Device for preparing ferrous oxalate from iron ions in wet-process phosphoric acid purification raffinate acid
The iron ions in oxalic acid are removed through the photocatalytic reaction device, and the problems of oxalic acid pollution and high cost in the prior art are solved, and efficient and low-cost preparation of ferrous oxalate is achieved.
Patent Information
- Application Number
- CN202422565883.2
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-10-23
- Publication Date
- 2025-08-26
- Estimated Expiration
- 2034-10-23
AI Technical Summary
In the prior art, when removing iron ions in oxalic acid and preparing ferrous oxalic acid, other reactants are produced during the reaction, which is complicated and costly.
Using a device including an anti-seepage light source, a reaction chamber and a reactor shell, the iron ions in the oxalic acid are removed by using a photocatalytic reaction, the light required for the photocatalytic reaction is provided through the anti-seepage light source, and the light required for the photocatalytic reaction is fixed through the connection between the multi-porous plate and the tetrafluoro plate, and the reaction process is monitored in combination with a temperature sensor to realize the preparation of ferrous oxalate.
The preparation of high-purity ferrous oxalate is achieved, the operation process is simplified, the production cost is reduced, and the oxalic acid can be put into use immediately after treatment, avoiding contamination of other compounds.
Smart Images
Figure CN223263814U_ABST
Abstract
Description
Technical Field
[0001] The utility model belongs to the technical field of sulfuric acid wet-process phosphoric acid purification and relates to a device for obtaining high-purity ferrous oxalate. Background Art
[0002] During the wet-process phosphoric acid purification process, a large amount of impurity ions accumulate in the raffinate, making it difficult to digest and utilize the raffinate. The present invention removes a large amount of impurity ions from the raffinate through an extraction process, separates the iron ions, and performs high-value conversion to produce a high-purity ferrous oxalate product. The MER value of the iron-magnesium-aluminum-calcium sesquioxides enriched in the raffinate has a value of about 15%, which makes the raffinate viscosity high and difficult to utilize. When the raffinate is added to produce DAP / MAP, the nutrients and moisture content are unqualified. In order to utilize the raffinate in a high-value manner, a solvent extraction method is used to remove the impurity cations in the raffinate, and the iron ions are stripped with a stripping agent to obtain the iron salt of oxalic acid. Summary of the Invention
[0003] To address these issues, a pre-extraction and impurity removal device was developed to address the shortcomings of existing extraction technologies. This device effectively removes impurities from wet-process phosphoric acid, particularly iron, magnesium, and aluminum, resulting in high-purity wet-process purified phosphoric acid. The overall process boasts a high extraction rate and low raffinate acid yield, making it suitable for large-scale production.
[0004] The purpose of the utility model is to provide a device for removing iron ions in oxalic acid and preparing ferrous oxalate, so as to solve the problems raised in the above background technology.
[0005] Aiming at the problems that the existing methods for removing iron ions from oxalic acid and preparing ferrous oxalate have the problem that other reactants appear during the reaction process to contaminate the oxalic acid, making it impossible to use the oxalic acid immediately, as well as high production costs and complicated operations, a device for removing iron ions from oxalic acid and preparing ferrous oxalate is disclosed, comprising:
[0006] A device for removing iron ions from oxalic acid and producing ferrous oxalate comprises an impermeable light source, a reaction chamber, and a reactor housing. The impermeable light source is located at the center of the reaction chamber to provide the reaction chamber with light required for a photocatalytic reaction. The reaction chamber is located at the center of the reactor housing and is spaced relative to the impermeable light source to facilitate the photocatalytic reaction. The photoreactor housing comprises a polytetrafluoroethylene plate, a porous plate, a lug, a feed port, a vent valve, a discharge port, and a temperature sensor.
[0007] In the improved solution, a metal gas pipe is provided inside the anti-seepage light source to inject nitrogen into the anti-seepage light source for replacement.
[0008] In the improved solution, the anti-seepage light source is connected to the external power source by relying on the positive and negative poles of the light to provide the reaction chamber with the light required for the photocatalytic reaction.
[0009] In the improved solution, the anti-seepage light source and the metal air pipe are connected and fixed by interference fit of a porous plate.
[0010] In the improved solution, the polytetrafluoroethylene plate in the reactor shell is bolted to the reactor shell by chrome-plated bolts to achieve a sealing effect.
[0011] In the improved solution, the anti-seepage light source and the PTFE plate are connected by bolts via a connecting shaft.
[0012] The lower part of the photoreactor shell is provided with a feed port, a vent valve and a discharge port; and a temperature sensor is provided inside the photoreactor shell.
[0013] Beneficial effects of the utility model
[0014] The technical effects achieved by this new technology are as follows:
[0015] 1. Remove iron ions from oxalic acid.
[0016] 2. Preparation of high-purity ferrous oxalate.
[0017] 3. Simple operation.
[0018] 4. No other compounds will be produced to contaminate oxalic acid, so the treated oxalic acid can be put into use immediately.
[0019] 5. Production costs are reduced. BRIEF DESCRIPTION OF THE DRAWINGS
[0020] Figure 1 A structural diagram of a device for removing iron ions from oxalic acid and preparing ferrous oxalate, wherein the diagram includes: 1. metal gas pipe; 2. connecting shaft; 3. anti-seepage light source; 4. lamp tube bracket; 5. vent valve; 6. discharge port; 7. Teflon plate; 8. feed port; 9. reaction chamber; 10. hanging ear; 11. photoreactor shell; 12. temperature sensor; 13. porous plate 1; 14. Teflon plate; 15. positive and negative electrodes of the lamp tube; 16. chrome-plated bolts; 17. porous plate 2. DETAILED DESCRIPTION
[0021] Example 1
[0022] like Figure 1 As shown, this embodiment discloses a device for removing iron ions from oxalic acid and preparing ferrous oxalate, comprising: an anti-seepage light source 3, a reaction chamber 9 and a photoreactor housing 11, wherein the anti-seepage light source 3 is located at the axial center of the reaction chamber 9;
[0023] The reaction chamber 9 is located at the center of the photoreactor housing 11 and maintains a relative distance from the anti-seepage light source 3 .
[0024] There is a metal gas pipe 1 inside the anti-seepage light source 3, which is used to inject nitrogen into the anti-seepage light source 3 for replacement.
[0025] The anti-seepage light source 3 is connected to external power through the positive and negative electrodes 15 of the lamp tube to provide the reaction chamber with light required for the photocatalytic reaction.
[0026] The anti-seepage light source 3 and the metal air pipe 1 are respectively connected by interference fit through the upper porous plate 13 and the lower porous plate 2 17.
[0027] A polytetrafluoroethylene plate 14 is provided on the upper portion of the photoreactor housing 11 and is bolted to the photoreactor housing 11 via chrome-plated bolts 16 .
[0028] The anti-seepage light source 3 is connected to the PTFE plate 14 through the connecting shaft 2.
[0029] The lower portion of the photoreactor housing 11 is provided with a feed port 8 , a vent valve 5 , and a discharge port 6 ; a temperature sensor 12 is provided inside the photoreactor housing 11 .
[0030] The working method of this embodiment is as follows:
[0031] When it is necessary to remove iron ions from oxalic acid and prepare ferrous oxalate,
[0032] Open the metal gas pipe 1 and inject nitrogen into the anti-seepage light source 3 to remove all air;
[0033] Ten minutes later, the anti-seepage light source 3 is turned on to provide the light required for the photocatalytic reaction into the reaction chamber 9;
[0034] At the same time, the feed port 8 is opened to feed the reaction material into the reaction shell 11;
[0035] When the reaction material fills the reaction shell 11, it will enter the reaction chamber 9. The material is oxalic acid. Oxalic acid reacts with the light emitted by the anti-seepage light source 3 to produce ferrous oxalate. Since the temperature in the reaction chamber 9 is relatively high at this time, the ferrous oxalate will dissolve in the oxalic acid. During this period, the temperature in the reaction chamber is observed by observing the temperature sensor 13.
[0036] Open the discharge port and allow the reacted material to enter the external storage tank for cooling and crystallization. Ferrous oxalate precipitate can be obtained, and the remaining clear liquid is not contaminated by other compounds and can be used further.
[0037] After the material to be processed is processed, open the drain valve 5 to discharge the remaining liquid from the reaction shell.
[0038] The experimental data of this embodiment for treating the ferric oxalate ion content and preparing ferrous oxalate are as follows:
[0039]
[0040] The above shows and describes 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 above embodiments and descriptions are merely preferred examples of the present invention and are not intended to limit the present invention. Various changes and improvements may be made to the present invention without departing from the spirit and scope of the present invention, and such changes and improvements fall within the scope of the present invention. The scope of protection claimed in the present invention is defined by the appended claims and their equivalents.
Claims
1. A device for preparing ferrous oxalate by purifying iron ions in raffinate using wet-process phosphoric acid, characterized in that: include: An impermeable light source (3), a reaction chamber (9), and a photoreactor housing (11), wherein the impermeable light source (3) is located at the axial center of the reaction chamber (9); The reaction chamber (9) is located at the center of the photoreactor housing (11) and maintains a relative distance from the anti-seepage light source (3); A metal gas pipe (1) is provided in the anti-seepage light source (3) for injecting nitrogen into the anti-seepage light source (3) for replacement; The anti-seepage light source (3) and the metal air pipe (1) are respectively connected by interference fit through the upper porous plate 1 (13) and the lower porous plate 2 (17).
2. The device for preparing ferrous oxalate by purifying iron ions in raffinate by wet-process phosphoric acid according to claim 1, characterized in that: The anti-seepage light source (3) is connected to external electric energy via the positive and negative electrodes (15) of the lamp tube to provide the reaction chamber with light required for the photocatalytic reaction.
3. The device for preparing ferrous oxalate by purifying iron ions in raffinate by wet-process phosphoric acid according to claim 1, characterized in that: A polytetrafluoroethylene plate (14) is provided on the upper portion of the photoreactor housing (11) and is bolted to the photoreactor housing (11) via chrome-plated bolts (16).
4. The device for preparing ferrous oxalate by purifying iron ions in raffinate by wet-process phosphoric acid according to claim 1, characterized in that: The anti-seepage light source (3) is connected to the tetrafluoroethylene plate (14) through the connecting shaft (2).
5. The device for preparing ferrous oxalate by purifying iron ions in raffinate by wet-process phosphoric acid according to claim 1, characterized in that: The lower part of the photoreactor shell (11) is provided with a feed port (8), a vent valve (5), and a discharge port (6); a temperature sensor (12) is provided inside the photoreactor shell (11).