An ultrahigh-purity electronic-grade hydrogen peroxide production system and production process

Abstract

This invention relates to the field of hydrogen peroxide purification technology, and particularly to an ultra-high purity electronic-grade hydrogen peroxide production system, comprising: a first buffer tank for storing hydrogen peroxide to be purified; a filtration module located at the rear end of the first buffer tank for filtering the liquid supplied from the first buffer tank; a TOC removal module located at the rear end of the filtration module, comprising a main body, a purification unit, and a spacer assembly; the main body has an internal mounting cavity, and the spacer assembly divides the mounting cavity into an inlet cavity, a purification cavity, and an outlet cavity; the purification unit is located in the purification cavity and is used for ultraviolet treatment of the liquid stream to be treated on both the inner and outer sides; a resin exchange module for ion adsorption and exchange of the liquid stream to be treated after passing through the TOC removal module; and a second buffer tank located at the rear end of the resin exchange module for storing high-purity product. The ultra-high purity electronic-grade hydrogen peroxide production system provided by this invention can perform stable continuous production and has good industrial value.

Description

Technical Field

[0001] This invention relates to the field of hydrogen peroxide purification technology, and in particular to an ultra-high purity electronic-grade hydrogen peroxide production system and production process. Background Technology

[0002] Electronic-grade hydrogen peroxide is an indispensable key wet electronic chemical in semiconductor manufacturing, integrated circuits, flat panel displays, and the photovoltaic industry. It is widely used in core processes such as wafer cleaning, photoresist stripping, surface oxidation, and micro-etching. As chip manufacturing processes continue to evolve towards advanced nodes, extremely stringent requirements are placed on the purity of hydrogen peroxide. Typically, it must meet standards such as metal ion content ≤10ppt, total organic carbon (TOC) ≤10ppb, particulate matter (≥0.1μm) ≤25 particles / mL, and a stable concentration of 31%±0.5%. Even trace impurities can easily lead to wafer surface defects, increased leakage current, or decreased device reliability. Therefore, developing efficient, stable, and low-decomposition-risk ultra-high purity hydrogen peroxide preparation technology has become a crucial link in ensuring the safety and yield improvement of the semiconductor industry chain.

[0003] The current mainstream purification process in the industry adopts a combination of "membrane separation + ultraviolet oxidation + ion exchange + precision filtration". It mainly uses industrial-grade hydrogen peroxide as raw material. The raw material is purified by two-stage reverse osmosis (RO) and then diluted to 31% by heat exchange. Then, organic impurities are oxidized and degraded by 185 nm ultraviolet irradiation (UV-TOC) to stimulate ·OH free radicals. After that, metal ions, anions and neutral elements such as silicon and boron are deeply adsorbed by mixed bed resin. Finally, particles are intercepted by nanoscale filter element and stored at low temperature.

[0004] However, these processes currently suffer from common defects: uneven light field in straight-tube UV reactors and bubbles blocking the light path lead to fluctuations in oxidation efficiency; continuous irradiation can easily cause local overheating, accelerating the decomposition of hydrogen peroxide (decomposition rate 2.5% to 4.0%); the resin is prone to degradation and channeling in strong oxidizing environments, has insufficient adsorption stability and requires frequent replacement, making it difficult to reliably meet the continuous demand for ultra-high purity in advanced processes.

[0005] Therefore, how to further improve the production process of electronic-grade hydrogen peroxide to obtain ultra-high purity electronic-grade hydrogen peroxide more stably and controllably has become a research hotspot. Summary of the Invention

[0006] The technical problem to be solved by this invention is to provide an ultra-high purity electronic-grade hydrogen peroxide production system and process, which solves the problems of incomplete TOC removal and unstable quality control in existing production processes.

[0007] To solve the above-mentioned technical problems, the technical solution adopted by the present invention is: an ultra-high purity electronic-grade hydrogen peroxide production system, comprising: The first buffer tank is used to store the hydrogen peroxide to be purified. A filtration module, located at the rear end of the first buffer tank, is used to filter the liquid delivered from the first buffer tank. The TOC removal module is located at the rear end of the filter module and includes a main body, a purification unit, and a spacer assembly. The main body has an installation cavity inside. The spacer assembly is located at the lower and upper parts of the installation cavity and divides the installation cavity into an inlet cavity, a purification cavity, and an outlet cavity. The purification unit is located in the purification cavity. The two ends of the spiral flow channel of the purification unit are connected to the inlet cavity and the outlet cavity through the liquid flow holes on the spacer assembly. The purification unit is used to perform ultraviolet treatment on both the inner and outer sides of the liquid flow to be treated entering the spiral flow channel. The resin exchange module is located at the rear end of the TOC removal module and includes at least one ion exchange tower filled with ion exchange resin. The resin exchange module is used to adsorb and exchange ions in the liquid stream to be treated after passing through the TOC removal module. The second buffer tank, located at the rear end of the resin exchange module, is used to store the high-purity products processed by the resin exchange module.

[0008] In one embodiment, the purification unit includes a first sleeve, a reflective component, a spiral channel, a second sleeve, and an ultraviolet generator. The ultraviolet generator is distributed along the length of the first sleeve and is located at the center of the first sleeve. The second sleeve is fitted onto the ultraviolet generator. The spiral channel extends spirally from the bottom of the first sleeve upwards around the top of the first sleeve. The reflective component is spaced apart on the side of the spiral channel away from the second sleeve. The reflective component is used to reflect the ultraviolet light that penetrates the spiral channel back to the spiral channel.

[0009] In one embodiment, the reflective assembly includes a rotating frame, a compensating plate, an arc-shaped reflector, and an adjusting airbag; one side of the rotating frame is hinged to the inner wall of the first sleeve, the compensating plate is embedded in the rotating frame and rotatably connected to the rotating frame, and the arc-shaped reflector is hinged to the compensating plate; the adjusting airbag is disposed at the movable end of the adjacent rotating frame, and the adjusting airbag is provided with an adjusting tube that extends to the outside of the first sleeve.

[0010] In one embodiment, the rotating frame is provided with a sliding groove, and the compensation plate is slidably and rotatably connected to the sliding groove via a sliding pin; the adjusting airbag is connected to at least the side of the adjacent rotating frame away from the rotating frame.

[0011] In one embodiment, each purification unit has at least three sets of reflective components.

[0012] In one embodiment, the purification unit is provided with end caps at both ends. The end caps are provided with communication holes for communicating with the spiral flow channel and ventilation slots for communicating with the first sleeve and the spacer assembly. The spacer assembly delivers cooling airflow into the first sleeve through the ventilation slots.

[0013] In one embodiment, the spacer assembly includes a first spacer plate, a second spacer plate, and an airflow pipe. Both the first and second spacer plates are provided with an airflow cooling chamber and a liquid flow hole that penetrates the airflow cooling chamber. The liquid flow hole is connected to a connecting hole, and the airflow cooling chamber is connected to a ventilation groove. The airflow pipe extends from the outside of the main body into the airflow cooling chamber. The airflow pipe is used to allow external cooling airflow to enter from the top of the first sleeve and exit from the bottom of the first sleeve.

[0014] In one embodiment, a sealed circuit ring cavity is provided at both ends of the airflow cooling cavity corresponding to the ultraviolet generator, and the circuit ring cavity extends to the outside of the main body through a circuit connecting pipe.

[0015] In one embodiment, each purification unit is provided with at least two spiral flow channels, and the top of the second partition plate is provided with a conical collecting cavity corresponding to the spiral flow channel, the diameter of the conical collecting cavity gradually decreasing from bottom to top.

[0016] This invention also provides a production process using any of the ultra-high purity electronic-grade hydrogen peroxide production systems described above, the steps of which are as follows: S1. The hydrogen peroxide to be treated is introduced into the first buffer tank and then sent to the filtration module for at least two stages of reverse osmosis filtration. S2. The filtered hydrogen peroxide is introduced into the TOC removal module at a temperature of 20-25℃ and a concentration of 31±0.2%. The filtered hydrogen peroxide enters the purification unit through the inlet chamber and flows upward along the spiral channel. During the flow, it is treated by ultraviolet light transmitted from both the inside and outside of the spiral channel. The ultraviolet-treated hydrogen peroxide flows out from the outlet chamber. S3. The ultraviolet-treated hydrogen peroxide is transported to the resin exchange module and flows through several ion exchange towers in sequence to deeply adsorb and remove carbonate / bicarbonate anions, metal cations, neutral elements such as silicon and boron, and residual organic matter. S4. The hydrogen peroxide purified by the resin exchange module is cooled to below 15°C and then transported to the second buffer tank for low-temperature storage, thus obtaining the ultra-high purity electronic-grade hydrogen peroxide product.

[0017] The beneficial effects of this invention are as follows: 1. The purification unit in the ultra-high purity electronic-grade hydrogen peroxide production system provided by this invention addresses the problems of transmittance fluctuations in the hydrogen peroxide system and the susceptibility of traditional single-sided irradiation to bubble blockage by employing a dual-sided ultraviolet synergy. As the liquid flows within the spiral channel, it simultaneously receives direct irradiation from the central ultraviolet generator and secondary reflected irradiation from the peripheral reflective structure. This significantly improves the utilization rate of ultraviolet light and enhances the uniformity of light intensity distribution per unit cross-section. It effectively compensates for the absorption and scattering attenuation of ultraviolet light by the fluid medium, enabling efficient decomposition of total organic carbon (TOC). This substantially reduces the downstream resin load caused by incomplete oxidation, ensuring the continuous stability of the purification process.

[0018] 2. The ultra-high purity electronic-grade hydrogen peroxide production system provided by this invention constructs a gradient-progressive closed purification chain through a directional series layout of a first buffer tank, a filtration module, a TOC removal module, a resin exchange module, and a second buffer tank. The functional modules are physically isolated by chambers and connected by directional flow channels, eliminating the risk of cross-contamination between upstream and downstream processes. Combined with the pretreatment of the filtration module and the deep degradation of TOC molecules by the TOC removal module, along with the multi-stage adsorption of the downstream resin exchange module, it achieves efficient and graded retention of inorganic ions, metallic impurities, and residual organic matter, significantly improving the overall purification effect of the system and ensuring that the final product meets the requirements for electronic-grade hydrogen peroxide.

[0019] 3. The TOC removal module provided by this invention has a compact overall structure. Through the cooperation of the purification chamber and the spiral flow channel, the hydrogen peroxide to be treated is dispersed and guided, which ensures the UV treatment effect while reducing the local heat accumulation and pressure fluctuation that may occur during the UV treatment process. This reduces the safety risk of unintended decomposition of hydrogen peroxide, thereby improving the overall operating efficiency and automation level of the system while ensuring the purification effect. It has good industrial promotion value.

[0020] Other features and beneficial effects of the invention will be set forth in the following description, and will be apparent in part from the description, or may be learned by practicing the invention. The objects of the invention and other beneficial effects may be realized and obtained by means of the structures and / or components pointed out in the description and claims. Attached Figure Description

[0021] Figure 1 This is a schematic diagram of a structure according to an embodiment of the present invention; Figure 2 This is a perspective view of the TOC removal module in one embodiment of the present invention; Figure 3 This is a top view of the TOC removal module in one embodiment of the present invention; Figure 4 for Figure 3 Cross-sectional view at point AA; Figure 5 for Figure 4 A magnified view of a section at point I; Figure 6 This is a front view of the TOC removal module in one embodiment of the present invention; Figure 7 for Figure 6 Cross-sectional view at point BB; Figure 8 for Figure 7 Enlarged view of a section at point II; Figure 9 for Figure 6 Cross-sectional view at point C; Figure 10 This is an exploded view of the internal structure of the TOC removal module in one embodiment of the present invention; Figure 11 for Figure 10 A magnified view of section III in the middle.

[0022] Label Explanation: 1. TOC Removal Module; 11. Main Body; 111. Liquid Inlet Chamber; 112. Purification Chamber; 113. Liquid Outlet Chamber; 12. Purification Unit; 121. Spiral Flow Channel; 122. First Sleeve; 123. Second Sleeve; 124. Reflector Assembly; 1241. Rotating Frame; 1242. Compensation Plate; 1243. Arc-shaped Reflector Sheet; 1244. Adjustment Airbag; 1245. Adjustment Tube; 125. Ultraviolet Generator; 126. End Cap; 1261. Ventilation Slot; 1262. Connecting Hole; 13. Spacing Assembly; 131. First Spacing Plate; 132. Second Spacing Plate; 133. Airflow Pipe; 134. Airflow Cooling Chamber; 135. Liquid Flow Hole; 136. Circuit Ring Chamber; 137. Conical Collecting Chamber; 2. First Buffer Tank; 3. Filter Module; 4. Resin Exchange Module; 5. Second Buffer Tank. Detailed Implementation

[0023] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are some embodiments of the present invention, but not all embodiments. The technical features designed in the different embodiments of the present invention described below can be combined with each other as long as they do not conflict with each other. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0024] In the description of this invention, it should be noted that all terms used in this invention (including technical and scientific terms) have the same meaning as commonly understood by one of ordinary skill in the art to which this invention pertains, and should not be construed as limiting the invention; it should be further understood that the terms used in this invention should be understood to have the same meaning as those in the context of this specification and in the relevant field, and should not be understood in an idealized or overly formal sense, except as expressly defined in this invention.

[0025] To explain in detail the technical content, objectives, and effects of the present invention, the following description is provided in conjunction with the embodiments and accompanying drawings.

[0026] Please refer to Figures 1 to 11 A high-purity electronic-grade hydrogen peroxide production system, comprising: First buffer tank 2 is used to store hydrogen peroxide to be purified; The filter module 3 is located at the rear end of the first buffer tank 2 and is used to filter the liquid delivered from the first buffer tank 2. TOC removal module 1 is located at the rear end of filter module 3 and includes a main body 11, a purification unit 12 and a spacer assembly 13. The main body 11 has an installation cavity inside. The spacer assembly 13 is located at the lower and upper parts of the installation cavity and divides the installation cavity into an inlet cavity 111, a purification cavity 112 and an outlet cavity 113. The purification unit 12 is located in the purification cavity 112. The two ends of the spiral flow channel 121 of the purification unit 12 are connected to the inlet cavity 111 and the outlet cavity 113 through the liquid flow holes 135 on the spacer assembly 13. The purification unit 12 is used to perform ultraviolet treatment on both the inner and outer sides of the liquid flow to be treated entering the spiral flow channel 121. The resin exchange module 4 is located at the rear end of the TOC removal module 1 and includes at least one ion exchange tower filled with ion exchange resin. The resin exchange module 4 is used to adsorb and exchange ions in the liquid stream to be treated after passing through the TOC removal module 1. The second buffer tank 5 is located at the rear end of the resin exchange module 4 and is used to store the high-purity product processed by the resin exchange module 4.

[0027] Because hydrogen peroxide generates heat of reaction under ultraviolet irradiation, and the carbon dioxide and trace oxygen produced by oxidation form microbubbles in the flow channel, if a traditional straight pipe structure is used, the heat cannot be dissipated in time, which will lead to local temperature rise and accelerate the thermal decomposition of hydrogen peroxide. At the same time, the accumulation of bubbles will block the ultraviolet light path and reduce the light utilization rate. Therefore, in this embodiment, the purification unit 12 includes a first sleeve 122, a reflective component 124, a spiral channel 121, a second sleeve 123, and an ultraviolet generator 125. The ultraviolet generator 125 is distributed along the length of the first sleeve 122 and is disposed at the center of the first sleeve 122. The second sleeve 123 is sleeved on the ultraviolet generator 125. The spiral channel 121 extends spirally from the bottom of the first sleeve 122 upward around the top of the first sleeve 122. The reflective component 124 is disposed at intervals on the side of the spiral channel 121 away from the second sleeve 123. The reflective component 124 is used to reflect the ultraviolet light that penetrates the spiral channel 121 back to the spiral channel 121. This configuration allows the purification unit 12 to adopt a layered structure extending axially from the center outwards. The second sleeve 123 physically isolates and protects the UV generator 125, effectively blocking strong oxidizing media and maintaining the lamp's operating temperature, ensuring the long-term operational stability of the UV generator 125. The spiral flow channel 121 allows the liquid to be treated to simultaneously receive radial direct radiation from the central UV generator 125 and secondary reflection from the outer reflective components 124 as it spirals upwards axially, forming a synergistic three-dimensional light field that significantly improves UV light utilization efficiency. Furthermore, the spiral upward flow effectively induces secondary circulation, breaking the near-wall concentration and temperature boundary layer, enhancing radial mass transfer between ·OH free radicals and trace TOC molecules, further ensuring the degradation effect of TOC molecules. Simultaneously, the secondary circulation accelerates the coalescence and floating of microbubbles, facilitating the directional escape of gas along the top of the flow channel, thereby significantly reducing the probability of dynamic bubbles blocking the UV light path and ensuring the continuity and efficiency of the organic impurity oxidation reaction.

[0028] Specifically, the second sleeve 123 is a transparent quartz sleeve; the ultraviolet generator 125 can be a 185nm low-pressure mercury lamp.

[0029] Preferably, the spiral flow channel 121 is made of transparent quartz pipe, and at least two spiral flow channels 121 are provided in each purification unit 12, so that the ultraviolet treatment is not affected when a single spiral flow channel 121 is blocked or abnormal.

[0030] If the reflective component 124 is a fixed structure, its reflection angle and radial distance from the spiral channel 121 cannot be adjusted. In actual production, it cannot be adaptively adjusted according to the specific TOC load and flow rate of different influents, resulting in a rigid overall structure and affecting purification efficiency. Therefore, in this embodiment, the reflective component 124 includes a rotating frame 1241, a compensation plate 1242, an arc-shaped reflective sheet 1243, and an adjusting airbag 1244. One side of the rotating frame 1241 is hinged to the inner wall of the first sleeve 122. The compensation plate 1242 is embedded in the rotating frame 1241 and rotatably connected to the rotating frame 1241. The arc-shaped reflective sheet 1243 is hinged to the compensation plate 1242. The adjusting airbag 1244 is located at the movable end of the adjacent rotating frame 1241. The adjusting airbag 1244 is provided with an adjusting tube 1245, which extends to the outside of the first sleeve 122. This configuration allows operators or the automatic control system to inflate or deflate the adjustment airbag 1244 via the external adjustment pipe 1245. The flexible deformation of the airbag serves as the driving force, flexibly displacing the movable end of the rotating frame 1241. This, in turn, causes the compensation plate 1242 to slide within the rotating frame 1241, synchronously causing the arc-shaped reflector 1243 to deflect at an angle, resulting in a change in radial spacing. This adjusts the reflection angle and alters the distribution of the reflected ultraviolet light field. Furthermore, using the adjustment airbag 1244 for driving filters and buffers the mechanical vibrations experienced by the reflective assembly 124 as a whole. This ensures the adjustment effect while preventing damage to the arc-shaped reflector 1243 from rigid impacts, guaranteeing the overall structural stability and improving work efficiency.

[0031] Specifically, the same air supply pressure can be used for the adjustment pipes 1245 at the same height, so that the reflection angle and spacing of the same parts of different purification units 12 are the same, ensuring the uniformity of parameter adjustment.

[0032] Specifically, the substrate of the arc-shaped reflector 1243 is titanium foil or 316L stainless steel foil with a thickness of 0.05–0.15 mm. The surface of the substrate is sequentially coated with an 80–120 nm aluminum reflective layer, a 20–40 nm MgF2 protective layer, and a 5–10 nm ALD silicon fluoride nano-coating. While ensuring the reflective and anti-oxidation effects, the arc-shaped reflector 1243 also possesses partial flexible deformation capability, thereby cooperating with the rotation of the rotating frame 1241 and the compensation plate 1242 to ensure the stability and reliability of the adjustment of the reflective assembly 124.

[0033] In this embodiment, the rotating frame 1241 is provided with a sliding groove, and the compensation plate 1242 is slidably and rotatably connected to the sliding groove via a sliding pin. The adjusting airbag 1244 is connected to at least one side of the adjacent rotating frame 1241 away from the rotating frame 1241. This arrangement makes the sliding groove and the sliding pin form a guiding mechanism. When the adjusting airbag 1244 is inflated or deflated, the resulting flexible thrust acts on the movable end of the rotating frame 1241, forcing the rotating frame 1241 to deflect around the hinge point. At the same time, the sliding pin is constrained by the trajectory of the sliding groove, causing the compensation plate 1242 to slide smoothly radially, thereby converting the deformation of the airbag into the angular deflection of the rotating frame 1241 and the radial displacement of the compensation plate 1242. This allows for the synchronous adjustment of the tilt angle of the arc-shaped reflector 1243 and its distance from the spiral flow channel 121 through the hinge point. This not only simplifies the internal transmission chain but also ensures that the arc-shaped reflector 1243 maintains a stable posture without mechanical jamming during adjustment, guaranteeing the stability and reliability of the adjustment of the reflective assembly 124.

[0034] In this embodiment, each purification unit 12 has at least three sets of reflective components 124. Preferably, each purification unit 12 has multiple segments of reflective components 124 arranged in a surrounding manner, thereby allowing for targeted adjustment of the ultraviolet light field at different heights of the purification unit 12, further improving the overall adjustability.

[0035] During the operation of the purification unit 12, a large amount of waste heat generated by the ultraviolet generator 125 during continuous irradiation cannot be dissipated in time, and the heat accumulates continuously in the end area, resulting in localized temperature rise within the purification unit 12. This localized temperature rise not only accelerates the thermal decomposition reaction of hydrogen peroxide, reducing purification efficiency, but also causes the end sealing material to age and deform due to accumulated thermal stress, potentially leading to seal failure and the infiltration of high-concentration hydrogen peroxide vapor into the electrical connection area. Long-term operation can easily cause electrode corrosion and insulation failure, threatening the operational stability of the ultraviolet generator 125 and the service life of the equipment. Therefore, in this embodiment, the purification unit 12 is provided with end caps 126 at both ends. The end caps 126 have connecting holes 1262 for communicating with the spiral flow channel 121 and venting grooves 1261 for communicating between the first sleeve 122 and the spacer assembly 13. The spacer assembly 13 delivers cooling airflow into the first sleeve 122 through the venting grooves 1261. The end cap 126 is sealed to the first sleeve 122, and the spiral flow channel 121 is connected to the liquid inlet chamber 111 through the connecting hole 1262. The venting groove 1261 is opened in the area between the end cap 126 and the first sleeve 122 and the second sleeve 123, so that the area inside the second sleeve 123 is sealed, preventing hydrogen peroxide or external factors from affecting the operation of the ultraviolet generator 125. In this way, the end cap 126 serves as a node for liquid distribution and interface sealing, separating the reaction liquid from other parts and guiding the flow to ensure continuous and stable flow. At the same time, the venting groove 1261 introduces cooling airflow into the purification unit 12, which not only removes accumulated waste heat but also prevents hydrogen peroxide decomposition. Moreover, the cooling airflow can flow directionally along the annular gap between the first sleeve 122 and the second sleeve 123 to form a protective air curtain, which further blocks the penetration of hydrogen peroxide vapor into the electrode area of ​​the ultraviolet generator 125, effectively avoiding the risks of strong oxidation corrosion and electrical short circuits, and further improving the overall reliability, safety and operational stability of the structure.

[0036] Preferably, the end cap 126 is rotatably connected. When needed, the liquid inlet and outlet of the corresponding purification unit 12 can be cut off by rotating the end cap 126, which facilitates timely blocking of liquid flow in case of production abnormality and does not affect the input of cooling airflow.

[0037] Specifically, the cooling airflow uses an inert gas. Preferably, the temperature of the inert gas is 15°C to 25°C.

[0038] Specifically, the two ends of the second sleeve 123 are sealed with the end cap 126 using double FFKM perfluoroether rubber sealing rings to ensure physical isolation of the ultraviolet generator 125.

[0039] To ensure that the gas and liquid flows do not interfere with each other, in this embodiment, the spacer assembly 13 includes a first spacer plate 131, a second spacer plate 132, and an airflow pipe 133. Both the first spacer plate 131 and the second spacer plate 132 are provided with an airflow cooling chamber 134 and a liquid flow hole 135 penetrating the airflow cooling chamber 134. The liquid flow hole 135 communicates with a connecting hole 1262, and the airflow cooling chamber 134 communicates with a venting groove 1261. The airflow pipe 133 extends from the outside of the main body 11 into the airflow cooling chamber 134. The airflow pipe 133 is used to allow external cooling airflow to enter from the top of the first sleeve 122 and exit from the bottom of the first sleeve 122. This arrangement allows the first spacer plate 131 and the second spacer plate 132 to cooperate with the purification unit 12 through the airflow cooling chamber 134 to form an independent gas circulation channel. The airflow pipe 133 guides the external cooling airflow into the purification unit 12, causing the inert cooling gas to descend along the annular gap, forming counter-current heat exchange and ensuring the heat exchange effect.

[0040] In this embodiment, sealed circuit ring cavities 136 are provided at both ends of the ultraviolet generator 125 within the airflow cooling cavity 134. The circuit ring cavities 136 extend to the outside of the main body 11 through circuit connecting pipes. The circuit ring cavities 136 keep the electrical connection lines of the ultraviolet generator 125 in a sealed state, ensuring the operational stability of the ultraviolet generator 125.

[0041] If the purification unit 12 has only a single spiral flow channel 121 or the outlet is directly connected to a straight chamber, not only will the system throughput be limited, but the multiple spiraling upward gas-liquid mixtures will easily generate disordered turbulence and pressure interference when they converge, leading to fluid deviation and pressure drop fluctuations. Therefore, in this embodiment, each purification unit 12 is provided with at least two spiral flow channels 121, and the top of the second partition plate 132 is provided with a conical collecting cavity 137 corresponding to the spiral flow channel 121. The diameter of the conical collecting cavity 137 gradually decreases from bottom to top. With this arrangement, multiple spiral flow channels 121 can improve the overall throughput and improve the uniformity of flow distribution, avoiding single-channel overload operation. When the gas-liquid mixture enters the conical collecting cavity 137, the flow cross-sectional area gradually shrinks from bottom to top, causing the axial flow velocity of the fluid to increase steadily. Combined with the centrifugal effect induced by the spiral flow, the microbubbles in the liquid flow are forced to converge towards the central axis of the cavity and accelerate to float and escape, which facilitates the subsequent separation of the gas. At the same time, the treated liquid flow rises along the conical wall to avoid dead zones and ensure the stability and effectiveness of the treatment.

[0042] Specifically, the filter module 3 can use a two-stage reverse osmosis (RO) membrane. Those skilled in the art can select a suitable RO membrane as needed, without making specific limitations.

[0043] Specifically, the resin exchange module 4 employs a three-stage series ion exchange tower, each filled with a non-renewable mixed-bed ion exchange resin. Those skilled in the art can select a suitable ion exchange resin as needed. Preferably, the resin is APV NEW-PTFE fluororesin.

[0044] Preferably, a mixing module is provided before the TOC removal module 1. The mixing module includes a mixing tank and a circulating mixer. The mixing module is used to dilute and cool the filtered hydrogen peroxide to a set concentration and stabilize it by adding ultrapure water.

[0045] This invention also provides a production process using any of the ultra-high purity electronic-grade hydrogen peroxide production systems described above, the steps of which are as follows: S1. The hydrogen peroxide to be treated is introduced into the first buffer tank 2 and then transported to the filter module 3 for at least two stages of reverse osmosis filtration. S2. The filtered hydrogen peroxide is introduced into the TOC removal module 1 at a temperature of 20-25℃ and a concentration of 31±0.2%. The filtered hydrogen peroxide enters the purification unit 12 through the liquid inlet chamber 111 and flows upward along the spiral flow channel 121. During the flow, it is treated by ultraviolet light transmitted from both the inside and outside of the spiral flow channel 121. The ultraviolet-treated hydrogen peroxide flows out from the liquid outlet chamber 113. S3. The ultraviolet-treated hydrogen peroxide is transported to the resin exchange module 4 and flows through several ion exchange towers in sequence to deeply adsorb and remove carbonate / bicarbonate anions, metal cations, neutral elements such as silicon and boron, and residual organic matter. S4. The hydrogen peroxide purified by the resin exchange module 4 is cooled to below 15°C and then transported to the second buffer tank 5 for low-temperature storage, thus obtaining the ultra-high purity electronic-grade hydrogen peroxide product.

[0046] Furthermore, those skilled in the art should understand that although many problems exist in the prior art, each embodiment or technical solution of the present invention can be improved in only one or a few aspects, without necessarily solving all the technical problems listed in the prior art or the background art simultaneously. Those skilled in the art should understand that any content not mentioned in a claim should not be construed as a limitation on that claim.

[0047] Although this document uses terms such as TOC removal module and subject extensively, the possibility of using other terms is not excluded. These terms are used merely for the convenience of describing and explaining the essence of the invention; interpreting them as any kind of additional limitation would contradict the spirit of the invention. The terms "first," "second," etc. (if present) in the specification and claims of the embodiments of the invention are used to distinguish similar objects and are not necessarily used to describe a specific order or sequence.

[0048] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, and not to limit them; although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some or all of the technical features; and these modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present invention.

Claims

1. A production system for ultra-high purity electronic-grade hydrogen peroxide, characterized in that, include: The first buffer tank (2) is used to store hydrogen peroxide to be purified; A filter module (3) is located at the rear end of the first buffer tank (2) and is used to filter the liquid delivered from the first buffer tank (2). The TOC removal module (1) is located at the rear end of the filter module (3) and includes a main body (11), a purification unit (12) and a spacer assembly (13). The main body (11) has an installation cavity inside. The spacer assembly (13) is located at the lower and upper parts of the installation cavity and divides the installation cavity into an inlet cavity (111), a purification cavity (112) and an outlet cavity (113). The purification unit (12) is located in the purification cavity (112). The two ends of the spiral flow channel (121) of the purification unit (12) are connected to the inlet cavity (111) and the outlet cavity (113) through the liquid flow holes (135) on the spacer assembly (13). The purification unit (12) is used to perform ultraviolet treatment on both the inner and outer sides of the liquid flow to be treated entering the spiral flow channel (121). The resin exchange module (4) is located at the rear end of the TOC removal module (1) and includes at least one ion exchange tower filled with ion exchange resin. The resin exchange module (4) is used to adsorb and exchange ions in the liquid stream to be treated by the TOC removal module (1). The second buffer tank (5) is located at the rear end of the resin exchange module (4) and is used to store the high-purity product processed by the resin exchange module (4).

2. The ultra-high purity electronic-grade hydrogen peroxide production system according to claim 1, characterized in that: The purification unit (12) includes a first sleeve (122), a reflective component (124), the spiral channel (121), a second sleeve (123), and an ultraviolet generator (125). The ultraviolet generator (125) is distributed along the length of the first sleeve (122) and is located at the center of the first sleeve (122). The second sleeve (123) is sleeved on the ultraviolet generator (125). The spiral channel (121) extends spirally from the bottom of the first sleeve (122) upward around the first sleeve (122) to the top of the first sleeve (122). The reflective component (124) is spaced apart on the side of the spiral channel (121) away from the second sleeve (123). The reflective component (124) is used to reflect the ultraviolet light that penetrates the spiral channel (121) back to the spiral channel (121).

3. The ultra-high purity electronic-grade hydrogen peroxide production system according to claim 2, characterized in that: The reflective assembly (124) includes a rotating frame (1241), a compensation plate (1242), an arc-shaped reflector (1243), and an adjusting airbag (1244). One side of the rotating frame (1241) is hinged to the inner wall of the first sleeve (122). The compensation plate (1242) is embedded in the rotating frame (1241) and rotatably connected to the rotating frame (1241). The arc-shaped reflector (1243) is hinged to the compensation plate (1242). The adjusting airbag (1244) is located at the movable end of the adjacent rotating frame (1241). The adjusting airbag (1244) is provided with an adjusting tube (1245), which extends to the outside of the first sleeve (122).

4. The ultra-high purity electronic-grade hydrogen peroxide production system according to claim 3, characterized in that: The rotating frame (1241) is provided with a sliding groove, and the compensation plate (1242) is slidably and rotatably connected to the sliding groove by a sliding pin; the adjusting airbag (1244) is connected to at least one side of the adjacent rotating frame (1241) away from the rotating frame (1241).

5. The ultra-high purity electronic-grade hydrogen peroxide production system according to claim 3, characterized in that: Each purification unit (12) has at least three sets of the reflective components (124).

6. The ultra-high purity electronic-grade hydrogen peroxide production system according to claim 2, characterized in that: The purification unit (12) has end caps (126) at both ends. The end caps (126) have a connecting hole (1262) for communicating with the spiral flow channel (121) and a ventilation groove (1261) for communicating with the first sleeve (122) and the spacer assembly (13). The spacer assembly (13) delivers cooling airflow into the first sleeve (122) through the ventilation groove (1261).

7. The ultra-high purity electronic-grade hydrogen peroxide production system according to claim 6, characterized in that: The spacer assembly (13) includes a first spacer plate (131), a second spacer plate (132), and an airflow pipe (133). The first spacer plate (131) and the second spacer plate (132) are each provided with an airflow cooling chamber (134) and a liquid flow hole (135) that passes through the airflow cooling chamber (134). The liquid flow hole (135) is connected to the connecting hole (1262). The airflow cooling chamber (134) is connected to the ventilation groove (1261). The airflow pipe (133) extends from the outside of the main body (11) into the airflow cooling chamber (134). The airflow pipe (133) is used to allow external cooling airflow to be input from the top of the first sleeve (122) and output from the bottom of the first sleeve (122).

8. The ultra-high purity electronic-grade hydrogen peroxide production system according to claim 7, characterized in that: The airflow cooling chamber (134) has sealed circuit ring cavities (136) at both ends corresponding to the ultraviolet generator (125), and the circuit ring cavities (136) extend to the outside of the main body (11) through circuit connecting pipes.

9. The ultra-high purity electronic-grade hydrogen peroxide production system according to claim 8, characterized in that: Each purification unit (12) is provided with at least two spiral channels (121), and the top of the second partition plate (132) is provided with a conical collecting cavity (137) corresponding to the spiral channel (121), and the diameter of the conical collecting cavity (137) gradually decreases from bottom to top.

10. A production process employing the ultra-high purity electronic-grade hydrogen peroxide production system according to any one of claims 1 to 9, characterized in that, The steps are as follows: S1. The hydrogen peroxide to be treated is introduced into the first buffer tank (2) and then transported to the filter module (3) for at least two stages of reverse osmosis filtration. S2. The filtered hydrogen peroxide is introduced into the TOC removal module (1) at a temperature of 20-25℃ and a concentration of 31±0.2%. The filtered hydrogen peroxide enters the purification unit (12) through the inlet chamber (111) and flows upward along the spiral channel (121). During the flow, it is treated by ultraviolet light transmitted from both the inside and outside of the spiral channel (121). The ultraviolet-treated hydrogen peroxide flows out from the outlet chamber (113). S3. The ultraviolet-treated hydrogen peroxide is transported to the resin exchange module (4) and flows through several ion exchange towers in sequence to deeply adsorb and remove carbonate / bicarbonate anions, metal cations, neutral elements such as silicon and boron, and residual organic matter. S4. The hydrogen peroxide purified by the resin exchange module (4) is cooled to below 15°C and then transported to the second buffer tank (5) for low-temperature storage, thus obtaining the ultra-high purity electronic-grade hydrogen peroxide product.

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