An apparatus for on-line determination of raffinate sulfate
The three-stage filtration system solves the problems of accuracy and equipment protection in the detection of sulfate in lithium battery raffinate, and realizes an automated and rapid detection process.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- GUANGXI ZHILIANG NEW MATERIALS CO LTD
- Filing Date
- 2025-07-14
- Publication Date
- 2026-07-24
AI Technical Summary
The detection of sulfate in lithium battery raffinate is easily affected by particulate matter and suspended matter, which leads to decreased detection accuracy and pipeline blockage. Existing devices are difficult to effectively filter and protect the equipment.
It adopts a three-stage filtration system, including a primary screen filter, a secondary ceramic membrane filter, and a tertiary adsorption layer filter, combined with a backwasher, to effectively remove impurities and prevent pipeline blockage.
It enables automatic sampling, filtration, and testing of raffinate, improving testing accuracy, preventing pipeline blockage, and ensuring stable equipment operation.
Smart Images
Figure CN224552808U_ABST
Abstract
Description
Technical Field
[0001] This utility model relates to the field of ion detection technology, specifically to an online device for determining sulfate ions in raffinate. Background Technology
[0002] In the preparation of lithium battery cathode materials, metal ions are often separated and purified from the leaching solution using solvent extraction. Sulfuric acid is a commonly used leaching agent, so sulfate ions may remain in the raffinate. When the sulfate content is high, the extraction is incomplete, leading to metal loss or contamination in subsequent processes. Therefore, it is necessary to monitor the SO4²⁻ concentration in the raffinate to ensure product quality and the stability of the production process. Common methods for sulfate detection include colorimetry, ion chromatography, and electrode methods. For example, Chinese invention patent CN 114034643 A discloses an online sulfate analysis device, including a main unit housing an analyzer system and an electrical control system. The analysis system includes a sulfate detector, a sulfate reactor, a feed pump, a discharge pump, a reagent dripping pump, a pure water pump, a plunger pump device, and a reagent switching device. The reagent switching device has a water inlet, a feed inlet, a liquid outlet, and a waste outlet. It uses colorimetry for sulfate detection and can achieve automatic sampling, automatic detection, automatic cleaning, automatic discharge, and automatic analysis. However, for the detection of lithium battery raffinate, the presence of particulate matter, metal oxides, suspended solids, and other substances in the raffinate can easily interfere with the detection accuracy or cause pipeline blockage and damage to the equipment. Utility Model Content
[0003] The purpose of this invention is to address the aforementioned problems by providing an online device for determining sulfate in raffinate. By setting up a three-stage filtration system, the raffinate entering the reactor can be effectively filtered, reducing interference with detection accuracy and preventing pipeline blockage and equipment damage.
[0004] To achieve the above objectives, the technical solution adopted by this utility model is as follows: An online device for determining sulfate in raffinate includes a main unit housing, which houses an analyzer system and an electrical control system. The analyzer system includes a reactor, a plunger pump, a detector, a diluent, a three-stage filtration device, a waste liquid storage tank, a pure water tank, and a reagent tank. The pure water tank is connected to one port of a four-way valve via a pure water pump. The other three ports of the four-way valve are respectively connected to the pure water ports of the diluent, the plunger pump, and the reactor. The reagent tank is connected to the reagent port of the reactor via a reagent pump. The reaction liquid inlet and outlet of the plunger pump device are connected to the discharge port of the reactor. The detector is located outside the piston cylinder of the plunger pump device. The waste liquid port of the reactor is connected to the waste liquid storage tank through the discharge pump. The inlet of the three-stage filtration device is connected to the feed pump. The outlet of the three-stage filtration device is connected to the feed inlet of the diluent. The waste liquid outlet of the three-stage filtration device is connected to the waste liquid storage tank. The outlet of the diluent is connected to one port of a three-way valve. The other two ports of the three-way valve are respectively connected to the reactor and the waste liquid storage tank.
[0005] Furthermore, the three-stage filtration device includes a primary screen filter, a secondary ceramic membrane filter, a tertiary adsorption layer filter, and a backwasher. The outlet of the primary screen filter is sequentially connected to the inlet of the secondary ceramic membrane filter and the tertiary adsorption layer filter. The backwasher is connected to the backwash inlet of the primary screen filter, the secondary ceramic membrane filter, and the tertiary adsorption layer filter via a backwash pump. The backwash waste liquid outlet of the primary screen filter, the secondary ceramic membrane filter, and the tertiary adsorption layer filter is connected to the waste liquid temporary storage tank.
[0006] Furthermore, the primary filter screen is equipped with a rotatable cylindrical stainless steel filter screen, and a scraper is provided on the outer side of the stainless steel filter screen. The pore size of the stainless steel filter screen is 100-120μm.
[0007] Furthermore, the filter membrane of the secondary ceramic membrane filter is a zirconia ceramic membrane with a pore size of 1-5 μm.
[0008] Furthermore, the adsorption layer material of the three-stage adsorption layer filter is a polypropylene fiber felt adsorption layer.
[0009] Furthermore, a first solenoid valve is installed on the inlet of the primary filter screen, a second solenoid valve is installed on the backwash inlet of the primary filter screen, the secondary ceramic membrane filter, and the tertiary adsorption layer filter, and a third solenoid valve is installed on the backwash waste liquid outlet of the primary filter screen, the secondary ceramic membrane filter, and the tertiary adsorption layer filter.
[0010] By adopting the above technical solution, this utility model has the following beneficial effects: The raffinate of this invention can be automatically sampled and automatically tested after three-stage filtration and dilution. After testing, it can be automatically discharged and automatically rinsed, resulting in fast testing efficiency. Since the raffinate being tested can be effectively filtered to remove impurities, the raffinate entering the reactor can be effectively filtered, reducing interference with the testing accuracy and avoiding pipeline blockage and equipment damage. Attached Figure Description
[0011] Figure 1 This is a schematic diagram of an online device for determining sulfate in raffinate according to the present invention. Figure 2 This is a schematic diagram of the three-stage filtration device of this utility model; Figure 3 This is a schematic diagram of the structure of the primary filter screen of this utility model; In the diagram: 1-Main unit chassis, 2-Pure water tank, 3-Pure water pump, 4-Reagent tank, 5-Reagent pump, 6-Four-way valve, 7-Diluter, 8-Plunger pump device, 9-Detector, 10-Three-stage filtration device, 11-Reactor, 12-Waste liquid temporary storage tank, 13-Feed pump, 14-Discharge pump, 15-Three-way valve, 101-First-stage filter, 1011-Stainless steel filter, 1012-Scraper, 102-Second-stage ceramic membrane filter, 103-Third-stage adsorption layer filter, 104-Backwasher, 105-Backwash pump, 106-First solenoid valve, 107-Second solenoid valve, 108-Third solenoid valve. Detailed Implementation
[0012] To enable those skilled in the art to better understand the present invention, the technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings of the embodiments of the present invention. Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by those skilled in the art to which the present invention pertains. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the present invention. The terms "first," "second," etc., in the specification, claims, and accompanying drawings of the present invention are used to distinguish different objects and not to describe a particular order. Furthermore, the terms "comprising" and "having," and any variations thereof, are intended to cover non-exclusive inclusion. For example, a process, method, system, product, or device that includes a series of steps or units is not limited to the listed steps or units, but may optionally include steps or units not listed, or may optionally include other steps or units inherent to these processes, methods, products, or devices.
[0013] In this document, the term "embodiment" means that a particular feature, structure, or characteristic described in connection with an embodiment may be included in at least one embodiment of the present invention. The appearance of this phrase in various places throughout the specification does not necessarily refer to the same embodiment, nor is it a separate or alternative embodiment mutually exclusive with other embodiments. It will be explicitly and implicitly understood by those skilled in the art that the embodiments described herein can be combined with other embodiments.
[0014] like Figure 1 As shown, an online device for determining sulfate in raffinate includes a main unit 1, which houses an analyzer system and an electrical control system. The analyzer system includes a reactor 11, a plunger pump 8, a detector 9, a diluent 7, a three-stage filtration device 10, a waste liquid storage tank 12, a pure water tank 2, and a reagent tank 4. The pure water tank 2 is connected to one port of a four-way valve 6 via a pure water pump 3. The other three ports of the four-way valve 6 are connected to the diluent 7, the plunger pump 8, and the pure water port of the reactor 11, respectively. The reagent tank 4 is connected to the reagent port of the reactor 11 via a reagent pump 5. The plunger pump 8... The inlet and outlet of the reaction liquid are connected to the discharge port of the reactor 11. A detector 9 is located outside the piston cylinder of the plunger pump device 8. The waste liquid port of the reactor 11 is connected to the waste liquid storage tank 12 via a discharge pump 14. The inlet of the three-stage filtration device 10 is connected to a feed pump 13. The outlet of the three-stage filtration device 10 is connected to the inlet of the diluent 7. The waste liquid outlet of the three-stage filtration device 10 is connected to the waste liquid storage tank 12. The outlet of the diluent 7 is connected to one port of a three-way valve 15. The other two ports of the three-way valve 15 are connected to the reactor 11 and the waste liquid storage tank 12, respectively. Liquid level sensors can be installed in the waste liquid storage tank 12, the pure water tank 2, and the reagent tank 4 to facilitate liquid level detection.
[0015] like Figure 2 As shown, the three-stage filtration device 10 includes a primary screen filter 101, a secondary ceramic membrane filter 102, a tertiary adsorption layer filter 103, and a backwasher 104. The outlet of the primary screen filter 101 is sequentially connected to the inlets of the secondary ceramic membrane filter 102 and the tertiary adsorption layer filter 103. The backwasher 104, via a backwash pump 105, is connected to the backwash inlets of the primary screen filter 101, the secondary ceramic membrane filter 102, and the tertiary adsorption layer filter 103. The backwash waste liquid outlets of the primary screen filter 101, the secondary ceramic membrane filter 102, and the tertiary adsorption layer filter 103 are connected to a waste liquid storage tank 12. The three-stage filtration device 10 effectively removes impurities, thereby reducing interference with subsequent testing and preventing blockages in pipelines. The backwasher 104 is used to backwash and clean each stage of the filter.
[0016] like Figure 3As shown, the primary filter 101 contains a rotatable cylindrical stainless steel filter screen 1011. A scraper 1012 is located on the outer side of the stainless steel filter screen 1011. The pore size of the stainless steel filter screen 1011 is 100-120 μm. It is used for filtering coarse particles. The stainless steel filter screen 1011 is motor-driven, and its surface is cleaned by the scraper 1012 and by reverse water flow backwashing. The secondary ceramic membrane filter 102 uses a zirconia ceramic membrane with a pore size of 1-5 μm, which can be used to filter medium-sized particulate impurities. The tertiary adsorption layer filter 103 uses a polypropylene fiber felt adsorption layer, which can adsorb substances such as grease.
[0017] A first solenoid valve 106 is installed on the inlet of the primary filter 101. A second solenoid valve 107 is installed on the backwash inlet of the primary filter 101, the secondary ceramic membrane filter 102, and the tertiary adsorption layer filter 103. A third solenoid valve 108 is installed on the backwash waste liquid outlet of the primary filter 101, the secondary ceramic membrane filter 102, and the tertiary adsorption layer filter 103.
[0018] The working process of this utility model: Pure water in pure water tank 2 enters the plunger pump device 8 through the four-way valve 6 inlet. Detector 9 detects and records the turbidity value of the pure water. After detection, the pure water is discharged into reactor 11 and then discharged to waste liquid storage tank 12 via waste liquid pump. The raffinate is also filtered through a three-stage filtration device 10 and then passed through diluent 7. Pure water in pure water tank 2 is sent to diluent 7 by pure water pump 3 to dilute the raffinate. After dilution, the raffinate is sent into reactor 11 through three-way valve 15. Reagent from reagent tank 4 is sent into reactor 11 by reagent pump 5 and reacts with the raffinate to be tested to produce precipitation. Plunger pump device 8 draws in the reaction liquid from reactor 11. Detector 9 tests the turbidity value of the reaction liquid. After testing, the reaction liquid is discharged into reaction cup and then discharged to waste liquid storage tank 12 via discharge pump 14. The sulfate content is calculated by the two test values. The diluter 7 can be automatically rinsed with pure water, and the waste liquid after rinsing is discharged into the waste liquid storage tank 12 through the three-way valve 15. The device can automatically sample the raffinate and automatically test it after three-stage filtration and dilution. After testing, it can automatically discharge the material and automatically rinse, making the testing efficient.
[0019] The present invention has been described in detail above. However, modifications or improvements can be made to it, which will be obvious to those skilled in the art. Therefore, any modifications or improvements that do not depart from the spirit of the present invention are within the protection scope of the present invention.
Claims
1. An online device for determining sulfate in raffinate, comprising a main unit housing an analyzer system and an electrical control system, characterized in that: The analyzer system includes a reactor, a plunger pump, a detector, a diluent, a three-stage filtration system, a waste liquid storage tank, a pure water tank, and a reagent tank. The pure water tank is connected to one port of a four-way valve via a pure water pump. The other three ports of the four-way valve are connected to the pure water ports of the diluent, the plunger pump, and the reactor, respectively. The reagent tank is connected to the reagent port of the reactor via a reagent pump. The reaction liquid inlet and outlet of the plunger pump are connected to the discharge port of the reactor. The detector is located outside the piston cylinder of the plunger pump. The waste liquid port of the reactor is connected to the waste liquid storage tank via a discharge pump. The inlet of the three-stage filtration system is connected to a feed pump. The outlet of the three-stage filtration system is connected to the inlet of the diluent. The waste liquid outlet of the three-stage filtration system is connected to the waste liquid storage tank. The outlet of the diluent is connected to one port of a three-way valve. The other two ports of the three-way valve are connected to the reactor and the waste liquid storage tank, respectively.
2. The online apparatus for determining sulfate ions in raffinate according to claim 1, characterized in that: The three-stage filtration device includes a primary screen filter, a secondary ceramic membrane filter, a tertiary adsorption layer filter, and a backwasher. The outlet of the primary screen filter is sequentially connected to the inlet of the secondary ceramic membrane filter and the tertiary adsorption layer filter. The backwasher is connected to the backwash inlet of the primary screen filter, the secondary ceramic membrane filter, and the tertiary adsorption layer filter via a backwash pump. The backwash waste liquid outlet of the primary screen filter, the secondary ceramic membrane filter, and the tertiary adsorption layer filter is connected to the waste liquid temporary storage tank.
3. The online apparatus for determining sulfate ions in raffinate according to claim 2, characterized in that: The primary filter contains a rotatable cylindrical stainless steel filter screen, and a scraper is provided on the outer side of the stainless steel filter screen. The pore size of the stainless steel filter screen is 100-120μm.
4. The online apparatus for determining sulfate ions in raffinate according to claim 2, characterized in that: The filter membrane of the secondary ceramic membrane filter is a zirconia ceramic membrane with a pore size of 1-5 μm.
5. The online apparatus for determining sulfate ions in raffinate according to claim 2, characterized in that: The adsorption layer material of the three-stage adsorption layer filter is a polypropylene fiber felt adsorption layer.
6. The online apparatus for determining sulfate ions in raffinate according to claim 2, characterized in that: A first solenoid valve is installed on the inlet of the primary filter screen, and a second solenoid valve is installed on the backwash inlet of the primary filter screen, the secondary ceramic membrane filter, and the tertiary adsorption layer filter, respectively. A third solenoid valve is installed on the backwash waste liquid outlet of the primary filter screen, the secondary ceramic membrane filter, and the tertiary adsorption layer filter, respectively.