Process device for preparing iron phosphate by recycling waste phosphoric acid
By designing a process device that utilizes chemical reactions and separation processes to convert waste phosphoric acid into iron phosphate, the problem of difficult treatment and resource utilization of waste phosphoric acid has been solved. This has enabled the efficient preparation of high-value iron phosphate, meeting the market demand for electronic-grade phosphoric acid and reducing disposal costs.
Patent Information
- Application Number
- CN202520395841.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2025-03-07
- Publication Date
- 2026-01-23
- Estimated Expiration
- 2035-03-07
AI Technical Summary
Existing technologies are insufficient for the effective treatment and resource utilization of phosphoric acid-containing waste liquids, resulting in resource waste and increased disposal costs, while the growing demand for electronic-grade phosphoric acid remains unmet.
A process device was designed, comprising a ferrous phosphate reaction device, a ferric phosphate reaction device, a pH adjustment device, a plate and frame filter press, a washing device, a centrifugal separation device, a drying device, a pulverizing device, and a packaging device. Waste phosphoric acid is converted into ferric phosphate through chemical reactions and separation processes. Chemical reagents such as hydrogen peroxide, ferrous sulfate, and ammonia are used for precipitation and pH adjustment to achieve the preparation of ferric phosphate.
This approach enables the resource utilization of waste phosphoric acid, producing high-value iron phosphate products that meet market demand, reduce disposal costs, and improve resource utilization.
Smart Images
Figure CN223818685U_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The utility model relates to a hazardous waste resource technology field especially relates to a process device for preparing ferrophosphorus from waste phosphoric acid. BACKGROUND
[0002] In the industrial production process of phosphoric acid production, chemical etching, electrochemical polishing, phosphating with phosphoric acid, chemical cleaning, pesticide production, etc., a large amount of phosphoric acid-containing waste liquid is generated every year. These waste liquids often contain high concentrations of phosphoric acid, sulfuric acid, nitric acid, acetic acid, hydrofluoric acid and various metal impurities, etc., and belong to hazardous waste. In recent years, driven by international situation and economic development, China's electronic industry has developed rapidly, and the development of semiconductor industry has been included in the national "14th Five-Year Plan". The demand for related chemicals is increasing year by year, and as a key chemical, the demand for electronic-grade phosphoric acid is growing significantly. Electronic-grade phosphoric acid, also known as ultra-high purity phosphoric acid, is mainly used for cleaning and etching of chips. Its cleanliness and purity have a great influence on the performance, reliability and yield of electronic components. For example, if the wafer is contaminated by impurities during processing, the yield of integrated circuits (IC) will decrease by about 50%. Therefore, in order to ensure the reliability of the product and obtain high-yield large-scale integrated circuits, the electronic industry must use high-purity electronic-grade phosphoric acid for cleaning and continuously supplement new electronic-grade phosphoric acid to the production process. With the increasing scale of integrated circuits year by year, the amount of phosphoric acid-containing waste liquid is increasing.
[0003] Ferrophosphorus is formed by the reaction of iron salt solution and phosphoric acid solution, and its upstream is the production raw material of ferrophosphorus. In the early stage, ferrophosphorus was used in the fields of ceramic glass, agriculture, steel and surface passivation, etc. With the in-depth research and the emergence and development of new energy vehicles, lithium iron phosphate battery has become the most important downstream industry in the ferrophosphorus industry chain. With the gradual reduction of the subsidy policy of new energy vehicles by the state policy, lithium iron phosphate battery with more cost advantage will occupy a larger market share, and the market demand will continue to rise. Therefore, the market demand for ferrophosphorus will continue to expand. The value-added of phosphoric acid is high, and simple neutralization disposal not only increases the disposal cost but also wastes a large amount of phosphorus resources. The use of waste phosphoric acid to prepare ferrophosphorus realizes the goal of turning waste into treasure. UTILITY MODEL CONTENTS
[0004] The utility model aims at: in order to solve the problem in the background art, the utility model provides a process device for preparing ferrophosphorus from waste phosphoric acid, which is simple in structure, safe in preparation process, and realizes the goal of turning waste into treasure.
[0005] In order to achieve the above-mentioned purpose, the utility model adopts the following technical scheme:
[0006] A process apparatus for preparing ferric phosphate from waste phosphoric acid includes, from top to bottom, a ferrous reaction device, a ferric phosphate reaction device, a pH adjustment device, a plate and frame filter press, a cleaning device, a centrifugal separation device, a drying device, a pulverizing device, and a packaging device. The ferrous reaction device is equipped with a hydrogen peroxide dosing port and a ferrous sulfate solution dosing port. The ferric phosphate reaction device is equipped with a waste phosphoric acid dosing port at its upper part. The pH adjustment device is equipped with an ammonia dosing port at its upper part. The cleaning device is equipped with a deionized water dosing port and an ethanol dosing port at its upper end.
[0007] As a further description of the above technical solution:
[0008] Liquid flow meters are installed on the hydrogen peroxide dosing port, ferrous sulfate solution dosing port, waste phosphoric acid dosing port, ammonia dosing port, deionized water dosing port, and ethanol dosing port.
[0009] As a further description of the above technical solution:
[0010] The upper end of the ferrous reaction device, the ferric phosphate reaction device, and the pH adjustment device are all equipped with a stirring paddle, and the pH adjustment device is equipped with a pH meter inside.
[0011] As a further description of the above technical solution:
[0012] The ferrous reactor is equipped with a cooling water circulation device, which, together with the outer wall of the ferrous reactor, forms a cooling water circulation chamber. A coolant inlet is provided on the side wall of the cooling water circulation chamber, and a coolant outlet is provided at the bottom of the cooling water circulation chamber.
[0013] As a further description of the above technical solution:
[0014] The ferric phosphate reactor is equipped with a hot water circulation device, which, together with the outer wall of the ferric phosphate reactor, forms a hot water circulation chamber. A hot water inlet is provided on the side wall of the hot water circulation chamber, and a hot water outlet is provided at the bottom of the hot water circulation chamber.
[0015] As a further description of the above technical solution:
[0016] The output end of the ferrous reaction device is equipped with a first pump, the output end of which is connected to the upper part of the ferric phosphate reaction device. The output end of the ferric phosphate reaction device is equipped with a second pump, the output end of which is connected to the upper part of the pH adjustment device. The output end of the pH adjustment device is equipped with a third pump, the output end of which is connected to the input end of the plate and frame filter press. The output end of the cleaning device is equipped with a fourth pump, the output end of which is connected to the inlet of the centrifugal separation device.
[0017] As a further description of the above technical solution:
[0018] The plate and frame filter press is equipped with a first conveyor belt at the slag outlet at the lower end and the washing device at the upper end. The centrifugal separation device outlet and the drying device inlet are equipped with a second conveyor belt. The drying device outlet and the pulverizing device inlet are equipped with a third conveyor belt. The pulverizing device outlet and the packaging device inlet are equipped with a fourth conveyor belt.
[0019] In summary, due to the adoption of the above technical solution, the beneficial effects of this utility model are:
[0020] In this invention, ferrous sulfate is prepared using ferrous sulfate and hydrogen peroxide, and ferric sulfate is prepared by reacting waste phosphoric acid with ferric sulfate, using ammonia as a precipitant. Through independent research and development of this device, the technology for preparing ferric phosphate has been mastered, turning waste into treasure and enabling the resource-based research of waste phosphoric acid to produce high-value ferric phosphate. Attached Figure Description
[0021] Figure 1 This is a schematic diagram of the process flow of a process device for preparing ferric phosphate from waste phosphoric acid, as proposed in this utility model.
[0022] Legend:
[0023] 1. Ferrous iron reaction apparatus; 2. Ferric phosphate reaction apparatus; 3. pH adjustment apparatus; 4. Plate and frame filter press; 5. Cleaning apparatus; 6. Centrifugal separation apparatus; 7. Drying apparatus; 8. Crushing apparatus; 9. Packaging apparatus; 10. Hydrogen peroxide dosing port; 11. Ferrous sulfate solution dosing port; 12. Waste phosphoric acid dosing port; 13. Ammonia dosing port; 14. Deionized water dosing port; 15. Ethanol dosing port; 16. First pump; 17. Second pump; 18. Third pump; 19. First conveyor belt; 20. Fourth pump; 21. Second conveyor belt; 22. Third conveyor belt; 23. Fourth conveyor belt. Detailed Implementation
[0024] The technical solutions of the present utility model will be clearly and completely described below with reference to the accompanying drawings of the embodiments. Obviously, the described embodiments are only some embodiments of the present utility model, and not all embodiments. Based on the embodiments of the present utility model, all other embodiments obtained by those skilled in the art without creative effort are within the protection scope of the present utility model.
[0025] Please see Figure 1This utility model provides a technical solution: a process device for preparing ferric phosphate from waste phosphoric acid, comprising, from top to bottom, a ferrous reaction device 1, a ferric phosphate reaction device 2, a pH adjustment device 3, a plate and frame filter press 4, a cleaning device 5, a centrifugal separation device 6, a drying device 7, a pulverizing device 8, and a packaging device 9. The ferrous reaction device 1 is provided with a hydrogen peroxide dosing port 10 and a ferrous sulfate solution dosing port 11. The ferric phosphate reaction device 2 is provided with a waste phosphoric acid dosing port 12 at its upper part. The pH adjustment device 3 is provided with an ammonia dosing port 13 at its upper part. The cleaning device 5 is provided with a deionized water dosing port 14 and an ethanol dosing port 15 at its upper end.
[0026] Specifically, such as Figure 1 As shown, liquid flow meters are installed on hydrogen peroxide dosing port 10, ferrous sulfate solution dosing port 11, waste phosphoric acid dosing port 12, ammonia dosing port 13, deionized water dosing port 14, and ethanol dosing port 15. Stirring paddles are installed at the top of ferrous reaction device 1, ferric phosphate reaction device 2, and pH adjustment device 3. A pH meter is installed inside the pH adjustment device 3.
[0027] Specifically, such as Figure 1 As shown, the ferrous reactor 1 is equipped with a cooling water circulation device. The cooling water circulation device and the outer wall of the ferrous reactor 1 enclose a cooling water circulation chamber. A coolant inlet is provided on the side wall of the cooling water circulation chamber, and a coolant outlet is provided at the bottom of the cooling water circulation chamber.
[0028] Specifically, such as Figure 1 As shown, the iron phosphate reactor 2 is equipped with a hot water circulation device. The hot water circulation device and the outer wall of the iron phosphate reactor 2 enclose a hot water circulation chamber. A hot water inlet is provided on the side wall of the hot water circulation chamber, and a hot water outlet is provided at the bottom of the hot water circulation chamber.
[0029] Specifically, such as Figure 1 As shown, the output end of the ferrous phosphate reaction device 1 is equipped with a first pump 16, the output end of the first pump 16 is connected to the upper part of the ferric phosphate reaction device 2, the output end of the ferric phosphate reaction device 2 is equipped with a second pump 17, the output end of the second pump 17 is connected to the upper part of the pH adjustment device 3, the output end of the pH adjustment device 3 is equipped with a third pump 18, the output end of the third pump 18 is connected to the input end of the plate and frame filter press 4, and the output end of the cleaning device 5 is equipped with a fourth pump 20, the output end of the fourth pump 20 is connected to the inlet of the centrifugal separation device 6.
[0030] Specifically, such as Figure 1 As shown, the plate and frame filter press 4 has a first conveyor belt 19 at the lower slag outlet and the upper end of the washing device 5. The centrifugal separation device 6 has a second conveyor belt 21 at the outlet and the drying device 7 at the inlet. The drying device 7 has a third conveyor belt 22 at the outlet and the crushing device 8 at the inlet. The crushing device 8 has a fourth conveyor belt 23 at the outlet and the packaging device 9 at the inlet.
[0031] Working principle: The specific principle is as follows:
[0032] 2Fe²⁺+H2O2+ 2H⁺=2Fe³⁺+2H2O
[0033] 2Fe 3+ +2H3PO4+XH2O=2FePO4.XH2O+6H +
[0034] H + +2OH - =H2O
[0035] A certain amount of ferrous sulfate and hydrogen peroxide are added to the ferrous reaction device 1 through the hydrogen peroxide dosing port 10 and the ferrous sulfate solution dosing port 11. After the reaction has been going on for a period of time, the first pump 16 is turned on to pump the reaction solution into the ferric phosphate reaction device 2.
[0036] Then, a certain amount of waste phosphoric acid is added through waste phosphoric acid dosing port 12, and at the same time, the hot water circulation device is turned on to heat the temperature to 80°C.
[0037] After the reaction, the reaction solution is pumped into the pH adjustment device 3 by the second pump 17, and a certain amount of ammonia is added by opening the ammonia water dosing port 13 to control the pH to 2.0.
[0038] The mixture is pumped into the plate and frame filter press 4 by the third pump 18. The solid filter residue is conveyed to the cleaning device 5 by the first conveyor belt 19. The solid filter residue is cleaned by opening the ethanol dosing port 15 and the deionized water dosing port 14. After cleaning, the mixture is pumped into the centrifugal separation device 6 by the fourth pump 20. After separation, the solid ferric phosphate is conveyed to the drying device 7 by the second conveyor belt 21. After drying, the ferric phosphate is conveyed to the crushing device 8 by the third conveyor belt 22. The finished ferric phosphate is conveyed to the packaging device 9 by the fourth conveyor belt 23, realizing the resource utilization of waste phosphoric acid to produce high-value ferric phosphate.
[0039] The above description is only a preferred embodiment of the present utility model, but the protection scope of the present utility model is not limited thereto. Any equivalent substitutions or changes made by those skilled in the art within the technical scope disclosed in the present utility model, based on the technical solution and the inventive concept of the present utility model, should be included within the protection scope of the present utility model.
Claims
1. A process apparatus for the resource utilization of waste phosphoric acid to prepare ferric phosphate, characterized in that, The device includes, from top to bottom, a ferrous reaction device (1), a ferric phosphate reaction device (2), a pH adjustment device (3), a plate and frame filter press (4), a cleaning device (5), a centrifugal separation device (6), a drying device (7), a pulverizing device (8), and a packaging device (9). The ferrous reaction device (1) is equipped with a hydrogen peroxide dosing port (10) and a ferrous sulfate solution dosing port (11). The ferric phosphate reaction device (2) is equipped with a waste phosphoric acid dosing port (12) at the top. The pH adjustment device (3) is equipped with an ammonia dosing port (13) at the top. The cleaning device (5) is equipped with a deionized water dosing port (14) and an ethanol dosing port (15) at the top.
2. The process apparatus for preparing ferric phosphate from waste phosphoric acid according to claim 1, characterized in that, Liquid flow meters are provided on the hydrogen peroxide dosing port (10), ferrous sulfate solution dosing port (11), waste phosphoric acid dosing port (12), ammonia dosing port (13), deionized water dosing port (14) and ethanol dosing port (15).
3. The process apparatus for preparing ferric phosphate from waste phosphoric acid according to claim 1, characterized in that, The upper ends of the ferrous reaction device (1), the ferric phosphate reaction device (2) and the pH adjustment device (3) are all equipped with stirring paddles, and the pH adjustment device (3) is equipped with a pH meter inside.
4. The process apparatus for preparing ferric phosphate from waste phosphoric acid according to claim 1, characterized in that, The ferrous reaction device (1) is equipped with a cooling water circulation device. The cooling water circulation device and the outer wall of the ferrous reaction device (1) form a cooling water circulation chamber. A coolant inlet is provided on the side wall of the cooling water circulation chamber, and a coolant outlet is provided at the bottom of the cooling water circulation chamber.
5. The process apparatus for preparing ferric phosphate from waste phosphoric acid according to claim 1, characterized in that, The iron phosphate reaction device (2) is equipped with a hot water circulation device. The hot water circulation device and the outer wall of the iron phosphate reaction device (2) form a hot water circulation chamber. A hot water inlet is provided on the side wall of the hot water circulation chamber, and a hot water outlet is provided at the bottom of the hot water circulation chamber.
6. The process apparatus for preparing ferric phosphate from waste phosphoric acid according to claim 1, characterized in that, The output end of the ferrous reaction device (1) is equipped with a first pump (16), the output end of the first pump (16) is connected to the upper part of the ferric phosphate reaction device (2), the output end of the ferric phosphate reaction device (2) is equipped with a second pump (17), the output end of the second pump (17) is connected to the upper part of the pH adjustment device (3), the output end of the pH adjustment device (3) is equipped with a third pump (18), the output end of the third pump (18) is connected to the input end of the plate and frame filter press (4), the output end of the cleaning device (5) is equipped with a fourth pump (20), the output end of the fourth pump (20) is connected to the inlet of the centrifugal separation device (6).
7. The process apparatus for preparing ferric phosphate from waste phosphoric acid according to claim 1, characterized in that, The plate and frame filter press (4) is equipped with a first conveyor belt (19) at the lower slag outlet and the upper end of the washing device (5). The centrifugal separation device (6) outlet and the drying device (7) inlet are equipped with a second conveyor belt (21). The drying device (7) outlet and the crushing device (8) inlet are equipped with a third conveyor belt (22). The crushing device (8) outlet and the packaging device (9) inlet are equipped with a fourth conveyor belt (23).