Efficient electronic sulfuric acid granularity filtering and separating device

By using multi-stage filtration units in the electronic sulfuric acid filtration system, including dynamic filtration and ultra-fine filtration, the problem that traditional technology cannot effectively remove impurities from micro-nano particles is solved, and efficient and fine filtration effect is achieved, which significantly improves the electronic sulfuric acid Purity and quality.

CN119488752APending Publication Date: 2025-02-21HUBEI SINOPHORUS ELECTRONIC MATERIALS CO LTD
View PDF 0 Cites 1 Cited by

Patent Information

Application Number
CN202411461904.4
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-10-18
Publication Date
2025-02-21

AI Technical Summary

Technical Problem

Traditional filtration and separation technologies cannot effectively remove impurities of micro-nano particles in electronic sulfuric acid, and cannot meet the needs of high-purity electronic grade chemicals.

Method used

Multi-stage filtration unit is adopted, including two stages: dynamic filtration and ultra-fine filtration. Dynamic filtration uses a hierarchical vibration filter and a rotary filter to separate particles through hydrodynamic principles and mechanical forces. Ultrafine filtration uses deep fiber filter elements and nanoscale filter media to further remove tiny particles and molecules.

Benefits of technology

It realizes efficient and fine particle size filtration and separation, significantly improves the purity and quality of electronic sulfuric acid, and meets the production needs of high-purity electronic chemicals.

✦ Generated by Eureka AI based on patent content.

Smart Images

  • Figure CN119488752A_ABST
    Figure CN119488752A_ABST
Patent Text Reader

Abstract

The invention provides an efficient electronic sulfuric acid granularity filtering and separating device. The device comprises a vibration filter, the bottom of the vibration filter is communicated with a rotary filter through a rotary filter inlet pipeline, a discharge port of the rotary filter is communicated with a feed port of a buffer tank through a pipeline via a circulating pump, and a discharge port at the bottom of the buffer tank is communicated with a superfine filter through a superfine filter inlet pipeline. The device is suitable for filtering various liquids, can efficiently and accurately remove the granularity through dynamic filtration, improves the purity and quality of electronic sulfuric acid, meets the production requirements of high-purity electronic chemicals, and has the advantages of flexibility in operation, simplicity and convenience in maintenance, high corrosion resistance and the like. The device adopts a multi-stage filtering mechanism, the mechanism comprises a dynamic filtering stage and a hyperfine filtering stage, and each stage is used for filtering particles with different sizes.
Need to check novelty before this filing date? Find Prior Art

Description

Technical Field

[0001] The invention relates to the field of preparation of high-purity electronic-grade chemicals, and in particular to a highly efficient electronic sulfuric acid particle size filtering and separation device. Background Art

[0002] Electronic grade sulfuric acid, also known as high purity sulfuric acid or ultrapure sulfuric acid, is an ultra-clean high purity reagent. It is an indispensable key basic chemical reagent in the development of microelectronics technology and one of the eight chemical reagents commonly used in the semiconductor industry. The consumption of electronic grade sulfuric acid is extremely large, accounting for about 30% of the total amount of high purity reagents, and is one of the most used chemicals in the semiconductor wafer manufacturing process.

[0003] High-purity electronic-grade chemicals play a vital role in semiconductor manufacturing, electronic component production, and other high-tech industries. These chemicals must have extremely high purity because even tiny particle contamination can cause product defects, affecting the performance and reliability of the final product. Electronic sulfuric acid (H2SO4) is a common cleaning and etching agent with a wide range of applications in the electronics industry. Therefore, it is critical to ensure the particle size control of electronic sulfuric acid.

[0004] Traditional filtration and separation technologies often fail to meet the needs of ultra-high purity electronic-grade chemicals and cannot effectively remove extremely small micro-nano particle impurities. In addition, a single filtration mechanism is difficult to cover a wide range of particle size distributions, which affects filtration efficiency and processing speed. Therefore, developing a particle size filtration and separation device that can adapt to high purity requirements, has high efficiency and reliability, is of great significance for improving the quality of electronic sulfuric acid and promoting the development of related industries. Summary of the invention

[0005] In order to solve the above problems, the present invention aims to provide a highly efficient electronic sulfuric acid particle size filtering and separation device.

[0006] The technical solution of the present invention is as follows: The present invention relates to a highly efficient electronic sulfuric acid particle size filtering and separation device, aiming to provide a solution that can effectively remove particles of different sizes and improve filtering efficiency. The device adopts a multi-stage filtering unit, including two stages of dynamic filtering and ultra-fine filtering, and each stage filters particles of different sizes to achieve the best filtering effect.

[0007] A high-efficiency electronic sulfuric acid particle size filtering and separation device, the device comprises an oscillating filter, the bottom of the oscillating filter is connected to the rotary filter through a rotary filter inlet pipe, the rotary filter discharge port is connected to the buffer tank feed port through a pipeline via a circulation pump, and the buffer tank bottom discharge port is connected to the ultra-fine filter through an ultra-fine filter inlet pipe. Preferably, the vibration filter comprises a first vibration baffle and a second vibration baffle of upper and lower layers, the first vibration baffle and the second vibration baffle have the same structure, including a vibration baffle frame, a vibration baffle filter is provided on the vibration baffle frame, and the first vibration baffle is driven by a vibration baffle drive motor.

[0008] Further preferably, the upper portion of the first vibration baffle is communicated with the first vibration filter housing, and the upper portion of the second vibration baffle is communicated with the second vibration filter housing.

[0009] Preferably, the oscillating filter is provided with a filtering solution inlet pipe, and a particle size detector is provided on the filtering solution inlet pipe.

[0010] Preferably, a rotary filter screen is provided inside the rotary filter, and a rotary filter housing is provided outside the rotary filter screen.

[0011] Further preferably, the rotary filter filtration solution inlet pipe passes through the rotary filter connector, the rotary filter drive motor and is connected to the interior of the rotary filter, and the rotary filter drive motor drives the rotary filter filter screen to rotate.

[0012] Further preferably, the ultrafine filter comprises an ultrafine filter first layer, an ultrafine filter second layer, an ultrafine filter third layer and an ultrafine filter housing, which are arranged right inside and outside.

[0013] More preferably, the pore size of the first layer filter element of the ultrafine filter is 100 nm-50 nm, the pore size of the second layer filter element of the ultrafine filter is 50 nm-20 nm, and the pore size of the third layer filter element of the ultrafine filter is 20 nm-2 nm. Specifically, the dynamic filtration unit includes a graded vibration filter and a rotary filter, which utilizes the principle of fluid dynamics to improve the particle separation efficiency through a centrifugal separation mechanism. The graded vibration filter and the rotary filter can change the flow direction of the fluid or apply mechanical force to separate the particles from the fluid. The dynamic filtration system is adjusted according to the characteristics of the particles to achieve the best filtration effect.

[0014] The ultra-fine filtration unit uses a deep fiber filter element and nano-scale filtration media, such as ultrafiltration membrane or nanofiltration membrane, to remove almost all tiny particles and molecules. The material selection of the fiber filter element takes into account acid resistance and mechanical strength, such as polypropylene, polytetrafluoroethylene, etc. The deep structure of the filter element allows the fluid to form a multi-level filtration when passing through the filter material, increasing the chance of particle capture.

[0015] Between each filtration stage, a detection point is set up to monitor the particles in the fluid in real time using a high-precision particle size analyzer to ensure that the filtration effect meets the requirements. The design of the filtration system allows independent control of each stage, and the filtration parameters such as flow rate, pressure and filter element replacement frequency can be adjusted according to actual needs.

[0016] Through the above technical scheme, the present invention can achieve efficient and fine particle size filtration and separation, improve the purity and quality of electronic sulfuric acid, and meet the production needs of high-purity electronic chemicals.

[0017] The first vibration baffle and the second vibration baffle of the vibration filter are made of corrosion-resistant PFA skeleton and PFA filter material to adapt to the corrosive environment of chemicals such as electronic sulfuric acid.

[0018] The driving mechanism: The driving mechanism of the oscillating baffle is driven by a vibrating baffle driving motor, which is used to generate and control the oscillating motion of the baffle. The motor uses a conventional stepping motor, and when entering the vibration filter: the vibrating baffle driving motor works in the vibration mode, so that the oscillating baffle can oscillate back and forth at a preset frequency and amplitude. The oscillation frequency of the vibrating baffle driving motor is 10-60Hz, and the oscillating motion helps the particles in the fluid to be separated by the PFA filter on the vibrating baffle and deposited on the baffle surface.

[0019] A detection point is set at the front end of the liquid entering the primary vibration filter inlet. The detection point is connected to a high-precision particle size analyzer via an online sampling pipeline to measure the particle size distribution and concentration of particles in the fluid.

[0020] Each level of vibration filter is designed with an independently adjustable vibration frequency to meet the filtering requirements of different particle sizes. In the first-level primary vibration filter, larger particles are separated by a lower vibration frequency.

[0021] In the second-stage primary vibration filter, smaller particles are further filtered through a higher vibration frequency. In order to achieve precise adjustment of the vibration frequency, the first-stage primary vibration filter and the second-stage primary vibration filter are equipped with a frequency regulator, which drives the motor connected to the control system of the vibration filter.

[0022] The frequency regulator can adjust the oscillation frequency according to the particle size of the particles and the fluid pressure parameters. By real-time monitoring the concentration and particle size distribution of the particles in the fluid, the frequency regulator can dynamically optimize the oscillation frequency to achieve the best filtering effect.

[0023] In the first vibration baffle first stage primary vibration filter, the vibration frequency is usually set in a lower range, 10-30 Hz, to separate larger particles. In the second vibration baffle second stage primary vibration filter, the vibration frequency is set in a higher range, 30-60 Hz, to separate smaller particles. The primary vibration filter is connected to the rotary filter through a pipeline. The liquid filtered by the primary vibration filter flows into the rotary filter through the pipeline. The inlet and outlet of the rotary filter are both provided with pipes. The inlet pipe is used to receive the fluid from the primary vibration filter, and the outlet pipe is used to discharge the fluid after further processing by the rotary filter.

[0024] The internal design of the rotary filter adopts a centrifugal separation mechanism. When the fluid enters the rotary filter, due to the rotation, the particles are pushed to the filter wall under the action of centrifugal force, thereby achieving effective separation of particles and fluid. The rotation speed of the rotary filter can be adjusted according to parameters such as the particle size and density of the particles and the flow rate and pressure of the fluid to optimize the particle separation effect.

[0025] The rotation frequency of the rotary filter ranges from 100-300 RPM to ensure that particles can be effectively separated.

[0026] The liquid filtered by the rotary filter is pumped into a buffer tank and allowed to stand in the buffer tank. The liquid after standing enters an ultrafine filter. The interior of the ultrafine filter is a three-layer structure. The three-layer structure is designed to provide a gradually fine filtering effect, and each layer captures particles and pollutants of different sizes.

[0027] The ultrafine filter consists of the first ultrafine filter layer, the second ultrafine filter layer, the third ultrafine filter layer and the filter element. The following is a specific design description of each layer: The first layer of the ultrafine filter, the pre-filter layer, is made of coarser fiber material, and its main purpose is to capture larger particles and a portion of smaller particles, preventing larger particles from entering the subsequent finer filter layers, so as not to quickly clog these layers or cause damage to them.

[0028] The function of the pre-filter layer is to extend the service life of the subsequent filter layer, reduce the maintenance frequency, and ensure the efficient operation of the entire filtration system. The pre-filter layer filter element selection range is 100 nm-50 nm.

[0029] The second layer of the ultrafine filter, i.e. the fine filter layer, uses finer fiber materials or deep-structured filter elements to capture smaller particles and microorganisms. The pore size of the filter element used in the fine filter layer ranges from 50 nm to 20 nm.

[0030] The third layer of the ultrafine filter, the ultrafine filtration layer, uses micro-nano filter media, such as ultrafiltration membrane or nanofiltration membrane, to remove almost all tiny particles, molecules and most microorganisms. This layer is designed to achieve the highest level of purification, ensuring that tiny particles and contaminants in the fluid are effectively removed.

[0031] The pore size of the ultra-fine filter layer can reach the nanometer level, which is crucial for the extremely demanding electronic chemical preparation process. The pore size selection range of the filter element used in the ultra-fine filter layer is 20 nm-2 nm.

[0032] Through this three-layer structure design, the ultra-fine filter can achieve gradual filtration from coarse to fine, ensuring that particulate matter in the fluid is effectively removed while maintaining efficient operation and a long service life of the system. The advantages of the present invention are: The device is suitable for filtering various liquids. The device of the present invention can provide efficient and accurate particle size removal through dynamic filtration, improve the purity and quality of electronic sulfuric acid, meet the production requirements of high-purity electronic chemicals, and has the advantages of flexible operation, simple maintenance and strong corrosion resistance. The device adopts a multi-stage filtration mechanism, which includes two stages: dynamic filtration and ultra-fine filtration. Each stage filters particles of different sizes. 1. Dynamic filtration: The dynamic filtration system uses the principle of fluid dynamics to further improve the particle separation efficiency through oscillation separation and centrifugal separation mechanisms. The device includes a graded vibration filter and a rotary filter, which can change the flow direction of the fluid or apply mechanical force to separate the particles from the fluid. The dynamic filtration system can be adjusted according to the characteristics of the particles (such as density, shape, size) to achieve the best filtration effect. 2. Ultra-fine filtration: The deep filtration unit uses a deep fiber filter element and uses a nano-scale filtration medium, such as an ultrafiltration membrane or a nanofiltration membrane, to remove almost all tiny particles, molecules and most microorganisms. The material selection of the fiber filter element takes into account acid resistance and mechanical strength, such as polypropylene, polytetrafluoroethylene, etc. The deep structure of the filter element allows the fluid to form multiple levels of filtration when passing through the filter material, increasing the chance of particle capture. When the fluid to be filtered enters the system, a detection point is set and a high-precision particle size analyzer is used to monitor the particles in the fluid in real time to ensure that the filtration effect meets the requirements. Filtration parameters such as flow rate, pressure and filter element replacement frequency can be adjusted according to actual needs. BRIEF DESCRIPTION OF THE DRAWINGS

[0033] Figure 1 It is the overall structural diagram of the device of the present invention; Figure 2 It is a schematic diagram of the structure of the present invention; Figure 3 It is a structural schematic diagram of the primary vibration filter of the present invention; Figure 4 It is a structural schematic diagram of the oscillation baffle of the present invention; Figure 5 It is a schematic diagram of the overall structure of the rotary filter of the present invention; Figure 6 This is a schematic diagram of the enlarged structure of the rotary filter of the present invention; Figure 7 It is a schematic diagram of the enlarged front cross-sectional structure of the ultrafine filter of the present invention; Figure 8 It is a schematic diagram of an enlarged top view of the cross section of the ultrafine filter of the present invention; In the figure: a first vibration filter housing 1, a first vibration baffle 2, a second vibration filter housing 3, a second vibration baffle 4, a rotary filter inlet pipe 5, a rotary filter drive motor 6, a rotary filter housing 7, a circulation pump 8, a buffer tank 9, an ultrafine filter inlet pipe 10, an ultrafine filter housing 11, a filtered solution inlet pipe 12, a particle size detector 13, a rotary filter screen 14, a rotary filter filtered solution inlet pipe 15 an inner layer of an ultrafine filter 16, an inner second layer of an ultrafine filter 17, an inner third layer of an ultrafine filter 18, a vibration baffle PFA frame 19, a vibration baffle PFA screen 20, and a vibration baffle drive motor 21. DETAILED DESCRIPTION The following will be combined with the specific embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. The embodiments described are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative work belong to the protection scope of the present invention. Example 1 A high-efficiency electronic sulfuric acid particle size filtering and separation device, the device comprises an oscillating filter, the bottom of the oscillating filter is connected to the rotary filter through a rotary filter inlet pipe 15, the rotary filter discharge port is connected to the buffer tank 9 feed port through a pipeline via a circulation pump 8, and the bottom discharge port of the buffer tank 9 is connected to the ultrafine filter through an ultrafine filter inlet pipe 10. Preferably, the vibration filter includes a first vibration baffle 2 and a second vibration baffle 4 in an upper and lower layer. The first vibration baffle 2 and the second vibration baffle 4 have the same structure, including a vibration baffle frame 19, and a vibration baffle filter 20 is provided on the vibration baffle frame 19. The first vibration baffle 2 is driven by a vibration baffle drive motor 21.

[0034] Further preferably, the upper portion of the first vibration baffle 2 is communicated with the first vibration filter housing 1 , and the upper portion of the second vibration baffle 4 is communicated with the second vibration filter housing 3 .

[0035] Preferably, the oscillating filter is provided with a filtration solution inlet pipe 12 , and a particle size detector 13 is provided on the filtration solution inlet pipe 12 .

[0036] Preferably, a rotary filter screen 14 is provided inside the rotary filter, and a rotary filter housing 7 is provided outside the rotary filter screen 14 .

[0037] Further preferably, the rotary filter filtration solution inlet pipe 15 passes through the rotary filter connector 5 and the rotary filter drive motor 6 and is connected to the interior of the rotary filter, and the rotary filter drive motor 6 drives the rotary filter screen 14 to rotate.

[0038] Further preferably, the ultrafine filter comprises an ultrafine filter first layer 16 , an ultrafine filter second layer 17 , an ultrafine filter third layer 18 and an ultrafine filter housing 11 from right inside to outside.

[0039] More preferably, the pore size of the first layer 16 of the ultrafine filter is between 100 nm and 50 nm, the pore size of the second layer 17 of the ultrafine filter is between 50 nm and 20 nm, and the pore size of the third layer 18 of the ultrafine filter is between 20 nm and 2 nm. The working steps are as follows: When the S1 liquid enters the oscillation filter, a small amount of liquid enters the set detection point and is connected to a high-precision particle size analyzer through an online sampling pipeline to measure the particle size distribution of particles in the fluid. According to the particle size and fluid pressure parameters of the particles, the oscillation frequency is dynamically optimized through the frequency regulator to achieve the best filtering effect.

[0040] After S2 is tested and analyzed by the particle size instrument, the electronic sulfuric acid is introduced into the vibration filter. According to the test data, the vibration frequency of the vibration filter is adjusted. When the particle size of the electronic grade sulfuric acid is 30nm and the particle size is ≥3000 pcs / ml, the vibration frequency adjustment rate of the first vibration baffle 2 is 40-60Hz, and the vibration frequency adjustment rate of the second vibration baffle 4 is 50-80Hz; when the particle size of the electronic grade sulfuric acid is 30nm and the particle size is ≤3000 pcs / ml, the vibration frequency adjustment rate of the first vibration baffle 2 is 30-40Hz, and the vibration frequency adjustment rate of the second vibration baffle 4 is 40-60Hz. The liquid filtered by the vibration filter enters the rotary filter.

[0041] The S3 vibration filter and the rotary filter are connected by a pipeline. A one-way valve is installed in the connecting pipeline, which only allows the liquid to flow from the vibration filter to the rotary filter in the device. When the particle size of electronic grade sulfuric acid 30nm is detected and the particle size is ≥3000 pcs / ml, the rotation frequency range of the rotary filter is 200-300 RPM. When the particle size of electronic grade sulfuric acid 30nm is detected and the particle size is ≤3000 pcs / ml, the rotation frequency range of the rotary filter is 100-200 RPM to ensure that the particles can be effectively separated.

[0042] S4 After the liquid is centrifugally filtered through the rotary filter, it is pumped into the buffer tank in front of the ultra-fine filter through a circulation pump for buffering and stabilization to alleviate the interference of bubbles generated during vibration and high-speed rotation.

[0043] S5 The liquid after buffering in the buffer tank enters the ultrafine filter, which is equipped with a 20-inch filter element commonly used in the market. The specific specifications are selected based on the data detected and analyzed by the particle size instrument. When the electronic grade sulfuric acid particle size is detected to be 30nm or less than 3000 pcs / ml, the first layer 16 of the ultrafine filter is 50 nmm, the second layer 17 of the ultrafine filter is 20 nmm, and the third layer 18 of the ultrafine filter is 10 nmm; when the electronic grade sulfuric acid particle size is detected to be 30nm or less than 3000 pcs / ml, the first layer 16 of the ultrafine filter is 100 nmm, the second layer 17 of the ultrafine filter is 50 nmm, and the third layer 18 of the ultrafine filter is 20 nmm; the selected filter element brand and specifications can be adjusted according to the specific conditions of the production line, and are not limited to the selection of the above specifications. After the liquid is filtered through the three-stage dynamic circulation from S1 to S5, the particle reduction ratio is high and the particle size meets the requirements of high-end processes. It meets the highest standard of electronic grade sulfuric acid classification in the industry and reaches the G5 level. The technical solution of the present invention is explained through the above embodiments, but the present invention is not limited to the above embodiments, that is, it does not mean that the present invention must rely on the above specific embodiments to be implemented. Any improvements made by technicians in the relevant field based on the present invention, or equivalent replacement of the materials selected by the present invention, etc., fall within the scope of protection of the patent.

Claims

1. A highly efficient electronic sulfuric acid particle size filtering and separation device, characterized in that: The device comprises an oscillating filter, the bottom of the oscillating filter is connected to the rotary filter via a rotary filter inlet pipe (15), the discharge port of the rotary filter is connected to the feed port of a buffer tank (9) via a pipe via a circulation pump (8), and the bottom discharge port of the buffer tank (9) is connected to the ultra-fine filter via an ultra-fine filter inlet pipe (10).

2. According to claim 1, a highly efficient electronic sulfuric acid particle size filtering and separation device is characterized in that: The vibration filter comprises a first vibration baffle (2) and a second vibration baffle (4) of upper and lower layers, the first vibration baffle (2) and the second vibration baffle (4) having the same structure, comprising a vibration baffle frame (19), a vibration baffle filter screen (20) being provided on the vibration baffle frame (19), and the first vibration baffle (2) being driven by a vibration baffle drive motor (21).

3. A highly efficient electronic sulfuric acid particle size filtering and separation device according to claim 2, characterized in that: The upper portion of the first vibration baffle (2) is in communication with the first vibration filter housing (1), and the upper portion of the second vibration baffle (4) is in communication with the second vibration filter housing (3).

4. According to claim 1, a highly efficient electronic sulfuric acid particle size filtering and separation device is characterized in that: The oscillating filter is provided with a filtration solution inlet pipe (12), and a particle size detector (13) is provided on the filtration solution inlet pipe (12).

5. According to claim 1, a highly efficient electronic sulfuric acid particle size filtering and separation device is characterized in that: A rotary filter screen (14) is provided inside the rotary filter, and a rotary filter housing (7) is provided outside the rotary filter screen (14).

6. A highly efficient electronic sulfuric acid particle size filtering and separation device according to claim 5, characterized in that: The rotary filter filtration solution inlet pipe (15) passes through the rotary filter connector (5) and the rotary filter drive motor (6) and is connected to the interior of the rotary filter. The rotary filter drive motor (6) drives the rotary filter filter screen (14) to rotate.

7. The high-efficiency electronic sulfuric acid particle size filtering and separation device according to claim 1 is characterized in that: The ultrafine filter comprises an ultrafine filter first layer (16) facing right inside and out, an ultrafine filter second layer (17), an ultrafine filter third layer (18) and an ultrafine filter housing (11).

8. A highly efficient electronic sulfuric acid particle size filtering and separation device according to claim 7, characterized in that: The pore size of the filter element of the first layer (16) of the ultrafine filter is between 100 nm and 50 nm, the pore size of the filter element of the second layer (17) of the ultrafine filter is between 50 nm and 20 nm, and the pore size of the filter element of the third layer (18) of the ultrafine filter is between 20 nm and 2 nm.

Citation Information

Cited By

  • High-precision filtering device for electronic-grade sulfuric acid

    CN120154985A