A high-substance-concentration ion exchange treatment apparatus
By combining a centrifugal exchange device and a centrifugal drive device, the problem of excessive cleaning wastewater in the treatment of high-concentration electroless nickel plating aging solutions is solved, achieving efficient adsorption and regeneration, and reducing production costs and energy consumption.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- DEXING CHEM (SUZHOU) CO LTD
- Filing Date
- 2022-07-21
- Publication Date
- 2026-05-01
AI Technical Summary
Existing technologies for treating high-concentration electroless nickel plating aging solutions generate large amounts of cleaning wastewater during ion exchange regeneration, increasing treatment costs and process complexity. Furthermore, traditional methods are inefficient and energy-intensive.
A high-concentration ion exchange treatment device is adopted, which includes a centrifugal exchange unit and a centrifugal drive unit. Ionic substances are adsorbed by chelating resin in the centrifugal exchange column, and the rotation of the centrifugal drive unit and the stirring of the air inlet pipe are used in combination with the controllable flow solenoid valve to achieve a high-efficiency adsorption and regeneration process.
It significantly reduces the amount of cleaning water used, lowers production costs, and improves the regeneration efficiency of the adsorbent through centrifugation, simplifying the process and reducing energy consumption.
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Figure CN115215479B_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the field of wastewater treatment, and specifically to an ion exchange treatment device with high substance concentration. Background Technology
[0002] The electroless nickel plating process for nickel-phosphorus alloys is characterized by the use of sodium hypophosphite as a reducing agent. The oxidized sodium hypophosphite, a byproduct of oxidation, significantly impacts the plating layer. The plating solution must be replaced after a certain period of use; the replaced solution is called the aging solution. The aging solution contains high concentrations of nickel ions, phosphite ions, sodium ions, sulfate ions, and ammonium ions. While these substances have a significant environmental impact, they are all usable resources.
[0003] Traditional methods, such as using chelating resin to adsorb and recover nickel from the aging solution generated by electroless nickel plating, evaporation and crystallization to remove sodium sulfate, and precipitation to remove phosphate ions, separate and utilize the harmful components of the aging solution, thus achieving resource utilization and effective disposal of the aging solution; however, the substance concentration of the aging solution is very high, and when using recovery ion exchange treatment, a large amount of clean water is required to wash the adsorbent, which will generate a large amount of wastewater that cannot be discharged.
[0004] For example, prior art 201710155570.1 discloses a method and treatment system for removing phosphorus and nickel from electroless nickel plating wastewater, which uses electrolytic oxidation, precipitation and ion exchange to treat electroless nickel plating wastewater. This generates a lot of hazardous waste and has high treatment costs. The ion exchange regeneration process generates a lot of cleaning wastewater, which increases costs. Another example is prior art 202110594658.X, which discloses a treatment device and process for recovering nickel from electroless nickel plating wastewater. This method uses pretreatment, electrodeposition to deposit nickel and activated carbon fiber to adsorb nickel to treat electroless nickel plating wastewater. This method not only requires many steps, but also has low electrodeposition efficiency and requires multiple treatments. It uses activated carbon fiber to adsorb nickel and uses steam for regeneration, which has high energy consumption. Summary of the Invention
[0005] The purpose of this invention is to overcome the shortcomings of the prior art and provide an ion exchange treatment device with high material concentration.
[0006] To achieve the above objectives, the technical solution adopted by the present invention is: a high-concentration ion exchange treatment device, comprising a base, a centrifugal exchange device and a centrifugal drive device respectively disposed on the base;
[0007] The centrifugal exchange device includes a tube vertically mounted on a base, a centrifugal exchange column rotatably mounted inside the tube and placed coaxially with the tube, and an outlet located at the bottom of the tube.
[0008] The centrifugal exchange column has a hollow structure and is filled with chelating resin; filter holes are provided on the surface and bottom of the centrifugal exchange column, respectively.
[0009] The centrifugal drive device is used to drive the centrifugal exchange column to rotate.
[0010] Preferably, a water distribution plate is provided above the chelating resin inside the centrifugal exchange column; the water distribution plate is placed horizontally and is provided with a quick connector.
[0011] Preferably, the diameter of the filter pores on the surface of the centrifugal exchange column increases from top to bottom.
[0012] Preferably, the centrifugal exchange column is provided with an inner lining mesh; the chelating resin is located inside the inner lining mesh; the mesh aperture of the inner lining mesh is smaller than the particle diameter of the chelating resin.
[0013] Preferably, the centrifugal exchange device further includes a vertically placed air inlet pipe and a telescopic mechanism for driving the air inlet pipe to extend into the centrifugal exchange column.
[0014] Preferably, the bottom of the pipe body is provided with a water collection groove; the water outlet is located at the lowest point of the water collection groove.
[0015] Preferably, there are multiple water outlets, each connected to a water outlet pipe; each water outlet pipe is equipped with a switch valve.
[0016] Preferably, the switching valve is a controllable flow solenoid valve.
[0017] Preferably, the bottom of the tube is provided with a support base; the bottom of the centrifugal exchange device is provided with a support shaft extending into the support base; and the top of the centrifugal exchange device is provided with a cross-shaped support frame.
[0018] The centrifugal drive device includes a motor mount on a base, a motor mounted vertically on the motor mount, a rotating shaft mounted vertically on a support frame, a belt drive for connecting the motor drive end and the rotating shaft, and a controller for controlling the operation of the motor.
[0019] Preferably, the bottom of the base is provided with a plurality of height-adjustable support feet.
[0020] Due to the application of the above technical solution, the present invention has the following advantages compared with the prior art:
[0021] This invention can recover precious nickel from liquids, separate and remove sodium ions, and reduce the residue of liquid on the adsorbent chelating resin by centrifugation, greatly reducing the amount of cleaning water used and lowering production costs. Attached Figure Description
[0022] The technical solution of the present invention will be further described below with reference to the accompanying drawings:
[0023] Appendix Figure 1This is a schematic diagram of the high-concentration ion exchange treatment device described in this invention.
[0024] Appendix Figure 2 This is a schematic diagram of the centrifugal exchange device in this invention;
[0025] Appendix Figure 3 This is a top view of the centrifugal exchange device in this invention;
[0026] Appendix Figure 4 This is a bottom view of the centrifugal exchange device in this invention.
[0027] The components are as follows: 1. Base; 11. Support foot; 2. Centrifugal exchange device; 21. Pipe body; 22. Centrifugal exchange column; 221. Filter hole; 23. Water outlet; 231. Liquid outlet; 232. Cleaning water outlet; 233. Acid outlet; 234. Alkali outlet; 235. Water outlet pipe; 236. Switch valve; 24. Water distribution plate; 25. Inner lining mesh; 26. Air inlet pipe; 27. Telescopic mechanism; 28. Water collection groove; 29. Liquid inlet pipe; 3. Centrifugal drive device; 31. Motor base; 32. Motor; 33. Belt drive; 34. Controller; 35. Support base; 36. Support shaft; 37. Support frame; 38. Rotating shaft. Detailed Implementation
[0028] The present invention will now be described in further detail with reference to the accompanying drawings and specific embodiments.
[0029] Appendix Figure 1-4 The high-concentration ion exchange treatment device of the present invention includes a base 1, a centrifugal exchange device 2 and a centrifugal drive device 3 respectively disposed on the base 1;
[0030] The centrifugal exchange device 2 includes a tube 21 vertically mounted on a base 1, a centrifugal exchange column 22 rotatably mounted inside the tube 21 and coaxially placed with the tube 21, and an outlet 23 located at the bottom of the tube 21.
[0031] The centrifugal exchange column 22 has a hollow structure and is filled with chelating resin; filter holes 221 are respectively provided on the surface and bottom of the centrifugal exchange column 22.
[0032] The centrifugal drive device 3 is used to drive the centrifugal exchange column 22 to rotate.
[0033] Furthermore, a water distribution plate 24 is provided above the chelating resin inside the centrifugal exchange column 22; the water distribution plate 24 is placed horizontally and is provided with a quick connector; the present invention uses the water distribution plate 24 to uniformly disperse the liquid in the inlet pipe 29 in the centrifugal exchange column 22; in addition, by providing a quick connector on the water distribution plate 24, it is convenient to quickly connect to the inlet pipe 29.
[0034] Furthermore, the diameter of the filter holes 221 on the surface of the centrifugal exchange column 22 increases from top to bottom. During operation, since the liquid enters from the top of the centrifugal exchange column 22, it will initially contact the uppermost chelating resin. If the diameter of the filter holes 221 is the same, the liquid may not have penetrated to the lowermost chelating resin before being discharged from the filter holes 221 on the surface of the centrifugal exchange column 22, resulting in uneven adsorption of the chelating resin inside the centrifugal exchange column 22. This invention, by making the diameter of the filter holes 221 on the surface of the centrifugal exchange column 22 increase from top to bottom, allows the liquid to slowly penetrate from the uppermost chelating resin to the lowermost chelating resin, resulting in more uniform adsorption.
[0035] Furthermore, an inner lining mesh 25 is provided inside the centrifugal exchange column 22; the chelating resin is located inside the inner lining mesh 25; the mesh aperture of the inner lining mesh 25 is smaller than the particle diameter of the chelating resin; by providing the inner lining mesh 25, the present invention prevents the chelating resin particles from flowing out of the filter holes 221 when the centrifugal drive device 3 drives the centrifugal exchange column 22 to rotate.
[0036] Furthermore, the centrifugal exchange device 2 also includes a vertically placed air inlet pipe 26 and a telescopic mechanism 27 for driving the air inlet pipe 26 into the centrifugal exchange column 22. The present invention improves the regeneration efficiency by setting the air inlet pipe 26 for stirring during chelate resin regeneration. In addition, by setting the telescopic mechanism 27, the air inlet pipe 26 is driven to descend and extend into the centrifugal exchange column 22 during chelate resin regeneration, and the air inlet pipe 26 is driven to rise and detach from the centrifugal exchange column 22 when the centrifugal drive device 3 drives the centrifugal exchange column 22 to rotate. The telescopic mechanism 27 is prior art, so its structure will not be described in detail.
[0037] Furthermore, a water collection groove 28 is provided at the bottom of the pipe body 21; the water outlet 23 is located at the lowest point of the water collection groove 28, so that no liquid will remain when draining.
[0038] Furthermore, the water outlet 23 is provided with four outlets, namely liquid outlet 231, cleaning water outlet 232, acid outlet 233, and alkali outlet 234; each of the liquid outlet 231, cleaning water outlet 232, acid outlet 233, and alkali outlet 234 is connected to a water outlet pipe 235; each of the water outlet pipes 235 is provided with a switch valve 236; during operation: the water outlet pipes 235 of the liquid outlet 231, cleaning water outlet 232, acid outlet 233, and alkali outlet 234 are respectively connected to the corresponding liquid storage tanks and controlled by the switch valves 236.
[0039] Furthermore, the switching valve 236 is a controllable flow solenoid valve, which facilitates flow control.
[0040] Furthermore, a support base 35 is provided at the bottom of the tube body 21; a support shaft 36 extending into the support base 35 is provided at the bottom of the centrifugal exchange device 2; and a cross-shaped support frame 37 is provided at the top of the centrifugal exchange device 2.
[0041] The centrifugal drive device 3 includes a motor base 31 mounted on a base 1, a motor 32 mounted vertically on the motor base 31, a rotating shaft 38 mounted vertically on a support frame 37, a belt drive 33 for connecting the drive end of the motor 32 and the rotating shaft 38, and a controller 34 for controlling the operation of the motor 32.
[0042] Furthermore, the bottom of the base 1 is provided with a plurality of height-adjustable support feet 11.
[0043] Working principle:
[0044] The water distribution plate 24 is connected to the liquid inlet pipe 29 via a quick connector. The liquid inlet pipe 29 then distributes the liquid evenly in the centrifugal exchange column 22 through the water distribution plate 24. After passing through the chelating resin in the centrifugal exchange column 22, the liquid adsorbs ionic substances. If the adsorption is not completed in one step, the liquid outlet 231 can be connected to the next centrifugal exchange column 22 through a liquid conduit to continue adsorption. This cycle continues until the adsorption is completed.
[0045] When the chelating resin in the centrifugal exchange column 22 is saturated with adsorption, regeneration and recovery are required. First, connect the outlet 231 to the raw material storage tank, then start the motor 32 through the controller 34, control the speed to 100-3500 rpm, drive the centrifugal exchange column 22 to rotate through the belt drive 33, centrifuge out the residual liquid in the chelating resin, and finally perform regeneration treatment.
[0046] Specific work process:
[0047] First, solid particles in the electroless nickel plating aging solution are filtered out. Then, the liquid is evenly dispersed in the centrifugal exchange column 22 through the inlet pipe 29 and the water distribution plate 24. After passing through the chelating resin in the centrifugal exchange column 22, ionic substances are adsorbed, and the liquid flows into the collection groove. A sample is taken at the outlet 231 for testing. If the nickel content is higher than 1.0 mg / L, the liquid is quickly connected to the water distribution plate 24 of the second centrifugal exchange column 22 through the outlet pipe 235. The liquid is then evenly dispersed in the centrifugal exchange column 22 through the water distribution plate 24. After passing through the chelating resin in the centrifugal exchange column 22, ionic substances are adsorbed, and the liquid flows into the collection groove. A sample is taken at the outlet 231 for testing. If the nickel content is higher than 1.0 mg / L, the liquid is then quickly connected to the water distribution plate 24 of the second centrifugal exchange column 22 through the outlet pipe 235. If the concentration is mg / l, it is quickly connected to the water distribution plate 24 of the third centrifugal exchange column 22 through the water outlet pipe 235 of the outlet 231. The water is evenly dispersed in the centrifugal exchange column 22 through the water distribution plate 24. After passing through the chelating resin in the centrifugal exchange column 22, the ionic substances are adsorbed and then flow into the collection groove. A sample is taken at the outlet 231 to test the nickel content.
[0048] When the nickel ion content at the outlet of the third centrifugal exchange column 22 exceeds 0.1 ppm, the first centrifugal exchange column 22 is regenerated, and the original second centrifugal exchange column 22 becomes the first. The order of the subsequent centrifugal exchange columns 22 is changed in sequence, and the regenerated centrifugal exchange column 22 is used as a spare.
[0049] Recycling process:
[0050] Step 1: First, drive the air inlet pipe 26 to rise and separate from the centrifugal exchange column 22 through the telescopic mechanism 27, then connect the liquid outlet 231 to the raw material liquid storage tank, and finally start the motor 32 through the controller 34, control the speed to 1500 rpm, work for 1-10 minutes and then stop, centrifuge out the residual liquid in the chelating resin.
[0051] Step 2: Close all outlet valves 23, then add 5% sulfuric acid through inlet pipe 29. Next, drive inlet pipe 26 downwards via telescopic mechanism 27 to extend into centrifugal exchange column 22, aerating and stirring. After 10-30 minutes, drive inlet pipe 26 upwards via telescopic mechanism 27 to detach from centrifugal exchange column 22. Then, open acid outlet valve 233 to drain the nickel sulfate and sulfuric acid mixture. Turn on motor 32 at 100-1500 rpm. Then, introduce clean water through inlet pipe 29 at a flow rate of 2 BV, while simultaneously driving the flow through telescopic mechanism 27... The intake pipe 26 descends and extends into the centrifugal exchange column 22, where air is introduced and stirred. Then, the intake pipe 26 is driven to rise and detach from the centrifugal exchange column 22 via the telescopic mechanism 27. The working motor 32 is started at a speed of 100-1500 rpm, and cleaning water enters the acid tank. Finally, the switch valve of the acid outlet 233 is closed. The acid concentration in the acid tank is detected. If it is less than 5%, sulfuric acid is added for the next use. The nickel ion content and acid content are detected. When the nickel ion content is 60 g / L, nickel sulfate can be evaporated and crystallized to produce crude nickel sulfate product for later use. The evaporated water can be reused to prepare acid regeneration solution.
[0052] Step 3: Close all outlet valves 23, then add 5% sodium hydroxide through inlet pipe 29. Next, drive the air inlet pipe 26 downwards via telescopic mechanism 27 to extend into the centrifugal exchange column 22, aerating and stirring. After 10-30 minutes, drive the air inlet pipe 26 upwards via telescopic mechanism 27 to detach from the centrifugal exchange column 22. Then, open the alkali outlet valve 234 to drain the mixture of sodium sulfate and sodium hydroxide. Turn on the operating motor 32 at 100-1500 rpm. Then, introduce clean water through inlet pipe 29 at a flow rate of 2 BV. Simultaneously, drive the telescopic mechanism... Mechanism 27 drives the air inlet pipe 26 to descend and extend into the centrifugal exchange column 22, where air is introduced and stirred. Then, the air inlet pipe 26 is driven to rise and detach from the centrifugal exchange column 22 via the telescopic mechanism 27. The working motor 32 is started at a speed of 100-1500 rpm, and cleaning water enters the alkali tank. Finally, the switch valve of the alkali solution port 234 is closed. The concentration of sodium hydroxide in the alkali tank is detected. If it is less than 5%, sodium hydroxide is added for the next use. The concentration of sodium sulfate is detected. If it is 60-100 g / L, the alkali solution is evaporated at low temperature to crystallize out sodium sulfate for disposal. The water is evaporated and used to prepare sodium hydroxide solution. Specific Implementation
[0053] Centrifugal exchange column 22 is filled with 2730L of chelating resin. The nickel content of the aging solution is 4532mg / L. The influent flow rate is adjusted to 60L / h. The air inlet pipe 26 is opened. When the nickel content of the effluent from the three centrifugal exchange columns 22 exceeds 1.0mg / L, the influent to the first centrifugal exchange column 22 is stopped. The outlet 231 is connected to the raw material storage tank, and the air pipe is raised. The motor 32 is started, and the speed is adjusted to 1200rpm. It is stopped after 2 minutes. The switch valve of the outlet 231 is closed, and 60L of 5% sulfuric acid is introduced through the air pipe. The system is stirred and aerated for 10 minutes. Then, the switch valve of the acid outlet 233 is opened, and the system is raised... Start the air inlet, start motor 32, adjust the speed to 1200 rpm, and stop after 2 minutes; close the switch valve of acid inlet 233, add 60 liters of clean water through the air inlet, and agitate with air for 10 minutes; open the switch valve of cleaning water inlet 232, raise the air inlet, start motor 32, adjust the speed to 1200 rpm, and stop after 2 minutes; close the switch valve of cleaning water inlet 232, add 60 liters of 5% sodium hydroxide through the air inlet, and agitate with air for 10 minutes; open the switch valve of alkali inlet 234, raise the air inlet, start motor 32, adjust the speed to 1200 rpm, and stop after 3 minutes; close the switch valve of alkali inlet 234. The first centrifugal exchange column 22 is regenerated and ready for use.
[0054] The equipment of this invention produces 60 liters of cleaning water, which is only 1 / 4 of the 240 liters produced by the traditional ion exchange method, greatly reducing the amount of cleaning water used and lowering production costs.
[0055] The above are merely specific application examples of the present invention and do not constitute any limitation on the scope of protection of the present invention. All technical solutions formed by equivalent transformations or substitutions fall within the scope of protection of the present invention.
Claims
1. A high-concentration ion exchange treatment device, characterized in that: It includes a base, a centrifugal exchange device and a centrifugal drive device respectively mounted on the base; The centrifugal exchange device includes a tube vertically mounted on a base, a centrifugal exchange column rotatably mounted inside the tube and placed coaxially with the tube, and an outlet located at the bottom of the tube; the centrifugal exchange column has a hollow structure and is filled with chelating resin. The centrifugal exchange column is provided with filter holes on its surface and bottom respectively; the diameter of the filter holes on the surface of the centrifugal exchange column increases from top to bottom. The centrifugal exchange device also includes a vertically placed air inlet pipe and a telescopic mechanism for driving the air inlet pipe to extend into the centrifugal exchange column. The bottom of the pipe body is provided with a water collection groove; the water outlet is located at the lowest point of the water collection groove; there are multiple water outlets, including liquid outlet, cleaning water outlet, acid outlet and alkali outlet, and each is connected to a water outlet pipe; each water outlet pipe is provided with a switch valve. The centrifugal drive device is used to drive the centrifugal exchange column to rotate.
2. The high-concentration ion exchange treatment device according to claim 1, characterized in that: The centrifugal exchange column has a water distribution plate positioned above the chelating resin; the water distribution plate is horizontally placed and equipped with a quick connector.
3. The high-concentration ion exchange treatment device according to claim 2, characterized in that: The centrifugal exchange column is equipped with an inner lining mesh; the chelating resin is located inside the inner lining mesh; the mesh aperture of the inner lining mesh is smaller than the particle diameter of the chelating resin.
4. The high-concentration ion exchange treatment device according to claim 3, characterized in that: The switching valve is a controllable flow solenoid valve.
5. The high-concentration ion exchange treatment device according to any one of claims 1-4, characterized in that: The bottom of the tube is provided with a support base; the bottom of the centrifugal exchange device is provided with a support shaft extending into the support base; the top of the centrifugal exchange device is provided with a cross-shaped support frame. The centrifugal drive device includes a motor mount on a base, a motor mounted vertically on the motor mount, a rotating shaft mounted vertically on a support frame, a belt drive for connecting the motor drive end and the rotating shaft, and a controller for controlling the operation of the motor.
6. The high-concentration ion exchange treatment device according to claim 5, characterized in that: The base has multiple height-adjustable support feet at its bottom.
Citation Information
Patent Citations
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