Separation and purification device for ultra-clean high-purity wet electronic chemicals and application of separation and purification device
By introducing electrolysis and adsorption components into the separation and purification device of ultra-clean high-purity wet electronic chemicals and optimizing heating and cooling systems, the problem of low heat utilization in existing devices is solved, achieving efficient purification and energy savings.
Patent Information
- Application Number
- CN202411598406.4
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-11
- Publication Date
- 2025-02-18
AI Technical Summary
The existing separation and purification devices for ultra-clean high-purity wet electronic chemicals have low heat utilization during distillation, resulting in low energy waste and purification efficiency.
A device including an electrolysis assembly, an adsorption assembly, a heater and a cooling assembly is designed to remove metal ion impurities and particle impurities through electrolysis, and further improve purity by using the adsorption assembly, while optimizing the combination of the heater and the cooling assembly. Heat energy utilization.
It realizes efficient purification of wet electronic chemicals, improves product purity, saves energy and improves distillation efficiency.
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Figure CN119455422A_ABST
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of chemical and chemical equipment, and in particular is a separation and purification device for ultra-clean high-purity wet electronic chemicals and an application thereof. Background Art
[0002] Ultra-clean high-purity electronic chemicals mainly include wet electronic chemicals, high-purity analytical reagents, electronic-grade special gases, high-purity additives, etc. Wet electronic chemicals refer to inorganic or organic chemicals used as cleaning agents or solvents in the fields of semiconductors, liquid crystal panels, photovoltaics, lithium batteries, etc. High-purity analytical reagents are mainly used for analytical testing, chromatography-grade preparation, etc. With the advancement of science and technology and the development of industry, the separation and purification technology of ultra-clean high-purity electronic chemicals is also constantly developing in the direction of high efficiency, environmental protection, and energy saving.
[0003] Today's ultra-clean high-purity wet electronic chemicals separation and purification devices play a vital role in many fields such as chemical industry, medicine, and food. They can significantly improve the purity and quality of chemicals. Usually, the purity of newly produced wet electronic chemicals cannot meet the purity requirements of semiconductor-grade ultra-clean high-purity wet electronic chemicals, that is, the content of particles greater than or equal to 0.03μm in the ultra-clean high-purity wet electronic chemical solution is less than or equal to 1500pcs / mL, and the metal ion concentration is ensured to be less than 10ppt. The separation and purification of wet electronic chemicals is crucial, that is, the separation of metal ion impurities and particulate impurities. Some of these wet electronic chemicals can be separated and purified by distillation due to their strong thermal stability and relatively low boiling point, such as NMP. NMP generally contains metal ions such as magnesium ions, aluminum ions, iron ions, calcium ions, zinc ions, cobalt ions, and nickel ions. Nowadays, when NMP is separated and purified by conventional distillation, the coolant in the condensing device directly enters the condensing box after heat exchange, and then most of the heat in the heated coolant dissipates in the condensing box, the utilization rate of heat energy is low, and energy is wasted. Therefore, it is necessary to propose a separation and purification device for ultra-clean high-purity wet electronic chemicals that can save energy and improve purification efficiency. Summary of the invention
[0004] In order to solve the above-mentioned problems, the purpose of the present invention is to provide a separation and purification device for ultra-clean high-purity wet electronic chemicals. Through the coordination of electrolysis components, adsorption components, heaters and cooling components, it is beneficial to remove metal ion impurities and particulate impurities in wet electronic chemicals, obtain ultra-clean high-purity wet electronic chemicals, improve purity and save energy.
[0005] In order to achieve the above-mentioned purpose, the technical scheme of the present invention is as follows: it comprises a heating kettle, a cooling component and a collecting box, wherein a heating chamber and a discharge chamber are arranged from top to bottom inside the heating kettle, the cooling component is connected with the heating chamber and a first solenoid valve is arranged at the connection point and is close to the top of the heating kettle, the cooling component is connected with an electrolysis component at one end away from the heating kettle, the electrolysis component is connected with the collecting box, a stirring rod is arranged in the heating chamber, a motor is fixedly connected with the top of the heating kettle, the top of the stirring rod passes through the heating kettle and is coaxially fixedly connected with the output shaft of the motor, a plurality of stirring blades are fixedly connected with the stirring rod, a discharge pipe is arranged in the discharge chamber, one end of the discharge pipe is connected with the heating chamber and a second solenoid valve is arranged at the connection point, the other end of the discharge pipe passes through the inner wall of the discharge chamber and extends to the outside of the heating kettle, a cleaning pipe connected with the heating chamber is arranged on the surface of the heating kettle, a third solenoid valve is arranged on the cleaning pipe, a heater is fixedly connected with the top wall of the discharge chamber, an adsorption component for adsorbing ions and particulate matter is connected with the collecting box, a pressure gauge connected with the heating chamber is arranged at the top of the heating kettle, a temperature sensor is arranged on the inner wall of the heating chamber, a storage component is connected with the top of the heating kettle and a fourth solenoid valve is fixedly connected with the connection point;
[0006] The electrolysis assembly includes an electrolysis box body fixed on the top of the collection box, wherein a shunt pipe, a confluence pipe and a plurality of electrolysis tubes are respectively arranged inside the electrolysis box body, one end of each electrolysis tube is connected to the shunt pipe, and the other end of each electrolysis tube is connected to the confluence pipe, one end of the shunt pipe extends through the electrolysis box body to the outside of the electrolysis box body and is connected to a cleaning tank for cleaning the electrolysis tube, one end of the confluence pipe extends through the electrolysis box body to the outside of the electrolysis box body and is connected to a cleaning recovery tank for recovering the cleaning liquid of the electrolysis tube, the shunt pipe is connected to the cooling assembly, and the confluence pipe is connected to a fifth delivery pipe, which is far away from one end of the confluence pipe. Passing through the electrolysis box and connected to the collection box, the inner wall of the electrolysis tube is embedded with a negative electrode plate for reducing metal ions in the wet electronic chemical liquid, the negative electrode plate is electrically connected to a negative charge generator, the inner wall of the electrolysis box is fixedly connected with a plurality of positive electrode plates, the positive electrode plates are all electrically connected to the negative charge generator, the chamber of the electrolysis box is filled with electrolyte, the bottom of the shunt tube is provided with an ion exchange membrane for unidirectional flow of anions in the solution in the shunt tube to the electrolyte, and the shunt tube, the confluence tube and the fifth delivery tube are respectively fixedly connected with a fifth electromagnetic valve, a sixth electromagnetic valve and a seventh electromagnetic valve;
[0007] The motor, the temperature sensor, the first solenoid valve, the second solenoid valve, the third solenoid valve, the fourth solenoid valve, the fifth solenoid valve, the sixth solenoid valve, the seventh solenoid valve, the negative charge generator, the pressure gauge and the heater are all electrically connected to the controller.
[0008] The principle of the basic scheme is: wet electronic chemicals are put into the heating chamber inside the heating kettle through the material storage component, and then the wet electronic chemicals in the heating chamber are heated by the heater, and stirred by the stirring blades at the same time, so that the wet electronic chemicals are heated faster and preliminarily purified, and then the corresponding wet electronic chemical gas generated flows to the condenser through the conduit, and is cooled by the condenser to re-form liquid, and then flows into the electrolysis tube in the electrolysis box through the conduit, and the metal ions in the solution are reduced to metal elements by electrons by providing negative charges to the negative electrode plates therein, and attached to the negative electrode plates, and then the solution flows into the fifth conveying pipe through the manifold and into the collection box, and then the liquid after electrolysis treatment is further treated with ions and particulate matter adsorption by the adsorption component, and then flows into the product tank to form the final product, that is, ultra-clean high-purity wet electronic chemicals;
[0009] At the same time, the temperature of the wet electronic chemicals in the heating chamber and the air pressure value in the heating chamber are constantly monitored through a pressure gauge, a temperature sensor and a controller.
[0010] The beneficial effects of the basic scheme are: 1. Through the negative electrode plate inside the electrolysis tube and the negative charge generator that provides negative charge to the negative electrode plate, when the wet electronic chemical liquid after distillation and condensation flows through the electrolysis tube, the metal ions (potassium ions, sodium ions, calcium ions, iron ions, cobalt ions, zinc ions and other metal ions) therein obtain the negative charge on the negative electrode plate, and are thereby reduced to metal elements and attached to the surface of the negative electrode plate, thereby achieving an efficient purification effect on the wet electronic chemicals.
[0011] 2. When the storage component is located near the top of the heating kettle, it can absorb the heat dissipated during the distillation of the heating kettle to preheat the untreated wet electronic chemicals inside the storage component, thereby reducing energy consumption.
[0012] 3. The design of the adsorption component is to adsorb the metal ions in the liquid after the electrolysis treatment, such as potassium ions, sodium ions, calcium ions, iron ions, zinc ions, aluminum ions and calcium ions, so as to further improve the purity of wet electronic chemicals.
[0013] 4. During distillation, the wet electronic chemicals in the heating chamber are stirred by stirring blades to speed up their flow, thereby accelerating heat transfer and making the wet electronic chemicals heat up more evenly, thereby improving distillation efficiency; at the same time, the rotation of the stirring blades can reduce the possibility of particulate impurities adhering to the stirring blades, thereby improving the filtering effect of subsequent distillation gas when passing through the stirring blades, so as to improve product purity.
[0014] Furthermore, the cooling assembly includes a conduit connected to the heating chamber, a condenser and a water pump. The end of the conduit away from the heating kettle passes through the condenser along the length direction of the condenser and extends to the electrolysis box body and is connected to the shunt pipe. The connection between the conduit and the condenser is a fixed connection. The water inlet and water outlet of the condenser are both connected to an inlet pipe and an outlet pipe. The inlet pipe is connected to the output end of the water pump, the outlet pipe is connected to the material storage assembly, and the input end of the water pump is connected to the cooling box. The part of the conduit located in the condenser is spiral, and the end of the conduit close to the heating kettle is located above the end of the conduit close to the collecting box.
[0015] The beneficial effect of the basic scheme is that when the distilled gas reaches the condenser through the conduit, the distilled gas is cooled by the condenser, so that the wet electronic chemicals are re-condensed into liquid and flow into the electrolysis box along the conduit for electrolysis treatment. At the same time, the coolant in the condenser is circulated through the water pump, thereby improving the distillation efficiency.
[0016] Furthermore, the condenser is divided into a first condensation chamber and a second condensation chamber from outside to inside. The inner wall of the second condensation chamber is provided with a plurality of connecting holes connected to the first condensation chamber. The water inlet of the condenser is connected to the first condensation chamber, and the water outlet of the condenser is connected to the second condensation chamber.
[0017] The beneficial effect of the basic scheme is: dividing the condenser into a first condensation chamber and a second condensation chamber can increase the residence time of the condensate in the condenser, allowing sufficient heat exchange, and at the same time enable the coolant that absorbs more heat to be discharged first, thereby improving the condensation efficiency and saving energy.
[0018] Furthermore, the connection between the heating chamber and the discharge chamber is arc-shaped; a sealing ring is provided at the connection between the stirring rod and the heating kettle, and the sealing ring material is polytetrafluoroethylene.
[0019] The beneficial effects of the basic scheme are: the connection between the heating chamber and the discharge chamber is an arc-shaped design, which can increase the heating area while making the wet electronic chemicals in the heating chamber evenly heated, thereby improving the distillation efficiency and safety; through the design of the polytetrafluoroethylene sealing ring, the sealing of the heating chamber during distillation is improved, thereby improving the distillation efficiency.
[0020] Furthermore, the adsorption component includes a supply pump, a plurality of adsorption columns and a liquid level sensor arranged in a collecting box, the input end of the supply pump is connected to the inside of the collecting box, the output end of the supply pump is connected to a first three-way valve, the first three-way valve is respectively connected to a first delivery pipe and a de-washing pipe, the de-washing pipe is connected to a de-washing pump, the input end of the de-washing pump is connected to a de-washing tank, the first delivery pipe is connected to a plurality of second delivery pipes, an adsorption cavity is provided in each adsorption column, the second delivery pipes are connected to the adsorption cavity, the adsorption cavity is filled with adsorption materials for adsorbing metal ions, a third delivery pipe connected to the adsorption cavity is provided at the bottom of the adsorption column, the third delivery pipe is connected to a fourth delivery pipe, the fourth delivery pipe is connected to a second three-way valve, the second three-way valve is respectively connected to a finished product tank and a de-washing recovery tank, the supply pump, the de-washing pump and the liquid level sensor are electrically connected to the controller.
[0021] The beneficial effect of the basic scheme is that the wet electronic chemical liquid in the collection box is transported to the adsorption column through the supply pump, and the metal ions in the solution, such as sodium ions, potassium ions, calcium ions, zinc ions, iron ions, cobalt ions and nickel ions, are adsorbed by the adsorption material in the adsorption column, thereby improving the purity of the final product.
[0022] Furthermore, a plurality of filtering holes are opened on the surface of the stirring blades; and the stirring blades are staggeredly distributed from top to bottom along the stirring rod.
[0023] The beneficial effects of the basic scheme are: the design of the filter holes can filter the particulate impurities in the wet electronic chemicals once when they are put in, and can reduce the possibility of bringing the particulate impurities in the liquid into the conduit when the wet electronic chemicals are heated to generate bubbles, thereby improving the purity; the design of the stirring blades staggered from top to bottom along the stirring rod can provide sufficient flow space for the flow of distilled gas while filtering, thereby improving the distillation efficiency.
[0024] Furthermore, a pressure reducing port connected to the heating chamber is provided on the top of the heating kettle, the pressure reducing port is connected to a vacuum pump, and the vacuum pump is connected to the controller signal.
[0025] The beneficial effect of the basic scheme is that the gas pressure in the heating chamber is reduced by a vacuum pump, thereby reducing the boiling point of wet electronic chemicals, thereby improving the distillation efficiency and saving energy.
[0026] Furthermore, the collecting box, product tank, de-washing tank, de-washing recovery tank, diversion pipe, converging pipe, fifth delivery pipe, first delivery pipe, de-washing pipe, second delivery pipe, third delivery pipe and fourth delivery pipe are all lined with polytetrafluoroethylene; the collecting box, first delivery pipe and the pipe connecting the de-washing tank with the supply pump are all lined with polytetrafluoroethylene, and the pipe connecting the de-washing reflux tank and the product tank with the fourth delivery pipe are all lined with polytetrafluoroethylene.
[0027] The beneficial effects of the basic solution are: through the design of polytetrafluoroethylene lining of pipes and tanks, it is ensured that the solution after electrolysis will not be contaminated by subsequent processes, thereby affecting the purity of the final product; at the same time, it can also protect various components from being corroded by wet electronic chemicals and ultra-clean high-purity wet electronic chemicals.
[0028] Furthermore, the material storage component includes a storage bin, inside which a spiral preheater for preheating chemicals is arranged from top to bottom, the water inlet and outlet of the preheater are respectively located at the top and bottom of the storage bin, and the water outlet of the preheater is connected to the cooling box.
[0029] The beneficial effect of the basic solution is that the wet electronic chemicals in the storage bin are preheated by the spiral preheater, thereby reducing the energy consumption during distillation and thus improving the distillation efficiency.
[0030] Further, an application of a separation and purification device for ultra-clean high-purity wet electronic chemicals comprises the following steps:
[0031] Step 1: Feeding and decompression: wet electronic chemicals are fed into the heating chamber inside the heating kettle through the storage bin, and then the air pressure in the heating chamber is reduced by a vacuum pump;
[0032] Step 2, heating and stirring: heating the liquid in the heating chamber by a heater, and starting a motor to stir the wet electronic chemicals by rotating a stirring blade;
[0033] Step 3, condensation preheating: the distilled gas formed after the wet electronic chemicals are heated flows through the condenser through the conduit at the top of the heating kettle to be condensed, and then flows into the electrolysis box; at the same time, the heated condensate flows into the preheater, so that the preheater is heated and the crude product in the storage bin is preheated;
[0034] Step 4, electrolysis treatment: the condensed wet electronic chemical liquid will flow into the shunt pipe, and then flow into each electrolysis tube. The negative charge generator is controlled by the controller so that the negative electrode plate therein is negatively charged, so that the metal ions in the solution obtain electrons and attach to the negative electrode plate. Then the liquid flows into the confluence pipe after the electrolysis tube, and then flows into the collection box through the fifth delivery pipe.
[0035] Step 5, adsorption by adsorption material: the liquid in the collection box passes through the adsorption column, and the residual ions and particulate matter therein are adsorbed by the adsorption material, and then the adsorbed liquid flows into the finished product tank lined with polytetrafluoroethylene to obtain ultra-clean high-purity wet electronic chemicals;
[0036] Step six, cleaning and regeneration: After the distillation is completed, the impurities in the heating chamber are cleaned by rotating the cleaning tube and the stirring blades, and discharged from the heating chamber through the discharge pipe; at the same time, the adsorption material is regenerated by injecting desolvation liquid into the adsorption column; the cleaning liquid is injected into the electrolysis tube through the shunt tube to clean the metal ions on the surface of the negative electrode plate to regenerate it; after cleaning and regeneration, the cleaning degree is checked.
[0037] The beneficial effects of the basic scheme are: removing some metal ion impurities and particulate impurities in the liquid by vacuum distillation of the wet electronic chemicals, and then condensing and collecting them, and then adsorbing the metal ions in the condensed and collected liquid by capacitors, and then adsorbing the ions and particulate matter in the liquid after electrolysis by the adsorption material in the adsorption column, thereby further removing the ions and particulate matter impurities in the wet electronic chemicals through the triple ion and particulate matter removal steps, thereby improving the cleanliness of the wet electronic chemicals and obtaining ultra-clean high-purity wet electronic chemicals; performing a cleaning degree inspection after cleaning and regeneration can reduce the possibility of affecting the purity of subsequent ultra-clean high-purity wet electronic chemicals separation and purification due to incomplete cleaning. BRIEF DESCRIPTION OF THE DRAWINGS
[0038] Figure 1 Schematic diagram of the application of the ultra-clean high-purity wet electronic chemicals separation and purification device in an embodiment of the present invention;
[0039] Figure 2 It is an axonometric diagram of a device for separating and purifying ultra-clean high-purity wet electronic chemicals in an embodiment of the present invention;
[0040] Figure 3 It is a cross-sectional view of a heating kettle of a device for separating and purifying ultra-clean high-purity wet electronic chemicals in an embodiment of the present invention;
[0041] Figure 4 It is a front cross-sectional view of the electrolysis component of the ultra-clean high-purity wet electronic chemical separation and purification device in an embodiment of the present invention.
[0042] The figure marks in the drawings of the specification include: heating kettle 1, conduit 2, motor 3, cleaning pipe 4, supply pump 5, stirring rod 6, stirring blade 7, discharge pipe 8, heater 9, condenser 10, collecting box 11, storage bin 12, pressure reducing port 13, first solenoid valve 14, third solenoid valve 15, second solenoid valve 16, vacuum pump 17, water inlet pipe 18, water outlet pipe 19, pressure gauge 20, temperature sensor 21, de-washing recovery tank 22, finished product tank 23, second three-way valve 24, fourth delivery pipe 25, adsorption column 26, first delivery pipe 27, de-washing tank 28, de-washing pump 29, first three-way valve 30, electrolysis box 31, diverter pipe 32, electrolysis tube 33, confluence pipe 34, fifth delivery pipe 35. DETAILED DESCRIPTION
[0043] The following is further described in detail through specific implementation methods:
[0044] Embodiment 1:
[0045] Basically as attached Figure 1 , Figure 2 , Figure 3 and Figure 4 As shown: a separation and purification device for ultra-clean high-purity wet electronic chemicals, including a heating kettle 1, a cooling component and a collecting box 11, a heating chamber and a discharge chamber are arranged inside the heating kettle 1 from top to bottom, the connection between the bottom wall of the heating chamber and the discharge chamber is arc-shaped, the cooling component is connected to the heating chamber and the connection is threadedly connected to a first electromagnetic valve 14 and is close to the top of the heating kettle 1, the other end of the cooling component is connected to the collecting box 11, a stirring rod 6 is arranged in the heating chamber, a motor 3 is fixedly connected to the top of the heating kettle 1, the top end of the stirring rod 6 passes through the heating kettle 1 and is coaxially fixedly connected to the output shaft of the motor 3, a sealing ring is fixedly connected to the connection between the stirring rod 6 and the heating kettle 1, a plurality of stirring blades 7 are fixedly connected to the stirring rod 6, and the stirring A plurality of filter holes are provided on the surface of the mixing blade 7, a discharge pipe 8 is fixedly connected in the discharge chamber, one end of the discharge pipe 8 is connected to the heating chamber and a second solenoid valve 16 is threadedly connected at the connection point, the other end of the discharge pipe 8 passes through the inner wall of the discharge chamber and extends to the outside of the heating kettle 1, a cleaning pipe 4 connected to the heating chamber is provided on the surface of the heating kettle 1, a third solenoid valve 15 is threadedly connected to the cleaning pipe 4, a heater 9 is fixedly connected to the top wall of the discharge chamber, a pressure gauge 20 connected to the heating chamber is provided on the top of the heating kettle 1, a temperature sensor 21 is provided on the inner wall of the heating chamber, an adsorption component for adsorbing ions and particulate matter is connected to the collection box 11, a material storage component is connected to the top of the heating kettle 1 and a fourth solenoid valve is fixedly connected at the connection point;
[0046] The electrolysis assembly includes an electrolysis box 31 fixed to the top of the collection box, and the electrolysis box 31 is provided with a shunt pipe 32, a confluence pipe 34 and a plurality of electrolysis tubes 33, one end of each electrolysis tube 33 is connected to the shunt pipe 32, and the other end of each electrolysis tube 33 is connected to the confluence pipe 34. One end of the shunt pipe 32 extends through the electrolysis box 31 to the outside of the electrolysis box 31 and is connected to a cleaning tank for cleaning the electrolysis tubes 33. One end of the confluence pipe 34 extends through the electrolysis box 31 to the outside of the electrolysis box 31 and is connected to a cleaning tank for recovering the electrolysis tubes 33. 3 cleaning liquid cleaning recovery tank, the shunt pipe 32 is connected to the cooling assembly, the manifold 34 is connected to the fifth delivery pipe 35, the end of the fifth delivery pipe 35 away from the manifold 34 passes through the electrolysis box 31 and is connected to the collection box 11, the inner wall of the electrolysis tube 33 is embedded with a negative electrode plate for adsorbing metal ions in the wet electronic chemical liquid, the negative electrode plate is electrically connected to the negative charge generator, the inner wall of the electrolysis box 31 is bonded with a plurality of positive electrode plates, the positive electrode plates are all electrically connected to the negative charge generator, and the chamber of the electrolysis box 31 is filled with electrolyte , an ion exchange membrane for unidirectional flow of anions in the solution in the shunt tube 32 to the electrolyte is provided at the bottom of the shunt tube 32, and a fifth solenoid valve, a sixth solenoid valve and a seventh solenoid valve are fixedly connected to the shunt tube 32, the confluence tube 34 and the fifth delivery pipe 35 respectively; and in order to ensure the safety of the electrolysis process, the electrolysis box 31 and the electrolysis tube 33 are lined with insulating materials with good chemical stability and solubility resistance, such as polytetrafluoroethylene, high-strength polyethylene, polyimide (PI), polyether ketone (PEEK), polystyrene (PS) and polyamide (PA) which perform well in ultra-clean high-purity wet electronic chemical solutions or wet electronic chemicals such as NMP, and the selection of specific insulating materials can be determined according to actual conditions; at the same time, it can minimize the interference between different electrolysis tubes 33, thereby achieving good insulation and electrolysis effect; and after the negative electrode plate has worked for a certain period of time, the negative electrode plate needs to be cleaned or replaced to avoid the metal element deposited on its surface reducing the subsequent work efficiency of removing metal ions.
[0047] The motor 3, the temperature sensor 21, the first solenoid valve 14, the second solenoid valve 16, the third solenoid valve 15, the fourth solenoid valve, the fifth solenoid valve, the sixth solenoid valve, the seventh solenoid valve, the negative charge generator, the pressure gauge 20 and the heater 9 are all connected to the controller signal, so that when the wet electronic chemicals are distilled and purified in the heating kettle 1, the temperature and pressure values in the heating chamber can be accurately controlled according to the distillation requirements of the wet electronic chemicals, thereby improving the distillation efficiency and reducing energy consumption.
[0048] The cooling assembly includes a conduit 2 connected to the heating chamber, a condenser 10 and a water pump. One end of the conduit 2 passes through the condenser 10 along the length direction of the condenser 10 and extends into the electrolysis box body 31 and is connected to the shunt pipe 32. The connection between the conduit 2 and the condenser 10 is a fixed connection. The water inlet and the water outlet of the condenser 10 are both connected to the water inlet pipe 18 and the water outlet pipe 19. The water inlet pipe 18 is connected to the output end of the water pump, the water outlet pipe 19 is connected to the material storage assembly, and the water pump input end is connected to the cooling box. The part of the conduit 2 located in the condenser 10 is spiral to increase the contact area between the conduit 2 and the coolant in the condenser 10, improve the condensation efficiency, and then improve the distillation efficiency. The end of the conduit 2 close to the heating kettle 1 is located above the end of the conduit 2 close to the collecting box 11.
[0049] The material storage component includes a material storage bin 12, and a spiral preheater for preheating wet electronic chemicals is arranged from top to bottom inside the material storage bin 12. The water inlet and outlet of the preheater are respectively located at the top and bottom of the material storage bin 12. The water outlet of the preheater is connected to the cooling box to preheat the wet electronic chemicals that have not been separated and purified, thereby saving energy.
[0050] The adsorption assembly includes a supply pump 5, a plurality of adsorption columns 26 and a liquid level sensor arranged in a collection box. The input end of the supply pump 5 is connected to the inside of the collection box 11, and the output end of the supply pump 5 is connected to a first three-way valve 30. The first three-way valve 30 is respectively connected to a first delivery pipe 27 and a de-washing pipe. The de-washing pipe is connected to a de-washing pump 29. The input end of the de-washing pump 29 is connected to a de-washing tank 28. The first delivery pipe 27 is connected to a plurality of second delivery pipes. The adsorption columns 26 are each provided with an adsorption cavity. The second delivery pipes are each connected to the adsorption cavity. The adsorption cavity is filled with an adsorption material. The adsorption material is one of PTFE, HDPE, PC, PMMA, etc. One or more kinds of materials are used to further adsorb metal ions so that the wet electronic chemicals can reach the electronic grade. The bottom of the adsorption column 26 is provided with a third delivery pipe connected to the adsorption chamber. The third delivery pipe is connected to the fourth delivery pipe 25. The fourth delivery pipe 25 is connected to the second three-way valve 24. The second three-way valve 24 is respectively connected to the finished product tank 23 and the de-washing recovery tank 22. The supply pump 5 and the de-washing pump 29 are electrically connected to the liquid level sensor. All the sealing connections of the device are provided with sealing rings made of PTFE material, which utilizes its excellent properties such as strong corrosion resistance, high temperature resistance and weather resistance to ensure the wet electronic chemicals during the distillation and purification process.
[0051] The specific implementation process is as follows: the separation and purification of some wet electronic chemicals can be processed by distillation. For example, taking NMP, a wet electronic chemical with good thermal stability, as an example, first, the fourth solenoid valve is opened by the controller to allow the NMP liquid that needs to be separated and purified in the storage bin 12 to flow into the heating chamber, and then the fourth solenoid valve is closed, and the heater 9 is started to heat the liquid in the heating chamber. At the same time, the motor 3 is started. The motor 3 will drive the stirring rod 6 coaxially fixedly connected to the output shaft of the motor 3, and then drive the stirring blade 7 fixedly connected to the stirring rod 6 to stir the NMP liquid in the heating chamber, so that it can be evenly heated to prevent the liquid from heating up too quickly locally, thereby improving the distillation efficiency and distillation safety.
[0052] During the heating process, the NMP distillation temperature and distillation pressure need to be strictly controlled to ensure that it is distilled under a vacuum of -0.97MPa and the distillation temperature is not higher than 132°C. Although NMP has a certain high-temperature stability, when the temperature exceeds 400°C, the bonds in the NMP molecules begin to break, producing gas and other compounds. This decomposition reaction is an exothermic process, which is accompanied by intense reactivity and possible explosion hazards. Therefore, the temperature sensor 21 is required to monitor the temperature of the liquid in the heating chamber at all times and transmit the temperature data to the controller, which analyzes these data and controls the heater 9 to make corresponding power adjustments, thereby accurately controlling the distillation temperature of NMP. At the same time, in order to further reduce the temperature of NMP distillation to improve safety and distillation efficiency, the air pressure in the heating chamber is reduced by the vacuum pump 17, so that the vaporization temperature of the NMP liquid is reduced, and then the temperature and pressure in the heating chamber are monitored and controlled in conjunction with the heating chamber pressure value detected by the pressure gauge 20, thereby improving the purity of the distilled product and the distillation efficiency while ensuring the safety of the entire distillation process; at the same time, the sealing ring provided at the connection between the motor 3 and the heating kettle 1 can ensure that external air does not enter the heating chamber and the internal distillation gas does not escape, thereby improving the safety and distillation efficiency of the distillation process and the purity of the product.
[0053] When the NMP liquid in the heating chamber reaches the distillation temperature, the first solenoid valve 14 connected to the controller signal is opened to allow the generated NMP gas to flow into the conduit 2 and then into the condenser 10. The portion of the conduit 2 located in the condenser 10 is spiral, which can increase the contact area between the conduit 2 and the coolant to improve the heat exchange efficiency, thereby improving the distillation efficiency and saving energy. At the same time, the coolant after heat exchange flows from the water outlet of the condenser 10 into the water outlet pipe 19, and then flows into the preheater connected to the water outlet pipe 19 through the water outlet pipe 19. When passing through the spiral preheater, since the preheater spirally surrounds the storage bin, the heat in the coolant will be transferred to the liquid in the storage bin 12, thereby preheating the unseparated and purified NMP, thereby reducing the time of the entire distillation and purification next time, so as to improve the distillation efficiency and save energy. After passing through the preheater, the coolant flows into the cooling box through the water outlet of the preheater connected to the cooling box, forming a closed loop of condensation, thereby saving energy.
[0054] During the NMP distillation process, a small amount of fine impurities in the NMP liquid may be mixed in the NMP gas and move upward with the NMP gas, passing through the stirring blade 7 during the movement. At this time, since the diameter of the filter hole on the stirring blade 7 is smaller than the diameter of these fine impurities, such as particles with a diameter of 0.03 μm, and the diameter of the filter hole is much larger than the diameter of the NMP gas molecule, these fine impurities are filtered out; these filtered fine impurities may accumulate around the filter hole and block the filter hole, affecting the subsequent filtering effect, and during the rotation of the stirring blade 7, these impurities will generate a certain centrifugal force, which forces these impurities to leave the filter hole under the action of the centrifugal force, thereby reducing the possibility of filter hole blockage, so as to improve the filtering efficiency and the purity of the NMP product.
[0055] The NMP liquid is distilled to make the content of particles greater than or equal to 0.03 μm in the condensed NMP liquid flowing into the collection box 11 less than or equal to 1500 pcs / mL, and the metal ion concentration therein is reduced; the condensed NMP liquid then flows into the shunt tube 32 through the conduit 2 connected to the shunt tube 32, and then is separated into each electrolysis tube 33 through the shunt tube 32, and at the same time, the negative charge generator is controlled by the controller to provide appropriate negative charge for the negative electrode plate in the electrolysis tube 33. Under the action of the external electric field, the metal cations in the liquid in the shunt tube 32 move toward the negative electrode plate, and the anions therein flow into the electrolyte through the ion exchange membrane, and the metal cations are The electrons on the surface of the negative electrode plate are reduced to metal elements and deposited on the surface of the negative electrode plate, thereby realizing the electrolytic cleaning of metal ions in wet electronic chemicals and improving the purity of the NMP liquid. Since the positive electrode plate will be continuously consumed during the electrolytic process, ions will be formed and dissolved in the electrolyte, which will increase the concentration of the electrolyte and affect the subsequent removal of metal ions in wet electronic chemicals. Therefore, the positive electrode plate and the electrolyte need to be replaced regularly. After the NMP liquid passes through the electrolytic tube 33, it flows into the manifold 34, and then flows into the collection box 11 through the fifth delivery pipe 35. While the NMP liquid is being electrolytically treated, the fifth solenoid valve and the sixth solenoid valve are closed, and the seventh solenoid valve is opened to ensure the normal progress of the electrolytic process. Because an external electric field is required, but the electric field may have a certain impact on other equipment, and also to ensure the safety and stability of the entire electrolysis process, the inner walls of the electrolysis box 31 and the electrolysis tube 33 are lined with polytetrafluoroethylene (PTFE), polyimide (PI) or other insulating materials that have excellent chemical stability and solubility resistance like polyimide (PI) and perform well in ultra-clean high-purity wet electronic chemical liquids such as NMP or wet electronic chemical liquids.
[0056] The NMP solution flowing into the collection box 11 after the electrolysis treatment may still contain certain large-size ions and particulates. In order to further reduce the concentration of large-size ions and particulates, during the distillation process, the liquid level sensor in the collection box 11 will always detect the liquid level of the liquid therein and transmit the liquid level information to the controller. When the liquid level reaches the preset liquid level, the controller starts the supply pump 5 to transport the NMP liquid in the collection box 11 to the adsorption column 26 through the first delivery pipe 27, so that the above liquid passes through the adsorption material, for example, the large-size ions and particulates in the NMP liquid are further adsorbed and removed, such as metal ions such as sodium ions, potassium ions, calcium ions, iron ions, cobalt ions and nickel ions and other acid radical ions in the NMP liquid, thereby further improving the purity of the NMP liquid and making the metal ion concentration therein Lower than 10ppt, reaching G5 level; at the same time, after the adsorption material is saturated or adsorbed once, the de-washing pipe is connected to the first delivery pipe 27 through the first three-way valve 30, and then the fourth delivery pipe 25 is connected to the de-washing recovery tank 22 through the second three-way valve 24, and then the de-washing pump 29 is started to make the de-washing liquid in the de-washing pipe flow into the adsorption chamber through the de-washing pipe and the first delivery pipe 27, so as to regenerate the adsorbent material therein, so as to facilitate the next adsorption and reduce costs. At the same time, the de-washed liquid flows into the de-washing recovery tank 22 through the fourth delivery pipe 25, so as to facilitate the subsequent secondary treatment and recycling of these recovered liquids, and a one-way valve is provided at the connection between the de-washing recovery tank 22 and the second three-way valve 24, so as to prevent the liquid in the de-washing recovery tank 22 from flowing back into the fourth delivery pipe 25, thereby affecting the separation and purification of NMP liquid.
[0057] After one or more distillations, the metal compound impurities and particulate impurities in the NMP liquid will remain in the heating chamber. In order to prevent these impurities from affecting the subsequent distillation efficiency and the purity of the distilled product, they are cleaned. At this time, the third solenoid valve 15 is opened to allow clean water to continue to flow into the heating chamber through the cleaning pipe 4. At the same time, the motor 3 is started to drive the stirring rod 6 and the stirring blade 7 to rotate, so that the cleaning liquid can flow fully in the heating chamber. After stirring and cleaning for a certain period of time, the second solenoid valve 16 is opened to allow the cleaning liquid to flow out through the discharge pipe 8 at the bottom of the heating chamber. The cleaning is completed and inspected to improve the purity of the subsequent distilled product.
[0058] Embodiment 2:
[0059] The difference from the above embodiment is that the condenser 10 is divided into a first condensation chamber and a second condensation chamber from the outside to the inside, and the inner wall of the second condensation chamber is provided with a plurality of connecting holes connected to the first condensation chamber, the water inlet of the condenser 10 is connected to the first condensation chamber, and the water outlet of the condenser 10 is connected to the second condensation chamber.
[0060] The specific implementation process is as follows: during condensation, the condensed water first enters the first condensation chamber through the water inlet of the condenser 10, and then flows into the second condensation chamber through the connecting hole between the first condensation chamber and the second condensation chamber, and contacts the threaded conduit 2 in the second condensation chamber and conducts heat conduction with it, and then flows out through the water outlet of the condenser 10, so that the coolant that absorbs more heat can be discharged first, so as to make full use of the coolant to absorb heat, and at the same time, it can also increase the residence time of the coolant in the condenser 10, thereby further improving the condensation efficiency.
[0061] Embodiment 3:
[0062] like Figure 3 As shown, the difference from the above embodiment is that the stirring blades 7 are staggeredly distributed along the stirring rod 6 from top to bottom.
[0063] The specific implementation process is as follows: when the temperature has not reached the boiling point of the wet electronic chemicals, the bubbles generated by heating the wet electronic chemicals may bring out the particulate impurities therein and float them in the heating chamber, and then flow into the collection box 11 through the conduit 2, so the staggered distribution of the stirring blades 7 can filter the particulate impurities therein while stirring, thereby improving the purity of the wet electronic chemicals, and can provide sufficient flow space for the flow of the distillation gas to improve the distillation efficiency.
[0064] Embodiment 4:
[0065] like Figure 2 As shown, the difference from the above embodiment is that a pressure reducing port 13 connected to the heating chamber is provided on the top of the heating kettle 1, and the pressure reducing port 13 is connected to a vacuum pump 17, and the vacuum pump 17 is connected to the controller signal. The vacuum pump 17 reduces the air pressure in the heating chamber, thereby improving the distillation efficiency and saving energy.
[0066] The specific implementation process is as follows: before distillation heating, the vacuum pump 17 is started by the controller, and the vacuum pump 17 draws air from the heating chamber through the pressure reducing port 13 connected to the heating chamber, thereby reducing the air pressure in the heating chamber and further reducing the boiling point of the wet electronic chemicals, thereby shortening the time of the entire distillation process to improve the distillation efficiency and save energy.
[0067] Embodiment 5:
[0068] like Figure 1 As shown, the difference from the above embodiment is that the application of a separation and purification device for ultra-clean high-purity wet electronic chemicals includes the following steps:
[0069] Step 1, feeding and decompression: after the fourth solenoid valve is opened, the wet electronic chemicals flow into the heating chamber from the storage bin 12, and then the fourth solenoid valve is closed, and the vacuum pump 17 is started to reduce the air pressure in the heating chamber, thereby reducing the boiling point of the wet electronic chemicals and improving the distillation efficiency.
[0070] Step 2, heating and stirring: heating the liquid in the heating chamber by the heater 9, and starting the motor 3 at the same time, stirring the wet electronic chemicals by the rotation of the stirring blade 7, so that the wet electronic chemicals are evenly heated and the heating efficiency is improved;
[0071] Step three, condensation preheating: the distilled gas formed after the wet electronic chemicals are heated flows through the conduit 2 at the top of the heating kettle 1 through the condenser 10 for condensation, and flows into the electrolysis box 31; at the same time, the heated condensate flows into the preheater, so that the preheater is heated and the crude product in the storage bin 12 is preheated.
[0072] Step 4, electrolysis treatment: the condensed wet electronic chemical liquid will flow into the shunt pipe 32, and will be diverted by the shunt pipe 32 into each electrolysis tube 33. The negative charge generator is controlled by the controller so that the negative electrode plate is filled with negative charge, so that the metal ions in the solution gain electrons, are reduced to metal elements, precipitate and adhere to the negative electrode plate, and then the liquid flows into the collector 34 after passing through the electrolysis tube 33, and then flows into the collection box 11 through the fifth delivery pipe 35.
[0073] Step 5, adsorption by adsorption material: The liquid in the collection box 11 is processed through the adsorption column 26, and the adsorption material in the adsorption column effectively adsorbs the residual large-size ions and particulate matter therein, thereby removing these impurities. After the adsorption treatment, these liquids become purer and then flow into the finished product tank 23 lined with polytetrafluoroethylene to ensure the quality of the final product and obtain ultra-clean high-purity wet electronic chemicals.
[0074] Step six, cleaning and regeneration: after the distillation is completed, open the third solenoid valve 15 to allow clean water to flow into the heating chamber through the cleaning pipe 4, and start the motor 3 to fully clean the impurities in the heating chamber, and then open the second solenoid valve 16 and discharge the impurities from the heating chamber through the discharge pipe 8 to complete the cleaning work; at the same time, it is necessary to transport the dewashing liquid in the dewashing tank 28 to the adsorption chamber through the supply pump 5, so as to dewash and regenerate the adsorbed material after adsorption, so as to facilitate the next adsorption treatment, and then collect the dewashed liquid into the dewashing recovery tank 22 for centralized recovery and treatment, which protects the environment and saves costs; and the cleaning liquid can be injected into the electrolysis tube 33 through the shunt pipe 32 to clean the metal ions on the surface of the negative electrode plate and regenerate it; after cleaning and regeneration, the cleaning degree is checked.
[0075] 1. Experimental Subjects
[0076] The same NMP liquid was evenly divided into four 1L portions of NMP liquid, three of which were separated and purified by the present device, a conventional distillation device and a conventional ion separation device, respectively. The NMP liquids obtained after separation and purification were experimental group A, control group B and control group C, and the other portion was the original solution D.
[0077] 2. Experimental Results
[0078]
[0079] Table 1 NMP separation and purification data
[0080]
[0081] Table 2 Comparison of metal ions and particles before and after separation and purification of NMP solution
[0082] The analysis and comparison of the above experimental results show that the device can improve the purity of NMP to G5 level standard, shorten the distillation purification time to save energy, and thus improve the separation and purification efficiency. In addition, the device is suitable for all wet electronic chemicals with stable chemical properties, such as γ-butyrolactone and N-butylpyrrolidone.
[0083] It should be noted that, in this article, relational terms such as first and second, etc. are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Moreover, the terms "include", "comprise" or any other variants thereof are intended to cover non-exclusive inclusion, so that a process, method, article or device including a series of elements includes not only those elements, but also other elements not explicitly listed, or also includes elements inherent to such process, method, article or device.
[0084] The above is only an embodiment of the present invention. The common sense such as the known specific structure and characteristics in the scheme is not described in detail here. The ordinary technicians in the relevant field know all the common technical knowledge in the technical field of the invention before the application date or priority date, can obtain all the existing technologies in the field, and have the ability to apply the conventional experimental means before that date. The ordinary technicians in the relevant field can improve and implement this scheme in combination with their own abilities under the enlightenment given by this application. Some typical known structures or known methods should not become obstacles for ordinary technicians in the relevant field to implement this application. It should be pointed out that for those skilled in the art, without departing from the structure of the present invention, several deformations and improvements can be made, which should also be regarded as the protection scope of the present invention, which will not affect the effect of the implementation of the present invention and the practicality of the patent. The protection scope required by this application shall be based on the content of its claims, and the specific implementation methods and other records in the specification can be used to interpret the content of the claims.
Claims
1. A separation and purification device for ultra-clean high-purity wet electronic chemicals, characterized in that: The invention comprises a heating kettle, a cooling assembly and a collecting box, wherein a heating chamber and a discharge chamber are arranged from top to bottom inside the heating kettle, the cooling assembly is connected with the heating chamber and a first solenoid valve is arranged at the connection point and is close to the top of the heating kettle, an end of the cooling assembly away from the heating kettle is connected with an electrolysis assembly, the electrolysis assembly is connected with the collecting box, a stirring rod is arranged in the heating chamber, a motor is fixedly connected with the top of the heating kettle, the top end of the stirring rod passes through the heating kettle and is coaxially fixedly connected with the output shaft of the motor, a plurality of stirring blades are fixedly connected with the stirring rod, a discharge pipe is arranged in the discharge chamber, one end of the discharge pipe is connected with the heating chamber and a second solenoid valve is arranged at the connection point, the other end of the discharge pipe passes through the inner wall of the discharge chamber and extends to the outside of the heating kettle, a cleaning pipe connected with the heating chamber is arranged on the surface of the heating kettle, a third solenoid valve is arranged on the cleaning pipe, a heater is fixedly connected to the top wall of the discharge chamber, an adsorption assembly for adsorbing ions and particulate matter is connected to the collecting box, a pressure gauge connected with the heating chamber is arranged at the top of the heating kettle, a temperature sensor is arranged on the inner wall of the heating chamber, a storage assembly is connected with the top of the heating kettle and a fourth solenoid valve is fixedly connected at the connection point; The electrolysis assembly includes an electrolysis box body fixed on the top of the collection box, wherein a shunt pipe, a confluence pipe and a plurality of electrolysis tubes are respectively arranged inside the electrolysis box body, one end of each electrolysis tube is connected to the shunt pipe, and the other end of each electrolysis tube is connected to the confluence pipe, one end of the shunt pipe extends through the electrolysis box body to the outside of the electrolysis box body and is connected to a cleaning tank for cleaning the electrolysis tube, one end of the confluence pipe extends through the electrolysis box body to the outside of the electrolysis box body and is connected to a cleaning recovery tank for recovering the cleaning liquid of the electrolysis tube, the shunt pipe is connected to the cooling assembly, the confluence pipe is connected to a fifth delivery pipe, and the fifth delivery pipe is far away from the confluence pipe. The end passes through the electrolysis box and is connected to the collection box. A negative electrode plate for reducing metal ions in the wet electronic chemical liquid is embedded in the inner wall of the electrolysis tube. The negative electrode plate is electrically connected to a negative charge generator. A plurality of positive electrode plates are fixedly connected to the inner wall of the box. The positive electrode plates are all electrically connected to the negative charge generator. The chamber of the electrolysis box is filled with electrolyte. An ion exchange membrane for unidirectional flow of anions in the solution in the shunt tube to the electrolyte is provided at the bottom of the shunt tube. A fifth electromagnetic valve, a sixth electromagnetic valve and a seventh electromagnetic valve are fixedly connected to the shunt tube, the confluence tube and the fifth delivery pipe, respectively. The motor, the temperature sensor, the first solenoid valve, the second solenoid valve, the third solenoid valve, the fourth solenoid valve, the fifth solenoid valve, the sixth solenoid valve, the seventh solenoid valve, the negative charge generator, the pressure gauge and the heater are all electrically connected to the controller.
2. The ultra-clean high-purity wet electronic chemical separation and purification device according to claim 1, characterized in that: The cooling assembly includes a conduit connected to the heating chamber, a condenser and a water pump. The end of the conduit away from the heating kettle passes through the condenser along the length direction of the condenser and extends into the electrolysis box body and is connected to the shunt pipe. The connection between the conduit and the condenser is a fixed connection. The water inlet and outlet of the condenser are both connected to an inlet pipe and an outlet pipe. The inlet pipe is connected to the output end of the water pump, the outlet pipe is connected to the material storage assembly, and the input end of the water pump is connected to a cooling box. The part of the conduit located in the condenser is spiral, and the end of the conduit close to the heating kettle is located above the end of the conduit close to the collection box.
3. The ultra-clean high-purity wet electronic chemical separation and purification device according to claim 2, characterized in that: The condenser is divided into a first condensation chamber and a second condensation chamber from outside to inside. The inner wall of the second condensation chamber is provided with a plurality of connecting holes connected to the first condensation chamber. The water inlet of the condenser is connected to the first condensation chamber, and the water outlet of the condenser is connected to the second condensation chamber.
4. The ultra-clean high-purity wet electronic chemical separation and purification device according to claim 1, characterized in that: The connection between the heating chamber and the discharge chamber is arc-shaped; a sealing ring is arranged at the connection between the stirring rod and the heating kettle, and the sealing ring material is polytetrafluoroethylene.
5. The ultra-clean high-purity wet electronic chemical separation and purification device according to claim 1, characterized in that: The adsorption component includes a supply pump, a plurality of adsorption columns and a liquid level sensor arranged in a collecting box. The input end of the supply pump is connected to the inside of the collecting box, the output end of the supply pump is connected to a first three-way valve, the first three-way valve is respectively connected to a first delivery pipe and a de-washing pipe, the de-washing pipe is connected to a de-washing pump, the input end of the de-washing pump is connected to a de-washing tank, the first delivery pipe is connected to a plurality of second delivery pipes, an adsorption cavity is provided in each adsorption column, the second delivery pipes are connected to the adsorption cavity, the adsorption cavity is filled with adsorption materials for adsorbing metal ions, a third delivery pipe connected to the adsorption cavity is provided at the bottom of the adsorption column, the third delivery pipe is connected to a fourth delivery pipe, the fourth delivery pipe is connected to a second three-way valve, the second three-way valve is respectively connected to a finished product tank and a de-washing recovery tank, the supply pump, the de-washing pump and the liquid level sensor are electrically connected to the controller.
6. The ultra-clean high-purity wet electronic chemical separation and purification device according to claim 1, characterized in that: A plurality of filtering holes are provided on the surfaces of the stirring blades; the stirring blades are staggeredly distributed from top to bottom along the stirring rod.
7. The ultra-clean high-purity wet electronic chemical separation and purification device according to claim 1, characterized in that: A pressure reducing port connected to the heating chamber is arranged on the top of the heating kettle. The pressure reducing port is connected to a vacuum pump, and the vacuum pump is connected to the controller signal.
8. The ultra-clean high-purity wet electronic chemical separation and purification device according to claim 1, characterized in that: The collecting box, product tank, de-washing tank, de-washing recovery tank, diversion pipe, converging pipe, fifth delivery pipe, first delivery pipe, de-washing pipe, second delivery pipe, third delivery pipe and fourth delivery pipe are all lined with polytetrafluoroethylene; the collecting box, first delivery pipe and the pipe connecting the de-washing tank with the supply pump are all lined with polytetrafluoroethylene, and the pipe connecting the de-washing reflux tank and the product tank with the fourth delivery pipe are all lined with polytetrafluoroethylene.
9. The ultra-clean high-purity wet electronic chemical separation and purification device according to claim 1, characterized in that: The material storage component includes a material storage bin, inside which a spiral preheater for preheating chemicals is arranged from top to bottom, the water inlet and outlet of the preheater are respectively located at the top and bottom of the material storage bin, and the water outlet of the preheater is connected to a cooling box.
10. An application of a separation and purification device for ultra-clean high-purity wet electronic chemicals, based on the separation and purification device for ultra-clean high-purity wet electronic chemicals in any one of claims 1 to 9, characterized in that: The following steps are involved: Step 1: Feeding and decompression: wet electronic chemicals are fed into the heating chamber inside the heating kettle through the storage bin, and then the air pressure in the heating chamber is reduced by a vacuum pump; Step 2, heating and stirring: heating the liquid in the heating chamber by a heater, and starting a motor at the same time, stirring the wet electronic chemicals by rotating a stirring blade; Step 3, condensation preheating: the distilled gas formed after the wet electronic chemicals are heated flows through the condenser through the conduit at the top of the heating kettle to be condensed, and then flows into the electrolysis box; at the same time, the heated condensate flows into the preheater, so that the preheater is heated and the crude product in the storage bin is preheated; Step 4, electrolysis treatment: the condensed wet electronic chemical liquid will flow into the shunt pipe, and then flow into each electrolysis tube. The negative charge generator is controlled by the controller so that the negative electrode plate therein is negatively charged, so that the metal ions in the solution obtain electrons and attach to the negative electrode plate. Then the liquid flows into the confluence pipe after the electrolysis tube, and then flows into the collection box through the fifth delivery pipe. Step 5, adsorption by adsorption material: the liquid in the collection box passes through the adsorption column, and the residual ions and particulate matter therein are adsorbed by the adsorption material, and then the adsorbed liquid flows into the finished product tank lined with polytetrafluoroethylene to obtain ultra-clean high-purity wet electronic chemicals; Step 6, cleaning and regeneration: After the distillation is completed, the impurities in the heating chamber are cleaned by rotating the cleaning pipe and the stirring blades, and discharged from the heating chamber through the discharge pipe; at the same time, the adsorption material is regenerated by injecting the de-washing liquid into the adsorption column; Cleaning liquid is injected into the electrolysis tube through the shunt tube to clean the metal ions on the surface of the negative electrode plate to regenerate it; after cleaning and regeneration, the cleaning degree is checked.