipment. During the production process, the saturated resin column can be regenerated without stopping the machine, and the normal use of other adsorption tanks is not affected. Moreover, the adsorption tanks in the non-regeneration state can be used in series to increase the adsorption stage of the raw materials and ensure the purification effect. BRIEF DESCRIPTION OF THE DRAWINGS
[0038] In order to more clearly illustrate the technical solutions in the embodiments of the present invention or the prior art, the following will briefly introduce the drawings required for use in the description of the embodiments or the prior art. Obviously, the following drawings are only the embodiments of the present invention. For those of ordinary skill in the art, other drawings can be obtained according to the provided drawings without creative efforts.
[0039] Figure 1 It is a schematic diagram of the wet-process phosphoric acid purification equipment provided by the present invention;
[0040] Figure 2 It is a schematic diagram of another embodiment of the wet-process phosphoric acid purification equipment provided by the present invention;
[0041] Figure 3 It is a schematic flow chart of the equipment regeneration method provided by the present invention;
[0042] Figure 4 It is a schematic flow chart of the usage method provided by the present invention.
[0043] In the figure:
[0044] 1. Adsorption tank; 11. Raw material filling port; 12. Gas filling port; 13. Flushing liquid filling port; 14. Raw material discharge port; 15. Flushing material discharge port;
[0045] 1a. First adsorption tank; 1b. Second adsorption tank; 1c. Third adsorption tank;
[0046] 2. Buffer tank; 3. Heat exchanger; 4. Phase separation tank; 5. Solvent recovery tank; 6. Main raw material filling pipeline; 7. Main gas pipeline; 8. Main flushing liquid pipeline;
[0047] 9a. First stop valve; 9b. Second stop valve; 9c. Third stop valve; 9d. Fourth stop valve; 9e. Fifth stop valve; 9f. Sixth stop valve; 9g. Seventh stop valve; 9h. Eighth stop valve. Detailed implementation manners
[0048] Next, the technical solutions in the embodiments of the present invention will be clearly and completely described in conjunction with the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present invention.
[0049] The core of the present invention is to provide a wet-process phosphoric acid purification device, which uses a resin column as an adsorption medium, combines the two processes of desorption and adsorption decolorization into one, uses the adsorption effect of the resin column to perform adsorption decolorization on the product, and regenerates the resin column by flushing, with simple maintenance, low use cost, and during the regeneration process, sodium hydroxide is not required, avoiding sodium ion contamination of the product.
[0050] The core of the present invention is to provide a regeneration method applied to the above-mentioned wet-process phosphoric acid purification device. Through water washing and steam washing, organic substances in the resin column are quickly precipitated, and cold water cooling and compressed air drying are used to achieve rapid regeneration of the resin column.
[0051] The core of the present invention is to provide a usage method applied to the above-mentioned wet-process phosphoric acid purification device. The resin columns in multiple adsorption tanks are regenerated in turn, avoiding equipment shutdown, and the adsorption tanks in the non-regeneration state can be used in series to achieve multi-stage adsorption of raw materials and ensure the purification effect of raw materials.
[0052] Please refer to Figure 1 , a wet-process phosphoric acid purification device, comprising:
[0053] Adsorption tank 1, with a raw material discharge port 14 and a flushing material filling port at the top, and a raw material filling port 11 and a flushing material discharge port 15 at the bottom. The adsorption tank 1 is filled with a resin column for adsorbing organic substances in the raw material;
[0054] A heat exchanger 3 is connected in series to the flush discharge port 15 for cooling the discharge from the flush discharge port 15.
[0055] By filling the resin column in the adsorption tank 1, the large pore size adsorption in the resin column is used to adsorb and decolorize the organic substances in phosphoric acid, reducing the production cost. Moreover, by flushing the resin column for regeneration, the regeneration process is simple, the regeneration cycle is short, and no new metal ions need to be introduced during the regeneration process, avoiding secondary pollution to the finished acid.
[0056] Meanwhile, the adsorption tank 1 is provided with a raw material filling port 11, a raw material discharge port 14, a flush filling port, and a flush discharge port 15. By closing the flush filling port and the flush discharge port 15, normal production operations can be carried out. That is, raw materials such as phosphoric acid containing organic substances are injected from the raw material filling port 11 at the bottom of the adsorption tank 1, gradually submerging the resin column in the adsorption tank 1, and then the resin column adsorbs the organic substances in the raw materials, and the adsorbed raw materials are discharged from the raw material discharge port 14 at the top of the adsorption tank 1;
[0057] After closing the raw material filling port 11 and the raw material discharge port 14, the flush is filled from the flush filling port at the top of the adsorption tank 1, and the flush flushes the resin column from top to bottom. During this process, there is no need to convert the form of the adsorption tank 1, so the flushing operation is relatively simple. Moreover, compared with traditional graphite rectification towers and activated carbon adsorption methods, the method of using resin column adsorption has a lower production cost and a shorter regeneration cycle, which is beneficial to reducing the overall production efficiency and production cost.
[0058] Moreover, a heat exchanger 3 is connected in series downstream of the flush discharge port 15, which can cool or liquefy the waste generated by flushing, promote the liquefaction and precipitation of the organic substances in the waste, facilitate collection, reduce emissions, and contribute to environmental protection.
[0059] In some embodiments, there are N adsorption tanks 1, N≥3, N is a positive integer, and the N adsorption tanks 1 are arranged in a form of annular series connection, and a first stop valve 9a is provided in the series pipeline;
[0060] The raw material filling ports 11 of all the adsorption tanks 1 are communicated with the main raw material filling pipeline 6, and a second stop valve 9b is provided between the raw material filling port 11 and the main raw material filling pipeline 6;
[0061] The raw material discharge ports 14 of all the adsorption tanks 1 are communicated with the buffer tank 2 for storing the produced raw materials, and a third stop valve 9c is provided between the raw material discharge port 14 and the buffer tank 2.
[0062] Such as Figure 2As shown, N groups of adsorption tanks 1 are used in combination, such as the first adsorption tank 1a, the second adsorption tank 1b and the third adsorption tank 1c are used in combination. During use, the raw material filling port 11 and the raw material discharge port 14 of the first adsorption tank 1a, the second adsorption tank 1b and the third adsorption tank 1c are connected end to end in sequence, forming a ring structure as a whole;
[0063] During use, three groups of adsorption tanks 1 can be used in parallel, that is, the raw material is discharged into the buffer tank 2 after the first-stage adsorption; or three groups of adsorption tanks 1 can be used in series, that is, the raw material is discharged into the buffer tank 2 after the third-stage adsorption, thereby increasing the adsorption level of the raw material and helping to improve the purification effect of the raw material.
[0064] At the same time, during use, when the resin column in one group of adsorption tanks 1 is saturated, a single group of adsorption tanks 1 can be selected for flushing to achieve regeneration of the internal resin column, while the remaining two groups are used in series or in parallel to perform two-stage or single-stage adsorption of raw materials, thereby achieving non-stop regeneration of the resin column and improving production efficiency;
[0065] In the above production method, when the resin column in the adsorption tank 1 is regenerated, when the remaining adsorption tanks 1 are used in series, the saturation time of the resin columns in the adsorption tanks 1 at different adsorption levels is different, so different adsorption tanks 1 can be regenerated in turn, and in the process of rotation, the adsorption level of the same adsorption tank 1 changes, and the adsorption levels and order experienced by each group of adsorption tanks 1 are the same, so the regeneration interval period of each group of adsorption tanks 1 is equal, which is convenient for realizing automatic control.
[0066] In some embodiments, the flushing material outlets 15 of all adsorption tanks 1 are connected to the heat exchanger 3, and a fourth stop valve 9d is provided between the flushing material outlet 15 and the heat exchanger 3;
[0067] The flushing material filling ports of all adsorption tanks 1 are connected to the flushing pipeline for supplying the flushing material, and a stop valve is provided between the flushing material filling port and the flushing pipeline.
[0068] like Figure 2 As shown, each group of adsorption tanks 1 is connected to the flushing pipeline and the heat exchanger 3, that is, any group of adsorption tanks 1 can be flushed separately to regenerate the resin columns inside, and the regeneration process will not affect the normal operation of the remaining adsorption tanks 1.
[0069] In some embodiments, the flushing material filling port includes a gas filling port 12 and a flushing liquid filling port 13;
[0070] The gas filling ports 12 of all adsorption tanks 1 are respectively connected to the gas main pipeline 7 for gas source supply, and a fifth stop valve 9e is provided between the gas filling port 12 and the gas main pipeline 7;
[0071] The flushing liquid filling ports 13 of all adsorption tanks 1 are all communicated with the main flushing liquid pipeline 8 for flushing liquid supply, and a sixth stop valve 9f is arranged between the flushing liquid filling port 13 and the main flushing liquid pipeline 8.
[0072] As Figure 1 shown, the flushing material filling ports at the top of the adsorption tank 1 include two groups of independent flushing liquid filling ports 13 and gas filling ports 12, and the flushing liquid filling ports 13 and gas filling ports 12 of each group of adsorption tanks 1 are respectively communicated with the corresponding main flushing liquid pipeline 8 and main gas pipeline 7, so as to realize the separate supply of the flushing gas and the flushing liquid, and they will not interfere with each other.
[0073] In some embodiments, the flushing material filling ports are respectively communicated with the main gas pipeline 7 supplied by the gas source and the main flushing liquid pipeline 8 for flushing liquid supply through a reversing valve.
[0074] Only one group of flushing material filling ports is arranged at the top of the adsorption tank 1, and the main gas pipeline 7 and the main flushing liquid pipeline 8 are communicated through a three-position three-way reversing valve, and the corresponding main pipeline can be selectively communicated according to the filling situation of the flushing material.
[0075] In some embodiments, the inlet end of the main gas pipeline 7 is communicated with the steam pipeline and the compressed air pipeline in parallel, and a seventh stop valve 9g is arranged between the main gas pipeline 7 and the steam pipeline and the compressed air pipeline.
[0076] As Figure 2 shown, the inlet end of the main gas pipeline 7 is simultaneously connected to the steam pipeline and the compressed air pipeline, and seventh stop valves 9g are arranged at the output ends of the steam pipeline and the compressed air pipeline. According to the gas supply demand of the main gas pipeline 7, the steam pipeline or the compressed air pipeline can be selectively conducted.
[0077] In some embodiments, the inlet end of the main flushing liquid pipeline 8 is communicated with the cold water pipeline and the hot water pipeline in parallel, and an eighth stop valve 9h is arranged between the main flushing liquid pipeline 8 and the cold water pipeline and the hot water pipeline.
[0078] As Figure 2 shown, the inlet end of the main flushing liquid pipeline 8 is simultaneously connected to the cold water pipeline and the hot water pipeline, and eighth stop valves 9h are arranged at the output ends of the cold water pipeline and the hot water pipeline. According to the liquid supply demand of the main flushing liquid pipeline 8, the hot water pipeline or the cold water pipeline can be selectively conducted.
[0079] In some embodiments, a phase separation tank 4 is arranged at the outlet end of the heat exchanger 3 for phase separation of the discharged materials of the heat exchanger 3.
[0080] As Figure 1 and Figure 2As shown, a phase separation tank 4 is provided at the output end of the heat exchanger 3, so that the waste liquid cooled or condensed by the heat exchanger 3 is phase-separated in the phase separation tank 4, and then the organic substances and raw materials are separated, and the organic substances can be recovered into the solvent recovery tank 5.
[0081] In addition to the wet-process phosphoric acid purification equipment disclosed in the above various embodiments, the present invention also provides an equipment regeneration method applied to the above wet-process phosphoric acid purification equipment and method, including the following steps:
[0082] Control the raw material filling port 11 and the raw material discharge port 14 to be closed, control the flushing material filling port to fill hot water, wash the resin column, and the waste water is discharged through the flushing material discharge port 15;
[0083] Control the flushing material filling port to fill high-temperature steam, scour the resin column, and the waste gas is discharged through the flushing material discharge port 15;
[0084] Control the flushing material filling port to fill cold water, wash the resin column, and the waste water is discharged through the flushing material discharge port 15;
[0085] Control the flushing material filling port to fill compressed air, dry the resin column, and the waste gas is discharged through the flushing material discharge port 15;
[0086] Control the waste water or waste gas discharged from the flushing material discharge port 15 to enter the heat exchanger 3, cool the waste water, and condense the waste gas.
[0087] As Figure 3 shown, when regenerating the resin column, first use hot water to wash the resin column to wash the raw materials attached to the surface of the resin column. And during the washing process, compared with cold water, hot water has a higher solubility of raw materials, which can ensure the washing cleanliness of the resin column. At the same time, hot water can heat the resin column once, promoting the precipitation and volatilization of organic substances inside;
[0088] Then, use high-temperature steam to heat and scour the resin column, that is, perform secondary heating on the resin column to raise its temperature again, increase the precipitation amount and volatility of organic substances, and the volatilized organic substances can be discharged with the steam flow;
[0089] Continue to use cold water to wash the resin column, that is, cool the resin column to avoid a decrease in the adsorption efficiency of organic substances during the subsequent production process due to high temperature;
[0090] Finally, use compressed air to dry the resin column to ensure its adsorption efficiency for organic substances during the production process and complete the regeneration of the resin column.
[0091] In addition to the wet-process phosphoric acid purification equipment disclosed in the above various embodiments, the present invention also provides a usage method applied to the above wet-process phosphoric acid purification equipment and method, including the following steps:
[0092] Control the closure of the raw material filling port 11 and the raw material discharge port 14 of the Y-level adsorption tank 1, and control the injection of the flushing material through the flushing material filling port of the adsorption tank 1, and control the discharge of the flushing waste through the flushing material discharge port 15 of the adsorption tank 1 for the regeneration of the resin column in the adsorption tank 1, where ;
[0093] Control the filling of raw materials through the raw material filling port 11 of the Z-level adsorption tank 1, and control the discharge of raw materials through the raw material discharge port 14 of the X-level adsorption tank 1; when time, ; when time, , ; when time, , .
[0094] As Figure 2 and Figure 4 shown, when the resin column in one of the groups of adsorption tanks 1 is saturated, taking the saturation of the resin column in the first adsorption tank 1a as an example, at this time, the regeneration of the resin column in the first adsorption tank 1a is carried out, and the method adopts the above-mentioned equipment regeneration method, and the remaining second adsorption tank 1b and third adsorption tank 1c can be used in parallel or in series. Taking the series connection of the two as an example, the raw materials enter through the raw material filling port 11 of the second adsorption tank 1b, are adsorbed by the internal resin column, and are discharged through the raw material discharge port 14 of the second adsorption tank 1b. Then the raw materials enter through the raw material filling port 11 of the third adsorption tank 1c, are adsorbed again by the internal resin column, and finally are discharged through the raw material discharge port 14 of the third adsorption tank 1c. During this process, the second adsorption tank 1b serves as the primary adsorption tank, and the third adsorption tank 1c serves as the secondary adsorption tank. Therefore, the resin column in the second adsorption tank 1b is preferentially saturated. At this time, the regeneration is switched to the second adsorption tank 1b, and the third adsorption tank 1c serves as the primary adsorption tank, and the first adsorption tank 1a serves as the secondary adsorption tank, thereby realizing the rotation regeneration of the adsorption tank 1.
[0095] In this specification, the various embodiments are described in a progressive manner. The key points of each embodiment are the differences from other embodiments. For the same and similar parts between the various embodiments, reference can be made to each other.
[0096] The above has introduced in detail the wet-process phosphoric acid purification equipment, regeneration method and usage method provided by the present invention. Specific examples are used in this article to elaborate on the principle and implementation manner of the present invention. The description of the above embodiments is only used to help understand the method and its core idea of the present invention. It should be noted that for those of ordinary skill in the art in this technical field, without departing from the principle of the present invention, several improvements and modifications can still be made to the present invention, and these improvements and modifications also fall within the protection scope of the claims of the present invention.
Claims
1. A wet phosphoric acid purification device, characterized in that: include: An adsorption tank (1) is provided with a raw material discharge port (14) and a flushing material filling port at the top, and a raw material filling port (11) and a flushing material discharge port (15) at the bottom. The adsorption tank (1) is filled with a resin column for adsorbing organic matter in the raw material; A heat exchanger (3) is connected in series to the flushing material discharge port (15) and is used to cool the discharge from the flushing material discharge port (15).
2. The wet phosphoric acid purification equipment according to claim 1, characterized in that: The adsorption tanks (1) are in N groups, N≥3, N is a positive integer, and the N groups of adsorption tanks (1) are arranged in a circular series, and a first stop valve (9a) is provided in the series pipeline; The raw material filling ports (11) of all the adsorption tanks (1) are connected to the raw material filling main pipeline (6), and a second stop valve (9b) is provided between the raw material filling ports (11) and the raw material filling main pipeline (6); The raw material discharge ports (14) of all the adsorption tanks (1) are connected to a buffer tank (2) for storing output raw materials, and a third stop valve (9c) is provided between the raw material discharge ports (14) and the buffer tank (2).
3. The wet phosphoric acid purification equipment according to claim 2, characterized in that: The flushing material discharge ports (15) of all the adsorption tanks (1) are in communication with the heat exchanger (3), and a fourth stop valve (9d) is provided between the flushing material discharge ports (15) and the heat exchanger (3); The flushing material filling ports of all the adsorption tanks (1) are connected to a flushing pipeline for supplying flushing material, and a stop valve is provided between the flushing material filling port and the flushing pipeline.
4. The wet phosphoric acid purification equipment according to claim 3, characterized in that: The flushing material filling port comprises a gas filling port (12) and a flushing liquid filling port (13); The gas filling ports (12) of all the adsorption tanks (1) are respectively connected to a gas main pipeline (7) for gas source supply, and a fifth stop valve (9e) is provided between the gas filling port (12) and the gas main pipeline (7); The flushing liquid filling ports (13) of all the adsorption tanks (1) are connected to a flushing liquid main pipeline (8) for supplying flushing liquid, and a sixth stop valve (9f) is provided between the flushing liquid filling ports (13) and the flushing liquid main pipeline (8).
5. The wet phosphoric acid purification equipment according to claim 4, characterized in that: The flushing material filling port is connected to a gas main pipeline (7) for supplying a gas source and a flushing liquid main pipeline (8) for supplying a flushing liquid through a reversing valve.
6. The wet phosphoric acid purification equipment according to claim 4, characterized in that: The inlet end of the gas main pipeline (7) is connected to a steam pipeline and a compressed air pipeline in parallel, and a seventh stop valve (9g) is provided between the gas main pipeline (7) and the steam pipeline and the compressed air pipeline.
7. The wet phosphoric acid purification equipment according to claim 4, characterized in that: The inlet end of the flushing liquid main pipeline (8) is connected to the cold water pipeline and the hot water pipeline in parallel, and an eighth stop valve (9h) is provided between the flushing liquid main pipeline (8) and the cold water pipeline and the hot water pipeline.
8. The wet phosphoric acid purification equipment according to any one of claims 2 to 7, characterized in that: The outlet end of the heat exchanger (3) is provided with a phase separation tank (4) for performing phase separation on the discharge of the heat exchanger (3).
9. A device regeneration method, characterized in that: The wet phosphoric acid purification equipment according to any one of claims 1 to 8 comprises the following steps: Controlling the raw material filling port (11) and the raw material discharge port (14) to be closed, controlling the flushing material filling port to be filled with hot water to rinse the resin column, and discharging waste water through the flushing material discharge port (15); Controlling the flushing material filling port to add high-temperature steam to flush the resin column, and exhaust gas is discharged through the flushing material discharge port (15); Controlling the flushing material filling port to add cold water to rinse the resin column, and discharging waste water through the flushing material discharge port (15); Controlling the flushing material filling port to fill with compressed air to dry the resin column, and exhausting the waste gas through the flushing material discharge port (15); The waste water or the waste gas discharged from the flushing material discharge port (15) is controlled to enter the heat exchanger (3), so as to cool the waste water and condense the waste gas.
10. A method of use, characterized in that: The wet phosphoric acid purification equipment as claimed in any one of claims 2 to 8 comprises the following steps: Controlling the raw material filling port (11) and the raw material discharge port (14) of the adsorption tank (1) of the Yth stage to be closed, controlling the flushing material filling port of the adsorption tank (1) to inject flushing material, and controlling the flushing material discharge port (15) of the adsorption tank (1) to discharge flushing waste for regeneration of the resin column in the adsorption tank (1), wherein Y≤N; The raw material filling port (11) of the Z-th adsorption tank (1) is controlled to fill the raw material, and the raw material discharge port (14) of the X-th adsorption tank (1) is controlled to discharge the raw material; when Y<N, X+1=Y=Z-1; when Y=N, X+1=Y, Z=1; when Y=1, X=N, Z=Y+1.