Intelligent manufacturing equipment and process for ultra-high purity quartz sand for semiconductors
By using intelligent manufacturing equipment and processes, combined with technologies such as magnetic separation, flotation, and microwave acid leaching, the problem of insufficient purity of quartz sand in traditional processes has been solved, achieving efficient and stable production of ultra-high purity quartz sand to meet the needs of high-end industries such as semiconductors.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- TUOYA SEMICONDUCTOR TECHNOLOGY (YUNNAN) CO LTD
- Filing Date
- 2026-02-26
- Publication Date
- 2026-06-05
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Abstract
Description
Technical Field
[0001] This invention relates to the field of non-metallic mineral purification materials technology, and in particular to an intelligent manufacturing equipment and process for ultra-high purity quartz sand for semiconductors. Background Technology
[0002] High-purity quartz ore contains three types of impurities: gangue minerals, inclusions, and lattice impurities. Their content, occurrence state, and distribution are the core factors determining the effectiveness of impurity removal. Gangue minerals (feldspar, mica, etc.) exist as independent minerals and can be removed by magnetic separation, flotation, and acid leaching without affecting the final purity. Inclusions are divided into microscopic (>1μm, including fluid, melt, and mineral inclusions, and are the main source of impurities such as alkali metals) and submicron-nanometer (<1μm, mostly mineral or melt inclusions, needle-like / elongated in shape, affecting purity). Lattice impurities are composed of P... 5+ 、Ge 4+ Ti 4+ Al 3+ Ga 3+ Fe 3+ B 3+ Plasma substitution of Si in Si-O tetrahedra 4+ Formation, equivalent substitution (such as Ti) 4+ 、Ge 4+ Replacement of Si 4+ ), ion group substitution (such as Al) 3+ With P 5+ Or Al 3+ with Na + Replacement of Si 4+ ) and charge compensation substitution (such as Al) 3+ Fe 3+ The formed [AlO4 / M + ] 0 or [FeO4 / M] + ] 0 (Structural center) Three methods; Ti-O and Al-O have high bond energies and are the most difficult to remove; Fe 3+ Cu 2+ Ca 2+ Mn 2+ The Me-O bonds of such bonds are easily removed.
[0003] Traditional processes struggle to remove inclusions and trace lattice impurities, failing to meet the 5N and higher purity requirements for semiconductors. Manual operation leads to low efficiency and inconsistent quality, while equipment hinders process innovation. High-purity quartz sand of 5N grade and above is used in semiconductor quartz crucibles and wafer auxiliary materials; its purity directly impacts chip performance. There is an urgent need for independent research and development of intelligent manufacturing processes and equipment to ensure supply chain security and improve self-sufficiency. Summary of the Invention
[0004] This invention provides an intelligent manufacturing process and equipment for ultra-high purity quartz sand used in semiconductors, which solves the following problems: traditional processes are difficult to remove inclusions and trace impurities in the crystal lattice, and cannot meet the purity requirements of 5N and above for semiconductors; manual operation leads to low efficiency and unstable quality, and equipment hinders process innovation; high purity quartz sand of 5N grade and above is used in semiconductor quartz crucibles, wafer auxiliary materials, etc., and its purity directly affects chip performance.
[0005] To achieve the above objectives, the present invention adopts the following technical solution: A smart manufacturing process equipment for ultra-high purity quartz sand for semiconductors includes a smart equipment rack 1 and a system smart control center 2; The intelligent control center 2 of the system includes a material preparation system 3, a high-purity quartz sand purification system 4, an ultra-high-purity quartz sand purification system 5, a quality control and product collection and processing system 6, a process auxiliary system 7, and a system monitoring center 8. The material preparation system 3 includes an intelligent ore bin 10, a raw ore mobile lifting tank washing machine 15, a raw ore crushing and grading integrated machine 21, a color sorter 29, a vacuum microwave roasting furnace 44, a gradient reaction vessel I 62, a ball mill 80, and a hydrocyclone classifier 90. The intelligent ore bin 10 is equipped with an inlet, an outlet, a raw ore inlet 11, and a conveyor belt I 12; The raw ore mobile lifting tank washing machine 15 includes a feed inlet I 13, an ultrapure water interface I 14, a rotating high-pressure rinsing water cover 16, a waste liquid treatment interface I 17, a discharge outlet I 18, and a conveyor belt II 19. The raw ore crushing and grading integrated machine 21 includes a discharge port II 22, a return hopper 23, a fine crushing and grading machine 24, a medium crushing and grading machine 25, a coarse crushing and grading machine 26, a feed port II 27, an exhaust port and a waste gas treatment interface I 28. The color sorter 29 includes a feed inlet Ⅲ31, a vibrating feeder 32, a signal processor 33, a chute 34, a light source 35, a sensor 36, compressed air 37, a spray valve 38, a discharge outlet Ⅲ39, and an impurity box 40. The vacuum microwave roasting furnace 44 includes an exhaust port and waste gas treatment interface II 41, a feed port IV 42, a vacuum interface I 45, a temperature controller I 46, a furnace shell I 47, a magnetron I 48, a stainless steel plate I 49, basalt fiber I 50, a silicon carbide tube I 51, a quartz tube I 52, a reaction chamber I 53, a reaction gas and flow meter interface I 54, an inert gas and flow meter interface I 55, and a discharge port IV 56. The gradient reactor I62 includes a feed inlet V57, a timer I59, a temperature controller II60, an auxiliary material inlet I61, a pressure gauge I63, an exhaust port and waste gas treatment interface III64, an ultrapure water interface II65, a furnace shell II66, a magnetron II67, a stainless steel plate II68, a lining I69, a waste liquid discharge channel I70, a gradient acid leaching tank I71, a cleaning device I72, a waste liquid treatment interface II73, and a discharge port V74. The ball mill 80 includes a feed inlet VI 75, a return outlet 76, an ultrapure water interface Ⅲ 78, a feeding device 79, a base 81, ball milling media 82, a ball milling chamber 83, gears and a vibration device 84, a waste liquid treatment interface Ⅲ 85, a discharge device 86, and a discharge outlet VI 87; the cyclone classifier 90 includes an underflow trough 88, an underflow outlet 89, a cyclone chamber 91, and a feed pipe Ⅰ 92; The high-purity quartz sand purification system 4 includes a magnetic separator 96, a slurry preparation tank I 119, a flotation machine I 127, a slurry preparation tank II 144, a flotation tank II 152, a multi-functional reactor I 166, a vacuum microwave purification furnace 184, a gradient reactor II 214, and a multi-functional reactor II 225. The magnetic separator 96 includes a water-cooled outlet 94, a water-cooled inlet 95, a material pipe II 97, a pulsation device 98, an excitation coil 99, an iron yoke 100, a feed inlet VII 101, a rotating ring 102, a magnetic medium 103, an ultrapure water interface IV 104, a rinsing water pipe 105, a magnetic material unloading hopper 106, a rinsing water 107, a magnetic material box 108, magnetic poles 109, a support base 110, a waste liquid treatment interface IV 111, a discharge outlet VII 112, and a non-magnetic material hopper 114. The mixing tank I119 includes a material pipe III115, a mixing tank inlet I116, a reagent and ultrapure water addition tank I117, a mixing tank outlet I118, and a stirring device I120. The flotation cell I127 includes a feed pipe IV121, a waste liquid treatment interface V122, a feed inlet VIII124, a timer II125, a temperature controller III126, a collection tank I128, an exhaust port and waste gas treatment interface IV129, a gas collection hood I130, a scraper device I131, a motor I132, a hollow shaft I133, an air pipe I134, a stator I135, an impeller I136, an ultrapure water interface V137, an ultrasonic device I138, and a discharge port VIII139. The mixing tank II144 includes a feed pipe V140, a mixing tank inlet II141, a reagent and ultrapure water addition tank II142, a mixing tank outlet II143, and a stirring device II145. The flotation cell II152 includes a feed pipe VI146, a waste liquid treatment interface VI147, a feed inlet IX149, a timer III150, a temperature controller IV151, a collection tank II153, an exhaust port and waste gas treatment interface V154, a gas collection hood II155, a scraper device II156, a motor II157, a hollow shaft II158, an air pipe II159, a stator II160, an impeller II161, an ultrapure water interface VI162, an ultrasonic device II163, and a discharge port IX164. The multifunctional reactor I166 includes a feed pipe VII165, an auxiliary material inlet II167, a temperature controller V168, a timer IV169, a feed port X170, a pressure gauge II172, an exhaust port and waste gas treatment interface VI173, an ultrapure water interface VII174, a furnace shell III175, a magnetron III176, a stainless steel plate III177, a lining II178, a waste liquid discharge channel II179, a cleaning device II180, a multifunctional rotary acid leaching tank I181, a waste liquid treatment interface VII182, and a discharge port X183; The vacuum microwave chlorination purification furnace 184 includes a feed inlet XI185, an exhaust port and waste gas treatment interface VII187, a vacuum interface II188, a fixed rotating device I189, a support base I190, a sealing device I191, a feed inner tube II192, a reaction chamber II193, a quartz reactor II194, a silicon carbide tube II195, a basalt fiber layer II196, a stainless steel plate IV197, a magnetron IV198, a heating box I199, a sealing device II200, a fixed rotating device II201, a temperature controller VI202, an inert gas and flow meter interface II203, a reaction gas and flow meter interface II204, and a discharge port XI205. The gradient reactor II 214 includes a feed inlet XII 206, a timer V208, a temperature controller VII 209, an auxiliary material inlet III 210, a pressure gauge II 211, an exhaust port and waste gas treatment interface VIII 212, an ultrapure water interface VIII 213, an outer shell V215, a magnetron V216, a stainless steel plate V217, a lining III 218, a waste liquid discharge channel III 219, a gradient acid leaching tank 220, an acid leaching tank partition II 221, a waste liquid treatment interface VIII 222, and a discharge port XII 223; The multifunctional reactor II225 includes a feed pipe VIII224, an auxiliary material inlet IV226, a temperature controller VIII227, a timer VI228, a feed inlet XIII229, a pressure gauge IV231, an exhaust port and waste gas treatment interface IX232, an ultrapure water interface IX233, a furnace shell VI234, a magnetron VI235, a stainless steel plate VI236, a lining IV237, a waste liquid discharge channel IV238, a cleaning device IV239, a multifunctional rotary acid leaching tank II240, a waste liquid treatment interface IX241, and a discharge port XIII242; The ultra-high purity quartz sand purification system 5 includes a vacuum microwave plasma purification furnace 243; The vacuum microwave plasma purification furnace 243 includes a feed inlet XIV and a return inlet 244, an exhaust port and waste gas treatment interface X246, a vacuum interface III247, a fixed rotating device III248, a support II249, a sealing device III250, a feed inner tube II251, a reaction chamber III252, a reactor III253, a silicon carbide tube IV254, a basalt fiber layer IV255, a stainless steel plate VII256, a magnetron VII257, a heating box II258, a sealing device IV259, a fixed rotating device IV260, a temperature controller IX261, an inert gas and flow meter interface III262, a reaction gas and flow meter interface III263, and a discharge port XIV264. The quality control and product collection and processing system 6 includes a cooling furnace 265, a vacuum packaging machine 282, a vacuum return bin 284, a conveyor belt Ⅳ 285, a quality control system 286, and a product warehouse 288. The cooling furnace 265 includes a feed inlet XV 266, a temperature controller X 268, an inert gas and flow meter interface IV 269, a fixed rotating device V 270, a support base III 271, a sealing device V 272, a feed inner tube III 273, a cooling chamber 274, a quartz cooler 275, a sealing device VI 276, a fixed rotating device VI 277, an exhaust port and waste gas treatment interface XI 278, a vacuum interface IV 279, and a discharge port XV 280. The vacuum packaging machine 282 includes a vacuum interface V281, a product vacuum packaging interface 283, and a product vacuum packaging barrel 287; The process auxiliary system 7 includes a power supply system 289, a vacuum system 290, a temperature control system 291, a gas control system 292, a water cooling system 293, a water production system 294, a reagent preparation system 295, a waste gas treatment system 296, a waste liquid treatment system 297, and a waste solid treatment system 298. The monitoring system center 8 includes monitoring system I 299, monitoring system II 300, monitoring system III 301, monitoring system IV 302, and monitoring system V 303; The intelligent equipment rack 1 has five layers. The first layer has two layers, one high and one low, on the right side. The intelligent control center 2 is located at the left end of the lower layer of the first layer. The material preparation system 3 is located on the left side of the first and second layers and the left side of the third to fifth layers. The high-purity quartz sand purification system 4 is located on the right side of the third to fifth layers. The ultra-high purity quartz sand purification system 5 is located on the right side of the second layer. The quality control and product collection and processing system 6 is located on the right side of the upper and lower layers of the first layer. The process auxiliary system 7 is located on the left side of the lower layer. The system monitoring center 8 is located at the left end of the upper layer of the first layer. The intelligent ore bin 10, the raw ore mobile lifting trough washing machine 15, and the raw ore crushing and grading integrated machine 21 are arranged sequentially from right to left on the left side of the first layer; the color sorter 29 is arranged on the left side of the fifth layer; the vacuum microwave roasting furnace 44 is arranged on the left side of the fourth layer; the gradient reaction vessel I 62 is arranged on the left side of the third layer; and the ball mill 80 and the cyclone classifier 90 are arranged sequentially from left to right on the left side of the second layer. The magnetic separator 96 is located on the left side of the third layer; the slurry preparation tank I 119 and slurry preparation tank II 144 are sequentially located on the left side of the fourth layer; the flotation machine I 127, flotation II 152 and multifunctional reactor I 166 are sequentially located on the right side of the fifth layer from left to right; the vacuum microwave purification furnace 184 is located on the right side of the fourth layer; the gradient reactor II 214 and multifunctional reactor II 225 are sequentially located on the right side of the third layer from left to right. The vacuum microwave plasma purification furnace 243 is located on the right side of the second layer; The cooling furnace 265 is located on the first high floor, and from right to left on the right side of the low floor, the conveyor belt Ⅳ285, the vacuum return barrel 284, the quality control 286, the vacuum packaging machine 282 and the product warehouse 288 are arranged sequentially. The power supply system 289, vacuum system 290, temperature control system 291, gas control system 292, water cooling system 293, water production system 294, reagent preparation system 295, waste gas treatment system 296, waste liquid treatment system 297, and waste solid treatment system 298 are arranged from right to left on the left side of the first lower layer.
[0006] Preferably, the monitoring system I 299 is located in the material preparation system 3 area (right next to the top left of the center line of the second layer), the monitoring system II 300 is located in the high-purity quartz sand purification system 4 area (right next to the bottom right of the center line of the third layer), the monitoring system III 301 is located in the ultra-high purity quartz sand purification system 5 area (right next to the top right of the center line of the second layer), the monitoring system IV 302 is located in the quality control and product collection and processing system 6 area (right next to the top left of the upper layer of the first layer), and the monitoring system V 303 is located in the process auxiliary system area (right next to the top left of the lower layer of the first layer).
[0007] Preferably, the device further includes controller I9, controller II20, controller III30, controller IV43, controller V58, controller VI77, controller VII113, controller VIII123, controller IX148, controller X171, controller XI186, controller XII207, controller XIII230, controller XIV245, and controller XV267; The controller I9 is connected to the intelligent ore bin 10 and the raw ore mobile lifting trough washing machine 14; The controller II20 is connected to the raw ore crushing and grading integrated machine 21; The controller Ⅲ30 is connected to the color sorter 29; The controller Ⅳ43 is connected to the vacuum microwave roasting furnace 44; The controller V58 is connected to the gradient reactor I62; The controller VI77 is connected to the ball mill 80 and the hydrocyclone classifier 90; The controller VII113 is connected to the magnetic separator 96; The controller VIII 123 is connected to the slurry conditioning tank I 119 and the flotation tank I 127; The controller IX148 is connected to the slurry conditioning tank II144 and the flotation tank II152; The controller X171 is connected to the multi-functional reactor I166; The controller XI186 is connected to the vacuum microwave purification furnace 184; The controller XII207 is connected to the gradient reactor II214; The controller XⅢ230 is connected to the multi-functional reactor Ⅱ225; The controller XI N245 is connected to the vacuum microwave plasma purification furnace 243; The controllers X and V 267 are respectively connected to the cooling furnace 265, the vacuum packaging machine 282, the vacuum return barrel 284, the conveyor belt IV 285, the quality control 286, and the product warehouse 288; The controllers I9, II20, III30, IV43, V58, VI77, VII113, VIII123, IX148, X171, XI186, XII207, XIII230, XIV245, and XV267 are connected to different composite quartz sensors according to the control process parameters.
[0008] Preferably, the linings of the raw ore mobile lifting tank washing machine 15 and the raw ore crushing and grading integrated machine 21 are both made of pollution-free materials; the gradient reactor I 62 and gradient reactor II 214 are equipped with gradient acid leaching tanks; the multi-functional reactor I 166 and multi-functional reactor II 225 are equipped with multi-functional rotary acid leaching tank I 181 and multi-functional rotary acid leaching tank II 240, and the linings of the gradient reactor I 62, multi-functional reactor I 166, gradient reactor II 214 and multi-functional reactor II 225 are all made of pollution-free, acid-resistant, high-temperature resistant and pressure-resistant high-quality materials.
[0009] Preferably, both flotation cell I 127 and flotation cell II 152 are equipped with gas collection hoods I 130 and II 155 to collect waste gas, and an ultrasonic device is provided at the radial joint of the flotation cell I 127 and flotation cell II 152.
[0010] Preferably, the inner wall of the reaction chamber I53 of the vacuum microwave roasting furnace 44 is provided with quartz spiral reinforcing ribs; the reactors II194 and III253 of the vacuum microwave purification furnace 184 and the vacuum microwave plasma purification furnace 243 all use high-purity, high-quality quartz tubes with internal straight reinforcing ribs; the microwave generators used in the vacuum microwave roasting furnace 44, the vacuum microwave purification furnace 184, and the vacuum microwave plasma purification furnace 243 are preferably 2.45 GHz microwave power sources, and the silicon carbide tubes used are hollow tubes.
[0011] Preferably, the intelligent control center 2 of the system is connected to the material preparation system 3, the high-purity quartz sand purification system 4, the ultra-high-purity quartz sand purification system 5, the quality control and product collection and processing system 6, the process auxiliary system 7, and the system monitoring center 8, respectively; the system monitoring center 8 is connected to monitoring system I 299, monitoring system II 300, monitoring system III 301, monitoring system IV 302, and monitoring system V 303, respectively; monitoring system I 299 is connected to the material preparation system 3; monitoring system II 300 is connected to the high-purity quartz sand purification system 4; monitoring system III 301 is connected to the ultra-high-purity quartz sand purification system 5; monitoring system IV 302 is connected to the quality control and product collection and processing system 6; and monitoring system V 303 is connected to the process auxiliary system. The system 7 is connected; the power supply system 289 is connected to the system intelligent control center 2, the material preparation system 3, the high-purity quartz sand purification system 4, the ultra-high-purity quartz sand purification system 5, the quality control and product collection and processing system 6, the process auxiliary system 7, and the system monitoring center 8 respectively; the vacuum system 290 is connected to vacuum interface I 45, vacuum interface II 188, vacuum interface III 247, vacuum interface IV 279, and vacuum interface V281 respectively; the temperature control system 291 is connected to temperature controller I 46, temperature controller II 60, temperature controller III 126, temperature controller IV 151, temperature controller V168, temperature controller VI 202, temperature controller VII 209, temperature controller VIII 227, temperature controller IX 261, and temperature controller X 268 respectively; the gas control system System 292 is connected to the following interfaces respectively: reaction gas and flow meter interface I54, inert gas and flow meter interface I55, inert gas and flow meter interface II203, reaction gas and flow meter interface II204, inert gas and flow meter interface III262, reaction gas and flow meter interface III263, and inert gas and flow meter interface IV269; the water cooling system 293 is connected to the water cooling outlet interface 94 and the water cooling inlet interface 95; the water purification system 294 is connected to the following interfaces respectively: ultrapure water interface I14, ultrapure water interface II65, ultrapure water interface III78, ultrapure water interface IV104, ultrapure water interface V137, ultrapure water interface VI162, ultrapure water interface VII174, ultrapure water interface VIII213, and ultrapure water interface IX233; All process water is connected to the water treatment system 294; the reagent preparation system 295 and the water treatment system 294 are respectively connected to the reagent and ultrapure water addition tank I117 and the reagent and ultrapure water addition tank II142; the waste gas treatment system 296 is respectively connected to the exhaust port and waste gas treatment interface I28, exhaust port and waste gas treatment interface II41, exhaust port and waste gas treatment interface III64, exhaust port and waste gas treatment interface IV129, exhaust port and waste gas treatment interface V154, exhaust port and waste gas treatment interface VI173, exhaust port and waste gas treatment interface VII187, exhaust port and waste gas treatment interface VIII212, exhaust port and waste gas treatment interface IX232, exhaust port and waste gas treatment interface X246, and exhaust port and waste gas treatment interface XI278;The waste liquid treatment system 297 is connected to waste liquid treatment interfaces I16, II73, III85, IV111, V122, VI147, VII182, VIII222, IX241, and IX241 respectively; the treated water from the waste liquid treatment system 297 can be connected to the water treatment system 294; the solid waste treatment system 298 is connected to the impurity tank 40 and the magnetic material tank 108 respectively.
[0012] The present invention also provides an intelligent manufacturing process for ultra-high purity quartz sand for semiconductors. Using the above-mentioned intelligent manufacturing device for ultra-high purity quartz sand for semiconductors, the process includes the following four stages and a total of seven steps: the first stage is material preparation, including step one; the second stage is high-purity quartz purification, including steps two to five; the third stage is ultra-high purity quartz purification, including step six; and the fourth stage is quality control and product collection and processing, including step seven. Step 1: Raw Material Preparation: This includes raw ore beneficiation, raw ore storage, raw ore washing, crushing and grading, color sorting, chlorination and calcination, acid leaching, and ball milling and grading. First, high-purity quartz raw ore is selected according to requirements and stored in the intelligent ore bin of this invention. It is then washed clean using the raw ore mobile lifting trough washing machine of this invention. The integrated crushing and grading machine of this invention performs coarse, medium, and fine crushing and grading to obtain raw materials with a particle size of 1-3 mm. A color sorter is preferred to remove discolored particles and impurities. The ore is then chlorinated and calcined first using a vacuum microwave calcination furnace in conjunction with the microwave gradient reactor of this invention, followed by direct microwave acid leaching. The raw ore is initially purified by immersion and microwave cleaning. A wet ball mill and hydrocyclone classifier are then used for ball milling and classification to obtain qualified raw materials with a particle size of 0.1–0.3 mm, a purity of 4N or higher, and controllable impurities. The raw material preparation process parameters are as follows: The selected high-purity quartz ore quality is: SiO2 mass fraction higher than 3N, total impurities <100 μg / g; the selected quality meets the following reference standards: total impurity element (μg / g) <50, of which Al <30, Ti <10, Na <8, K <8, Li <5, Ca <5, Fe <3, P <2 and... B < 1, trace amounts of radioactive elements and gas-liquid inclusions; Reserve process parameters: Raw ore reserve: ore quantity for 72 hours of continuous production; Soaking process parameters: raw ore soaking agent 8%~12%H2C2O4++1%~10%HF, soaking time 4~24 hours, rinsing water pressure 1~10MPa; Crushing and grading process parameters: coarse crushing particle size 10~30mm, medium crushing particle size 5~10mm, fine crushing particle size 1~5mm; Color sorting process parameters: color sorting particle size range 0.08~5mm, color threshold: a narrow range close to white. Encirclement, spray intensity: gas valve pressure 0.4~0.6MPa; chlorination calcination process parameters: vacuum degree 0.1~0.01Pa, temperature 600~1200℃, time 1~4h, mixed gas flow rate 10~100sccm, Ar flow rate above 5N 10~100sccm, HCl gas flow rate above 5N 10~100sccm; microwave acid leaching process parameters: gradient acid leaching is achieved by sequentially using acid leaching agents 1~3: acid leaching agent 1: H2C2O 48~12%, acid leaching agent 2: acid ratio HF 3~10%+ H2C2O4 10~12%, acid leaching agent 3: acid ratio HF 3~10% + H2C2O4 8~12% + H2SiF6, liquid-solid ratio 2:1~4:1, acid leaching pressure 0.5~1MPa, acid leaching temperature 60~120℃, acid leaching time 30~240min, ultrapure water microwave cleaning, ultrapure water quality: resistivity ≥18.2MΩ·cm, ball milling classification process parameters: ball milling feed particle size 1~5mm, ball milling time 1~6h, cyclone classification discharge particle size 0.1~0.3mm; Step 2: Gradient Magnetic Separation: A vertical ring pulsating high-gradient wet magnetic separator is preferred to remove magnetic impurities. High-gradient magnetic separation process parameters: 1.5–2.0T background magnetic field, slurry concentration 25%–30%, pulsation frequency 200–300 times / min, feed particle size controlled at -0.074mm (≥80%), and washing water volume controlled at 1–2 m³ / min. 3 / t of ore, ensuring timely discharge of magnetic products and avoiding secondary adsorption; Step 3: Ultrasonic Flotation: The prepared slurry is subjected to two ultrasonic flotations and ultrasonic cleaning using the ultrasonic temperature-controlled flotation machine of this invention to remove gangue mineral impurities; Slurry preparation and ultrasonic flotation process parameters: First slurry preparation and ultrasonic flotation process parameters: A combined reagent system (oleic acid + dodecylamine + pH 2.5-3.5) and a microbubble flotation column (bubble diameter ≤50μm) are used to remove silicate mineral impurities such as feldspar and mica; impeller speed 100-300rpm; aeration rate 0.2-0.5m³. 3 / (m²·min), pulp concentration 20%-40%, ultrasonic frequency 20-40kHz, flotation temperature 30-50℃, flotation time 20-60min, ultrasonic cleaning with ultrapure water, ultrapure water quality: resistivity ≥18.2MΩ·cm; secondary pulp conditioning and ultrasonic flotation process parameters: for different mineral impurities, optimize the primary flotation reagent system, intelligently adjust the reagent dosage, adjust the pH value, ultrasonic flotation, and ultrasonic cleaning with ultrapure water to effectively remove various gangue mineral impurities; Step 4: Microwave acid leaching: Microwave acid leaching, microwave cleaning, and microwave drying are performed using the microwave multifunctional reactor of this invention to remove inclusions and impurities; Microwave acid leaching process parameters: Acid ratio of leaching agent: HCl 20~30% + H2SO4 10~20% + HF 3~5%, liquid-solid ratio 2:1~4:1, acid leaching pressure 0.5~1MPa, acid leaching temperature 60~120℃, acid leaching time 30~240min, microwave cleaning with ultrapure water, ultrapure water quality: resistivity ≥18.2MΩ·cm, microwave drying temperature 100~120℃; Step 5: Vacuum chlorination combined with hot-press acid leaching for fine purification: Using the vacuum microwave purification furnace of this invention in conjunction with a microwave reactor, lattice impurities are first removed by vacuum microwave treatment, followed by direct microwave acid leaching to remove burst micro-nano-scale inclusions, microwave cleaning, and microwave drying to obtain high-purity quartz sand with a purity of 5N or higher; Chlorination process parameters: Vacuum degree 0.1~0.01Pa, temperature 600~1200℃, time 30~240min, mixed gas flow rate 10~100sccm, Ar gas flow rate (5N or higher) 10~100sccm, HCl gas flow rate (5N or higher) 10~100sccm, environment: Class 100 cleanliness; Microwave acid leaching process parameters: First acid leaching: Acid leaching agent 1~3 times sequentially. The process involves gradient acid leaching: Acid leaching agent 1: 8-12% H2C2O4; Acid leaching agent 2: Acid ratio of 3-10% HF + 10-12% H2C2O4; Acid leaching agent 3: Acid ratio of 3-10% HF + 8-12% H2C2O4 + H2SiF6; Secondary acid leaching: Acid ratio of 20-30% HCl + 10-20% H2SO4 + 3-5% HF; Liquid-solid ratio 2:1-4:1; Acid leaching pressure 0.5-1MPa; Acid leaching temperature 60-120℃; Acid leaching time 30-240min; Microwave cleaning with ultrapure water; Ultrapure water quality: resistivity ≥18.2MΩ·cm; Microwave drying temperature 100-120℃; Total impurities less than 8ppm. Step Six: Plasma Fine Purification: Further fine purification using the vacuum microwave plasma purification furnace of this invention, i.e., in a high-vacuum device filled with hydrogen-mixed plasma, to completely remove residual micro-nano-scale inclusions and lattice impurities, obtaining ultra-high purity quartz sand with a purity of 6N or higher; Plasma purification process parameters: Vacuum degree 10 -2 ~10 -4 Pa gas, temperature 600~1500℃, time 10~180min, mixed gas flow rate 10~150sccm, Ar flow rate above 6N 10~125sccm, H2 flow rate above 6N 10~120sccm; environment: Class 100 cleanliness, plasma excitation frequency 2.45GHz. Step Seven: Quality Control and Product Collection and Processing: Finally, after vacuum cooling and quality inspection, qualified products are vacuum-packed, sealed, and stored for sale. This product meets the stringent requirements of ultra-high purity quartz sand in high-end fields such as semiconductors. Quality control and product collection and processing parameters: Vacuum degree 0.1 Pa, cooling medium: argon gas above 6N, argon gas flow rate 5–100 cm³ / h. 3 / min, cooling rate 20~50℃ / min: cooling to room temperature 0~25℃, cooling environment: Class 100 cleanliness, relative humidity not exceeding 40%, product quality control: purity above 6N, impurity content below 0.1ppm, particle size and particle size distribution are formulated according to product application requirements.
[0013] Preferably, in step one, the quality of the selected high-purity quartz ore is as follows: SiO2 mass fraction is higher than 3N, and total impurities (μg / g) < 100; the preferred quality meets the reference standard: total impurity elements (μg / g) < 50, of which Al < 30, Ti < 10, Na < 8, K < 8, Li < 5, Ca < 5, Fe < 3, P < 2 and B < 1, and trace amounts of radioactive elements and gas-liquid inclusions; in step one, the ore is calcined in a vacuum microwave calcination furnace in conjunction with a microwave reactor, followed by direct microwave acid leaching and microwave cleaning to complete the preliminary purification, thereby improving the quality of the ore and ensuring the quality requirements of subsequent purification processes; this invention is suitable for the fine purification of pegmatite and vein quartz, solving the problem of scarcity of high-purity quartz ore.
[0014] Preferably, steps one, four, and five utilize the microwave reactor of the present invention for microwave acid leaching, microwave cleaning, and microwave drying to remove various inclusions in different forms, effectively avoiding air pollution and improving product quality. Step two preferably uses a vertical ring pulsating high-gradient wet magnetic separator to remove particulate weakly magnetic impurities. Step three uses the ultrasonic temperature-controlled flotation machine of the present invention to optimize the primary flotation reagent system for different mineral impurities, intelligently adjusting reagent dosage and pH value, performing ultrasonic flotation and ultrasonic cleaning to effectively remove various gangue mineral impurities. Step five uses the vacuum microwave purification furnace of the present invention in conjunction with the microwave reactor to remove lattice impurities through vacuum microwaveation, while simultaneously using microwave acid leaching to further target... Various inclusions of different occurrence forms and distributions are precisely removed, and the burst micro-nano-sized inclusions are then washed with ultrapure water and microwave dried to obtain high-purity quartz sand with a purity of 5N or higher. In step six, the vacuum microwave plasma purification furnace of this invention is used in a high-vacuum device filled with hydrogen mixed gas plasma to thoroughly remove residual micro-nano-sized inclusions and lattice impurities to obtain ultra-high-purity quartz sand with a purity of 6N or higher. In step seven, the sand is finally cooled to room temperature under vacuum, and quality is tested. Qualified products are vacuum-packed, sealed, and stored for sale. Defective products can be returned to any step of the process for further processing based on their quality issues. This invention can meet the stringent quality requirements of products in terms of purity, particle size and particle size distribution, as well as the limitation of special elements.
[0015] Preferably, steps one to four are completed in a Class 1000 cleanroom environment, and steps six and seven are completed in a Class 100 cleanroom environment; all water used in steps one to six is ultrapure water with a resistivity ≥18.2 MΩ·cm; the exhaust gas generated in steps one to seven is treated to meet standards before being discharged, the wastewater generated is treated to meet standards before being discharged or returned to the water treatment system, and all waste generated is treated in a microwave plasma incinerator to meet standards before being discharged.
[0016] This invention has at least the following beneficial effects: 1. This invention possesses a series of advanced and unique purification technologies and processes for ultra-high purity quartz sand used in semiconductors, capable of raising the purity of quartz sand to levels exceeding 5N. These include high-gradient multi-step purification technologies (calcination, color sorting, magnetic separation, flotation, acid leaching, chlorination, and hydrogenation), plasma purification technologies for removing nanoscale impurities, vacuum chlorination-calcination direct acid leaching purification technologies, and vacuum microwave chlorination direct acid leaching purification technologies. These technologies effectively remove gangue mineral impurities, inclusions, and lattice impurities from quartz, resulting in product performance and quality far exceeding those of competitors. Furthermore, the products are stable, cost-effective, and generate significant value with a promising future. This invention features advanced processes and intelligent equipment, characterized by large industrial output, specialized preparation, high automation, environmental friendliness, and high efficiency. It enables large-scale, continuous, efficient, and clean production. Combined with high-quality quartz ore resources in China, it can produce high-purity and ultra-high-purity quartz sand products of varying purities and specifications to meet the needs of different customers.
[0017] 2. This invention establishes a rigorous quality control system throughout the production process via an intelligent control center. This system requires strict testing and monitoring at every stage, from selecting high-purity quartz ore and processing to finished product warehousing and quality control. Advanced testing equipment and technology are used to precisely test multiple indicators such as purity, particle size, chemical composition, and morphology of the products, ensuring that each batch meets high-quality standards and gains high customer approval.
[0018] 3. The ultra-high purity silica sand produced by this invention has wide applicability and can meet the needs of multiple high-end industries. In the semiconductor field, its products can be used to manufacture key components such as integrated circuits and chips. Due to its high purity and excellent physicochemical properties, it can ensure the high performance and reliability of semiconductor devices. In the photovoltaic field, high-purity silica sand is a key material for manufacturing solar cell crucibles, ensuring the quality and service life of the crucibles, thereby improving the production efficiency and quality of solar cells. In the optical communication field, its products can be used to manufacture optical fiber preforms, providing important support for the development of the optical communication industry.
[0019] 4. Based on fine purification and intelligent equipment, this invention utilizes monitoring technology, industrial internet, and automated control technology to construct an intelligent production control system. Through a real-time monitoring system set up in the system's intelligent manufacturing control center, key parameters such as the purity, particle size distribution, and impurity content of quartz sand are monitored online in real time. A database and model can be established to achieve dynamic monitoring and quality early warning of the production process. It can automatically collect and analyze various data during the production process and automatically adjust the operating status of production equipment according to preset process parameters and quality targets, achieving automated and intelligent control of the production process and ensuring the stability and consistency of product quality.
[0020] 5. This invention enables automated transportation and quality control of high-purity quartz ore, semi-finished products, finished products, and defective products. Through automated conveying equipment and quality control management software, production efficiency is improved, pollution and errors caused by manual operation are reduced, and the smooth operation of the production process is ensured.
[0021] 6. This invention can optimize traditional enterprise production processes and equipment, produce customized products to meet unique customer needs, and develop new products. The process and equipment of this invention can eliminate the manual sorting of high-purity quartz ore in traditional purification processes, saving labor and solving the pollution problem caused by manual operation.
[0022] 7. This invention promotes the high-quality development of the semiconductor industry, meets the needs of industrial upgrading, and ensures supply chain security. Ultra-high purity silica sand is a key material for manufacturing core components of semiconductor chips. Purification technology can effectively reduce its impurity content, significantly improving the electrical, optical, and stability properties of semiconductor products, thereby driving the development of the semiconductor industry. Advanced purification technology can produce ultra-high purity silica sand that meets the needs of industrial upgrading, providing strong material support for the sustainable development of the semiconductor industry and propelling the industry towards high-end development. The semiconductor industry has a huge demand for ultra-high purity silica sand, but global high-purity quartz mineral resources are unevenly distributed and the supply is unstable. The invention of ultra-high purity silica sand purification technology not only promotes the development of the semiconductor industry but also drives the coordinated development of upstream and downstream related industries. Upstream, it will stimulate the development of industries such as quartz mining and beneficiation; downstream, it will benefit the prosperity of industries such as electronics, communications, and new energy. This industrial linkage effect can create more job opportunities and promote economic growth; companies that master advanced purification technology have stronger competitiveness in the market. These companies are capable of producing high-quality, ultra-high-purity quartz sand products to meet customers' high-end needs, thereby gaining a competitive advantage in the market and improving their economic benefits and market share. At the same time, the growth and expansion of these companies also contribute to enhancing the country's international competitiveness in the semiconductor materials field. Attached Figure Description
[0023] To more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the following description of the embodiments will be briefly introduced. Obviously, the drawings described below are some embodiments of the present invention. For those skilled in the art, other drawings can be obtained based on these drawings without creative effort.
[0024] Figure 1 This is a schematic diagram of the structure of the device in Embodiment 1 of the present invention; Figure 2 This is a schematic diagram of the intelligent control center structure of the device in Embodiment 1 of the present invention. Figure 3This is a schematic diagram of the material preparation system of the equipment in Embodiment 1 of the present invention; Figure 4 This is a schematic diagram of the high-purity quartz sand purification system of the device in Embodiment 1 of the present invention; Figure 5 This is a schematic diagram of the ultra-high purity quartz sand purification system of the device in Embodiment 1 of the present invention; Figure 6 This is a schematic diagram of the quality control and product collection and processing system of the device in Embodiment 1 of the present invention; Figure 7 This is a schematic diagram of the process auxiliary system structure of the equipment in Embodiment 1 of the present invention; Figure 8 This is a schematic diagram of the system monitoring center structure of the device in Embodiment 1 of the present invention; Figure 9 This is a process flow diagram of Embodiment 2 of the present invention; In the diagram: 1 - Intelligent equipment rack, 2 - System intelligent control center, 3 - Material preparation system, 4 - High-purity quartz sand purification system, 5 - Ultra-high purity quartz sand purification system, 6 - Quality control and product collection and processing system, 7 - Process auxiliary system, 8 - System monitoring center, 9 - Controller I, 10 - Intelligent ore bin, 11 - Raw ore inlet, 12 - Conveyor belt I, 13 - Feed inlet I, 14 - Ultrapure water interface I, 15 - Raw ore mobile lifting tank washing machine, 16 - Rotary high-pressure flushing water cover, 17 - Waste liquid treatment interface I, 18 - Discharge outlet I, 19 - Conveyor belt II, 20 - Controller II, 21 - Raw ore crushing and grading integrated machine, 22 - Discharge outlet II, 23 - Return hopper, 24 - Fine crushing and grading machine, 25 - Medium crushing and grading machine, 26 - Coarse crushing and grading machine, 27 - Feed inlet II, 28 - Exhaust port and waste gas. Processing Interface I, 29 - Color Sorter, 30 - Controller III, 31 - Feed Inlet III, 32 - Vibrating Feeder, 33 - Signal Processor, 34 - Slide Chest, 35 - Light Source, 36 - Sensor, 37 - Compressed Air, 38 - Spray Valve, 39 - Discharge Port III, 40 - Impurity Box, 41 - Exhaust Port and Waste Gas Treatment Interface II, 42 - Feed Inlet IV, 43 - Controller IV, 44 - Vacuum Microwave Roasting Oven, 45 - Vacuum Interface I, 46 - Temperature Controller I, 47 - Oven Shell I, 48 - Magnetron I, 49 - Stainless Steel Plate I, 50 - Basalt Fiber I, 51 - Silicon Carbide Tube I, 52 - Quartz Tube I, 53 - Reaction Chamber I, 54 - Reaction Gas and Flow Meter Interface I, 55 - Inert Gas and Flow Meter Interface I, 56 - Discharge port IV, 57 - Feed port V, 58 - Controller V, 59 - Timer I, 60 - Temperature controller II, 61 - Auxiliary material inlet I, 62 - Gradient reactor I, 63 - Pressure gauge I, 64 - Exhaust port and waste gas treatment interface III, 65 - Ultrapure water interface II, 66 - Furnace shell II, 67 - Magnetron II, 68 - Stainless steel plate II, 69 - Lining I, 70 - Waste liquid discharge channel I, 71 - Gradient acid leaching tank I, 72 - Cleaning device I, 73 - Waste liquid treatment interface II, 74 - Discharge port V, 75 - Feed port VI, 76 - Return port, 77 - Controller VI, 78 - Ultrapure water interface III, 79 - Feeding device, 80 - Ball mill, 81 - Base, 82 - Ball milling media, 83 - Ball Grinding chamber, 84 - Gear and vibration device, 85 - Waste liquid treatment interface III, 86 - Discharge device, 87 - Discharge port VI, 88 - Underflow trough, 89 - Underflow port, 90 - Cyclone classifier, 91 - Cyclone chamber, 92 - Material pipe I, 93 - Overflow port, 94 - Water-cooled water outlet interface, 95 - Water-cooled water inlet interface, 96 - Magnetic separator, 97 - Material pipe II, 98 - Pulsation device, 99 - Excitation coil, 100 - Yoke, 101 - Inlet VII, 102 - Rotary ring, 103 - Magnetic medium, 104 - Ultrapure water interface IV, 105 - Rinse water pipe, 106 - Magnetic material unloading hopper, 107 - Rinse water, 108 - Magnetic material box, 109 - Magnetic pole, 110 - Support base, 111 - Waste liquid treatment interface IV112 - Discharge port VII, 113 - Controller VII, 114 - Non-magnetic material hopper, 115 - Material pipe III, 116 - Slurry mixing tank inlet I, 117 - Reagent and ultrapure water addition tank I, 118 - Slurry mixing tank outlet I, 119 - Slurry mixing tank I, 120 - Stirring device I, 121 - Material pipe IV, 122 - Waste liquid treatment interface V, 123 - Controller VIII, 124 - Feed inlet VIII, 125 - Timer II, 126 - Temperature controller III, 127 - Flotation cell I, 128 - Collection tank I, 129 - Exhaust port and waste gas treatment interface IV, 130 - Gas collection hood I, 131 - Scraper device I, 132 - Motor I, 133 - Hollow shaft I, 134 - Air pipe I, 135 - Stator I, 136 - Impeller I, 137 - Ultrapure water addition tank Pure water interface V, 138 - Ultrasonic device I, 139 - Discharge port VIII, 140 - Material pipe V, 141 - Slurry tank inlet II, 142 - Reagent and ultrapure water addition tank II, 143 - Slurry tank outlet II, 144 - Slurry tank II, 145 - Stirring device II, 146 - Material pipe VI, 147 - Waste liquid treatment interface VI, 148 - Controller IX, 149 - Feed inlet IX, 150 - Timer III, 151 - Temperature controller IV, 152 - Flotation cell II, 153 - Collection tank II, 154 - Exhaust port and waste gas treatment interface V, 155 - Gas collection hood II, 156 - Scraper device II, 157 - Motor II, 158 - Hollow shaft II, 159 - Air pipe II, 160 - Stator II, 161 - Impeller II, 162 - Ultrapure water interface VI - 163 - Ultrasonic Device II; 164 - Discharge Port IX; 165 - Material Pipe VII; 166 - Multifunctional Reactor I; 167 - Auxiliary Material Inlet II; 168 - Temperature Controller V; 169 - Timer IV; 170 - Feed Inlet X; 171 - Controller X; 172 - Pressure Gauge II; 173 - Exhaust Port and Waste Gas Treatment Interface VI; 174 - Ultrapure Water Interface VII; 175 - Furnace Shell III; 176 - Magnetron III; 177 - Stainless Steel Plate III; 178 - Lining II; 179 - Waste Liquid Discharge Channel II; 180 - Cleaning Device II; 181 - Multifunctional Rotary Acid Immersion Tank I; 182 - Waste Liquid Treatment Interface VII; 183 - Discharge Port X; 184 - Vacuum Microwave Chlorination Purification Furnace; 185 - Feed Inlet XI; 186 - Controller X 187 - Exhaust port and waste gas treatment interface VII; 188 - Vacuum interface II; 189 - Fixed rotating device I; 190 - Support base I; 191 - Sealing device I; 192 - Inner feed tube I; 193 - Reaction chamber II; 194 - Quartz reactor II; 195 - Silicon carbide tube II; 196 - Basalt fiber layer II; 197 - Stainless steel plate IV; 198 - Magnetron IV; 199 - Heating box I; 200 - Sealing device II; 202 - Fixed rotating device II; 202 - Temperature controller VI; 203 - Inert gas and flow meter interface II; 204 - Reaction gas and flow meter interface II; 205 - Discharge port XI; 206 - Inlet XII; 207 - Controller XII; 208 - Timer V; 209 - Temperature controller VII.210 – Auxiliary material inlet III, 211 – Pressure gauge II, 212 – Exhaust port and waste gas treatment interface VIII, 213 – Ultrapure water interface VIII, 214 – Gradient reactor II, 215 – Outer shell V, 216 – Magnetron V, 217 – Stainless steel plate V, 218 – Lining III, 219 – Waste liquid discharge channel III, 220 – Gradient acid leaching tank II, 221 – Cleaning device III, 222 – Waste liquid treatment interface VIII, 223 – Discharge port XII, 224 – Material pipe VIII, 225 – Multifunctional reactor II, 226 – Auxiliary material inlet IV, 227 – Temperature controller VIII, 228 – Timer VI, 229 – Inlet XIII, 230 – Controller XIII, 231 – Pressure gauge IV, 232 – Exhaust port and waste gas treatment interface IX, 233 – Ultrapure water interface IX - Furnace Shell VI - Magnetron VI - Stainless Steel Plate VI - Lining IV - Waste Liquid Discharge Channel IV - Cleaning Device IV - Multifunctional Rotary Acid Immersion Tank II - Waste Liquid Treatment Interface IX - Discharge Port XIII - Vacuum Microwave Plasma Purification Furnace - Feed Inlet XIV (Return Port) - Controller XIV - Exhaust Port and Waste Gas Treatment Interface X - Vacuum Interface III - Fixed Rotating Device III - Support Base II - Sealing Device III - Inner Feed Pipe II - Reaction Chamber III - Reactor III - Silicon Carbide Tube IV - Basalt Fiber Layer IV 256 – Stainless steel plate VII, 257 – Magnetron VII, 258 – Heating box II, 259 – Sealing device IV, 260 – Fixed rotating device IV, 261 – Temperature controller IX, 262 – Inert gas and flow meter interface III, 263 – Reaction gas and flow meter interface III, 264 – Discharge port XIV, 265 – Cooling furnace, 266 – Inlet XV, 267 – Controller XV, 268 – Temperature controller X, 269 – Inert gas and flow meter interface IV, 270 – Fixed rotating device V, 271 – Support base III, 272 – Sealing device V, 273 – Inlet inner pipe III, 274 – Cooling chamber, 275 – Quartz cooler, 276 – Sealing device VI, 277 – Fixed rotating device VI, 278 – Exhaust port and waste gas Processing Interface XI, 279 - Vacuum Interface IV, 280 - Discharge Port XV, 281 - Vacuum Interface V, 282 - Vacuum Packaging Machine, 283 - Product Vacuum Packaging Interface, 284 - Vacuum Return Bucket, 285 - Conveyor Belt IV, 286 - Quality Control, 287 - Product Vacuum Packaging Bucket, 288 - Product Warehouse, 289 - Power Supply System, 290 - Vacuum System, 291 - Temperature Control System, 292 - Gas Control System, 293 - Water Cooling System, 294 - Water Production System, 295 - Reagent Preparation System, 296 - Waste Gas Treatment System, 297 - Waste Liquid Treatment System, 298 - Solid Waste Treatment System, 299 - Monitoring System I, 300 - Monitoring System II, 301 - Monitoring System III, 302 - Monitoring System IV303 - Monitoring System V. Detailed Implementation
[0025] To make the objectives, technical solutions, and advantages of this invention clearer, the invention will be further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative and not intended to limit the invention.
[0026] Example 1: A smart manufacturing equipment for ultra-high purity quartz sand used in semiconductors, such as Figure 1-8 As shown, it includes an intelligent equipment rack 1, a system intelligent control center 2, a material preparation system 3, a high-purity quartz sand purification system 4, an ultra-high-purity quartz sand purification system 5, a quality control and product collection and processing system 6, a process auxiliary system 7, and a system monitoring center 8. The intelligent control center 2 system includes: material preparation system 3, high-purity quartz sand purification system 4, ultra-high purity quartz sand purification system 5, quality control and product collection and processing system 6, process auxiliary system 7, and system monitoring center 8; The material preparation system 3 includes: an intelligent ore bin 10, a raw ore mobile lifting trough washing machine 15, a raw ore crushing and grading integrated machine 21, a color sorter 29, a vacuum microwave roasting furnace 44, a gradient reaction vessel I 62, a ball mill 80, and a hydrocyclone classifier 90; the intelligent ore bin 10 includes: an inlet, an outlet, a raw ore inlet 11, and a conveyor belt 12I; the raw ore mobile lifting trough washing machine 15 includes: a feed inlet I 13, an ultrapure water interface I 14, a rotating high-pressure rinsing water cover 16, a waste liquid treatment interface I 17, a discharge outlet I 18, and a conveyor belt II 19; the raw ore crushing... The integrated grading machine 21 includes: discharge port II 22, return hopper 23, fine crushing and grading machine 24, medium crushing and grading machine 25, coarse crushing and grading machine 26, feed port II 27, and exhaust port and waste gas treatment interface I 28; the color sorter 29 includes: feed port III 31, vibrating feeder 32, signal processor 33, chute 34, light source 35, sensor 36, compressed air 37, spray valve 38, discharge port III 39, and impurity box 40; the vacuum microwave roasting furnace 44 includes: exhaust port and waste gas treatment interface II 41, feed port IV 42, and vacuum interface I 45. Temperature controller I46, furnace shell I47, magnetron I48, stainless steel plate I49, basalt fiber I50, silicon carbide tube I51, quartz tube I52, reaction chamber I53, reaction gas and flow meter interface I54, inert gas and flow meter interface I55, discharge port IV56; gradient reactor I62 includes: feed port V57, timer I59, temperature controller II60, auxiliary material inlet I61, pressure gauge I63, exhaust port and waste gas treatment interface III64, ultrapure water interface II65, furnace shell II66, magnetron II67, stainless steel plate I49, basalt fiber I50, silicon carbide tube I51, quartz tube I52, reaction chamber I53, reaction gas and flow meter interface I54, inert gas and flow meter interface I55, discharge port IV56; Steel plate II 68, lining I 69, waste liquid discharge channel I 70, gradient acid leaching tank I 71, cleaning device I 72, waste liquid treatment interface II 73, discharge port V 74; ball mill 80 includes: feed port VI 75, return port 76, ultrapure water interface III 78, feeding device 79, base 81, ball milling media 82, ball milling chamber 83, gears and vibration device 84, waste liquid treatment interface III 85, discharge device 86, discharge port VI 87; cyclone classifier 90 includes: underflow trough 88, underflow port 89, cyclone chamber 91, material pipe I 92; The high-purity quartz sand purification system 4 includes: a magnetic separator 96, a slurry preparation tank I 119, a flotation machine I 127, a slurry preparation tank II 144, a flotation tank II 152, a multi-functional reactor I 166, a vacuum microwave purification furnace 184, a gradient reactor II 214, and a multi-functional reactor II 225; the magnetic separator 96 includes: a water-cooled outlet 94, a water-cooled inlet 95, a material pipe II 97, a pulsation device 98, an excitation coil 99, an iron yoke 100, a feed inlet VII 101, a rotating ring 102, a magnetic medium 103, an ultrapure water interface IV 104, a rinsing water pipe 105, a magnetic material unloading hopper 106, rinsing water 107, a magnetic material box 108, and magnetic poles 109. Support base 110, waste liquid treatment interface IV 111, discharge port VII 112, non-magnetic material hopper 114; slurry mixing tank I 119 includes: material pipe III 115, slurry mixing tank inlet I 116, reagent and ultrapure water addition tank I 117, slurry mixing tank outlet I 118, stirring device I 120; flotation tank I 127 includes: material pipe IV 121, waste liquid treatment interface V 122, feed inlet VIII 124, timer II 125, temperature controller III 126, collection tank I 128, exhaust port and waste gas treatment interface IV 129, gas collection hood I 130, scraper device I 131, motor I 132, hollow shaft I 133, air pipe I 134, stator I 1 35. Impeller I 136, Ultrapure water interface V137, Ultrasonic device I 138, Discharge port VIII 139; Slurry preparation tank II 144 includes: feed pipe V140, slurry preparation tank inlet II 141, reagent and ultrapure water addition tank II 142, slurry preparation tank outlet II 143, stirring device II 145; Flotation tank II 152 includes: feed pipe VI 146, waste liquid treatment interface VI 147, feed inlet IX 149, timer III 150, temperature controller IV 151, collection tank II 153, exhaust port and waste gas treatment interface V154, gas collection hood II 155, scraper device II 156, motor II 157, hollow shaft II 158, air pipe II 159, stator II160, Impeller II161, Ultrapure Water Interface VI162, Ultrasonic Device II163, Discharge Port IX164; Multifunctional Reactor I166 includes: Material Pipe VII165, Auxiliary Material Inlet II167, Temperature Controller V168, Timer IV169, Inlet X170, Pressure Gauge II172, Exhaust Port and Waste Gas Treatment Interface VI173, Ultrapure Water Interface VII174, Furnace Shell III175, Magnetron III176, Stainless Steel Plate III177, Lining II178, Waste Liquid Discharge Channel II179, Cleaning Device II180, Multifunctional Rotary Acid Immersion Tank I181, Waste Liquid Treatment Interface VII182, Discharge Port X183;Vacuum microwave chlorination purification furnace 184 includes: feed inlet XI185, exhaust port and waste gas treatment interface VII187, vacuum interface II188, fixed rotating device I189, support base I190, sealing device I191, feed inner tube II192, reaction chamber II193, quartz reactor II194, silicon carbide tube II195, basalt fiber layer II196, stainless steel plate IV197, magnetron IV198, heating box I199, sealing device II200, fixed rotating device II201, temperature controller VI202, inert gas and flow meter interface II203, reaction gas and flow meter interface II204, and discharge port XI205; gradient reaction vessel II214 includes: feed inlet XII206, timer V208, temperature controller VII209, auxiliary material inlet III210, pressure gauge II211, exhaust port and waste gas treatment interface... Interface VIII 212, ultrapure water interface VIII 213, outer shell V215, magnetron V216, stainless steel plate V217, lining III 218, waste liquid discharge channel III 219, gradient acid leaching tank 220, acid leaching tank partition II 221, waste liquid treatment interface VIII 222, discharge port XII 223; multi-functional reactor II 225 includes: feed pipe VIII 224, auxiliary material inlet IV 226, temperature controller VIII 227, timer V I228, Inlet XIII229, Pressure gauge Ⅳ231, Exhaust port and waste gas treatment interface IX232, Ultrapure water interface IX233, Furnace shell VI234, Magnetron VI235, Stainless steel plate VI236, Lining Ⅳ237, Waste liquid discharge channel Ⅳ238, Cleaning device Ⅳ239, Multifunctional rotary pickling tank Ⅱ240, Waste liquid treatment interface IX241, Outlet XIII242; The ultra-high purity quartz sand purification system 5 includes: a vacuum microwave plasma purification furnace 243; the vacuum microwave plasma purification furnace 243 includes: feed inlet XⅣ (return port) 244, exhaust port and waste gas treatment interface X246, vacuum interface Ⅲ247, fixed rotating device Ⅲ248, support base Ⅱ249, sealing device Ⅲ250, feed inner tube Ⅱ251, reaction chamber Ⅲ252, reactor Ⅲ253, silicon carbide tube Ⅳ254, basalt fiber layer Ⅳ255, stainless steel plate VII256, magnetron VII257, heating box Ⅱ258, sealing device Ⅳ259, fixed rotating device Ⅳ260, temperature controller IX261, inert gas and flow meter interface Ⅲ262, reaction gas and flow meter interface Ⅲ263, and discharge port XIV264; The quality control and product collection and processing system 6 includes: a cooling furnace 265, a vacuum packaging machine 282, a vacuum return bin 284, a conveyor belt IV 285, a quality control system 286, and a product storage bin 288; the cooling furnace 265 includes: a feed inlet XV 266, a temperature controller X268, an inert gas and flow meter interface IV 269, a fixed rotating device V270, a support base III 271, a sealing device V272, a feed inner tube III 273, a cooling chamber 274, a quartz cooler 275, a sealing device VI 276, a fixed rotating device VI 277, an exhaust port and waste gas treatment interface XI 278, a vacuum interface IV 279, and a discharge port XV 280; the vacuum packaging machine 282 includes: a vacuum interface V281, a product vacuum packaging interface 283, and a product vacuum packaging bin 287. The process auxiliary system 7 includes: power supply system 289, vacuum system 290, temperature control system 291, gas control system 292, water cooling system 293, water production system 294, reagent preparation system 295, waste gas treatment system 296, waste liquid treatment system 297, and solid waste treatment system 298. The monitoring system center 8 includes: monitoring system I 299, monitoring system II 300, monitoring system III 301, monitoring system IV 302, and monitoring system V 303; The intelligent equipment rack 1 has five layers. The first layer has two layers, one high and one low, on the right side. The intelligent control center 2 of the system is located at the left end of the lower layer of the first layer. The material preparation system 3 is located on the left side of the first and second layers, and on the left side of the third to fifth layers, extending horizontally to the right to 1 / 4 of the width. The high-purity quartz sand purification system 4 is located on the right side of the third to fifth layers, extending horizontally to the left to 3 / 4 of the width. The ultra-high purity quartz sand purification system 5 is located on the right side of the second layer. The quality control and product collection and processing system 6 is located on the right side of the upper and lower layers of the first layer. The process auxiliary system 7 is located on the left side of the lower layer. The system monitoring center 8 is located at the left end of the upper layer of the first layer. The intelligent ore bin 10, the raw ore mobile lifting trough washing machine 15, and the raw ore crushing and grading integrated machine 21 are arranged from right to left on the left side of the first layer; the color sorter 29 is arranged on the left side of the fifth layer, horizontally to the right to 1 / 4 of the width; the vacuum microwave roasting furnace 44 is arranged on the left side of the fourth layer, horizontally to the right to 1 / 4 of the width; the gradient reaction vessel I 62 is arranged on the left side of the third layer, horizontally to the right to 1 / 4 of the width; the ball mill 80 and the hydrocyclone classifier 90 are arranged from left to right on the left side of the second layer. Magnetic separator 96 is positioned horizontally to the right from 1 / 4 width to 1 / 2 width on the left side of the third layer; slurry preparation tank I 119 and slurry preparation tank II 144 are sequentially positioned horizontally to the left from 1 / 4 width to 1 / 2 width on the left side of the fourth layer; flotation machine I 127, flotation II 152, and multi-functional reactor I 166 are sequentially positioned from left to right on the right side of the fifth layer; vacuum microwave purification furnace 184 is positioned on the right side of the fourth layer; gradient reactor II 214 and multi-functional reactor II 225 are sequentially positioned from left to right on the right side of the third layer. The vacuum microwave plasma purification furnace 243 is located on the right side of the second layer; Cooling furnace 265 is located on the first high floor. On the right side of the lower floor, from right to left, are conveyor belt Ⅳ285, vacuum return barrel 284, quality control 286, vacuum packaging machine 282 and product warehouse 288. The power supply system 289, vacuum system 290, temperature control system 291, gas control system 292, water cooling system 293, water production system 294, reagent preparation system 295, waste gas treatment system 296, waste liquid treatment system 297, and waste solid treatment system 298 are arranged from right to left on the left side of the first floor. Monitoring system I 299 is located in area 3 of the material preparation system (right next to the top left of the center line of the second layer); monitoring system II 300 is located in area 4 of the high-purity quartz sand purification system (right next to the bottom right of the center line of the third layer); monitoring system III 301 is located in area 5 of the ultra-high purity quartz sand purification system (right next to the top right of the center line of the second layer); monitoring system IV 302 is located in area 6 of the quality control and product collection and processing system (right next to the top left of the upper layer of the first layer); and monitoring system V 303 is located in the process auxiliary system area (right next to the top left of the lower layer of the first layer). The intelligent mining bin 10 is equipped with an inlet and an outlet. The inlet is located on the left side of the intelligent mining bin 10 at a height of 600 mm from the top downwards, and the outlet is located directly below the bottom of the longitudinal center line of the intelligent mining bin 10, adjacent to the raw ore inlet 11. Both are connected to the top of the head end of the conveyor belt I 12. The right side of the tail end of the conveyor belt I 12 is connected to the inlet, and the left side of the tail end of the conveyor belt I 12 is connected to the feed inlet I 13. The feed inlet I13 is located directly above the raw ore mobile lifting trough washing machine 15, 2 meters above the ground. A rotating high-pressure flushing water hood 16 is installed at the bottom of the raw ore mobile lifting trough washing machine 15. A waste liquid treatment interface I17 is located at the bottom left side of the raw ore mobile lifting trough washing machine 15, and a discharge outlet I18 is located next to it. A conveyor belt II19 is located directly below the discharge outlet I18 and is vertically connected to the head end of the conveyor belt II19. The feed inlet 22 and the return hopper are also connected to the head end of the conveyor belt II19. The conveyor belt II19 has three vertically upward-facing sub-strips. The raw ore crushing and grading integrated machine 21 has a feed inlet II 27 located directly above the center line. From top to bottom, a coarse crushing and grading machine 26, a medium crushing and grading machine 25, and a fine crushing and grading machine 24 are arranged in sequence. The discharge outlet II 22 is located directly below the fine crushing and grading machine 24. The discharge outlet II 22 is connected to the head end of the third branch of the conveyor belt II 19 directly below, and the tail end of the third branch is connected to the feed inlet III 31. The fine crushing and grading machine 24 has return hoppers 23 on both sides. The right return hopper is connected to the head end of the first branch of the conveyor belt II 19, and the tail end of the first branch is connected to the feed inlet II 27. The left return hopper is connected to the head end of the second branch of the conveyor belt II 19, and the tail end of the second branch is connected to the feed inlet II 27. The raw ore crushing and grading integrated machine 21 has an exhaust port and waste gas treatment interface I 28 located at the front end of the top right side. The color sorter 29 has a feed inlet Ⅲ31 located directly above the top, which is not connected to the end of the conveyor belt Ⅱ19. A vibrating feeder 32 is located directly below it. The vibrating feeder 32 is inclined at a 15-degree angle and connected to a chute 34. The chute 34 is inclined at a 30-degree angle. Two pairs of light sources 35 are located at both ends of the extension line of the inclined line of the chute 34. A sensor 36 is located in the middle of each pair of light sources. The sensor is connected to a signal processor 33. The signal processor 33 is connected to a spray valve 38. The spray valve 38 is connected to compressed air 37. An impurity box 40 is located at the lower left end and a discharge port Ⅲ39 is located at the lower right end. A quartz tube I52 is set at the longitudinal center of the vacuum microwave roasting furnace 44. A feed port IV42 is set directly above the top of the quartz tube I52 and vertically connected to the discharge port III39. A discharge port IV56 is set directly below the bottom and vertically connected to the feed port V57 of the gradient reactor I62. A silicon carbide tube I51, a basalt fiber layer I50, and a stainless steel plate I49 are set out of the quartz tube I52 in sequence. A magnetron I48 is set on the stainless steel plate I49. A furnace shell I47 is installed outside the magnetron I48. An exhaust port and waste gas treatment interface II41 are set at the top right side of the quartz tube I52. A vacuum interface I45 and a temperature controller I are set from top to bottom at the top left side. A reaction gas and flow meter interface I54 and an inert gas and flow meter interface I55 are set from top to bottom at the bottom. A gradient acid leaching tank I71 is located inside the centerline of the gradient reaction vessel I62. The top of the gradient acid leaching tank I71 has a feed inlet V57 that is vertically connected to the discharge outlet IV56, and the bottom has a discharge outlet V74 that is vertically connected to the feed inlet VI75. To the left of the feed inlet V57, from the inside out, are arranged a timer I59, a temperature controller II60, and an auxiliary material inlet I61. To the right of the feed inlet V57, from the inside out, are arranged a pressure gauge I63, an exhaust port and a waste gas treatment interface III64, and an ultrapure water interface II65. Waste liquid treatment interfaces II73 are arranged on both sides of the discharge outlet V74. The waste liquid treatment interfaces II73 are connected to the waste liquid discharge channel I70. The waste liquid discharge channel I70 is connected to the cleaning device I72. The cleaning device I72 is connected to the ultrapure water interface II65. The gradient acid leaching tank I71 is arranged outward from the lining I69 and a stainless steel plate II68. A magnetron II67 is installed on the stainless steel plate II68. The furnace shell II66 is installed on the outside. The ball mill 80 has a ball milling chamber 83 set at the center of the horizontal direction. The ball milling chamber 83 contains ball milling media 82. The left end of the ball milling chamber 83 is equipped with a feeding device 79. The right head of the feeding device 79 is vertically connected to the base 81. The center of the left side of the feeding device 79 is equipped with an ultrapure water interface Ⅲ78. The top is equipped with a feed port V75, which is vertically connected to the discharge port V74. The right end of the ball milling chamber 83 is equipped with a gear and a rotating device 84. The center of the gear is equipped with a discharge device 86 and a discharge port VI87. The discharge port VI87 is connected to the left end of the material pipe Ⅰ92. The right end of the material pipe Ⅰ92 is connected to the cyclone chamber 91. The bottom flow channel 88 is set directly below the bottom of the cyclone chamber 91. The left side of the bottom flow channel 88 is equipped with a bottom flow port 89, which is connected to the return port 76. The top of the cyclone chamber 91 is equipped with an overflow port 93, which is connected to the material pipe Ⅱ97. Magnetic separator 96 has a magnetic pole 109 at its center, with its bottom connected to support frame 110. Water-cooled outlet 94 and water-cooled inlet 95 are located sequentially from top to bottom on the lower right side of the separator. Iron yokes 100 are located on either side of the magnetic pole 109, and excitation coils 199 are located on either side of the iron yokes 100. From right to left, feed inlet VII101 and rinsing water 104 are located on the top of the magnetic pole 109. Feed inlet VII101 is connected to material pipe 297 at its upper end and to iron yoke 100 at its lower end. Rinsing water 104 is connected to ultrapure water interface Ⅳ104 and magnetic material... The magnetic separator is connected to the mass tank 109. The ultrapure water interface Ⅳ104 is located on the upper left of the magnetic separator Ⅰ96 and is connected to the rinsing water pipe Ⅰ105. The waste liquid treatment interface Ⅳ111 is located on the lower left of the magnetic separator 96. The magnetic pole 109 is connected to the rotating ring 102. The magnetic medium 103 is set on the rotating ring 102. The upper end of the rotating ring 102 is connected to the magnetic material unloading hopper 106, and the lower end is connected to the non-magnetic material hopper 114. The non-magnetic material hopper 114 is connected to the pulsation device Ⅰ98. The bottom of the magnetic separator is provided with the discharge port VII112, which is connected to the material pipe Ⅲ115. A stirring device I120 is installed at the top center of the mixing tank I119. A reagent and ultrapure water addition tank I117 is installed on the upper part of the mixing tank I119. A mixing tank inlet I116 is installed at the lower left end. The mixing tank inlet I116 is connected to the material pipe III115. A mixing tank outlet I118 is installed at the upper left end. The mixing tank outlet I118 is connected to the material pipe IV121. A motor I132 is located at the center of flotation cell I127. Motor I132 is connected to a hollow shaft I133, which in turn connects to a stator I135. An impeller I136 is mounted on the outside of stator I135, which is connected to a material pipe IV121. The hollow shaft I133 is connected to an air pipe I134. A gas collecting hood I130 is installed at the top of flotation cell I127. An exhaust port and waste gas treatment interface IV129 are located on the upper left side of the gas collecting hood I130. The hollow shaft I133 is equipped with scraper device I131 and collection tank I128 on both sides. The upper left side of the flotation tank 121 is equipped with temperature controller III120 and timer 119, and the lower end is equipped with waste liquid treatment interface V116. The side edge connection of the flotation tank I127 is equipped with ultrasonic device I138. The upper right side of the flotation tank I127 is equipped with ultrapure water interface V131, and the lower end is equipped with discharge port VIII139, which is connected to material pipe V140. A stirring device II145 is installed at the center of the top of the mixing tank II144. A reagent and ultrapure water addition tank II142 is installed on the upper part of the mixing tank II144. A mixing tank inlet II141 is installed at the lower left end and connected to the material pipe V140. A mixing tank outlet II143 is installed at the upper right end and connected to the material pipe VI146. From top to bottom, motor II157 is installed at the center of flotation cell II152. Motor II157 is connected to hollow shaft II158, which is connected to stator II160. An impeller II161 is installed externally. Stator II160 is connected to material pipe VI146. Hollow shaft II158 is connected to air pipe II159. A gas collecting hood II155 is installed at the top of flotation cell II152. An exhaust port and waste gas treatment interface V154 are installed on the upper left side of the gas collecting hood II155. Scraper devices II156 are installed on both sides of hollow shaft II158. A collection tank II153 is set on the outer edge of the scraper device II156. A temperature controller II151 and a timer 150 are set on the upper left side of the flotation cell II152. A feed inlet IX149 is set on the lower side. A waste liquid treatment interface VI147 is set below the feed inlet IX149. An ultrasonic device II163 is set at the side edge connection of the flotation cell II152. An ultrapure water interface VI162 is set on the upper right side of the flotation cell II152. A discharge port IX164 is set on the lower side. The discharge port IX164 is connected to the feed pipe VII165. Multifunctional rotary acid leaching tank I181 is located on the longitudinal centerline of multifunctional reactor I166. A feed inlet X170 is located at the top of multifunctional rotary acid leaching tank I181, connected to feed pipe VII165. To the left of feed inlet X170, from the inside out, are arranged a timer IV169, a temperature controller V168, and an auxiliary material inlet II167. To the right, from the inside out, are a pressure gauge II172, an exhaust port and waste gas treatment interface VI173, and an ultrapure water interface VII174. Multifunctional rotary acid leaching tank I1... 81 has a discharge port X183 at the bottom, which is connected to the inlet XI185. Waste liquid treatment interfaces VII182 are set on both sides of the discharge port X183. Waste liquid treatment interfaces VII182 are connected to waste liquid discharge channel II179. Waste liquid discharge channel II179 is connected to cleaning device II180. Cleaning device II180 is connected to ultrapure water interface VII174. The multi-functional rotary acid leaching tank I181 is arranged outward from the lining II178, stainless steel plate III177, magnetron III176 and furnace shell III175 in sequence. A quartz reactor 194 is positioned on the horizontal centerline of a vacuum microwave chlorination purification furnace 184 at a downward tilt of 15 degrees. A feed inlet XI185 is located at the high end of the quartz reactor 194, perpendicularly connected to the vertical end of the feed inner tube I192 within a fixed rotating device I189. The inclined end of the feed inner tube I192 enters the reaction chamber II193, with the inclination matching that of the quartz reactor II194. The quartz reactor 194 passes through the heating box I199, connecting at its high end to the fixed rotating device I189 with a sealing device I191 at the connection point, and at its low end to the fixed rotating device II201 with a sealing device II200 at the connection point. The upper end of the fixed rotating device I189 is perpendicularly connected to the feed inlet XI185, and an exhaust port and a waste gas treatment interface VII1 are sequentially arranged from top to bottom on the left end. 87 and vacuum interface II188, the right end is connected to quartz reactor 194, the lower end is connected to support I190, support I190 is fixed on the fourth layer intelligent equipment rack 1, fixed rotating device II201 is connected to quartz reactor 194 on the left end, and the right end is set with temperature controller VI202, inert gas and flow meter interface II203, reaction gas and flow meter interface II204 from top to bottom, and discharge port XI205 is set at the lower end. Discharge port XI205 is vertically connected to the feed port XII206 of gradient reactor II214; heating box IV199 is set with silicon carbide tube II195, basalt fiber layer II196, and stainless steel plate IV197 from the inside to the outside. Magnetron IV198 is set on stainless steel plate IV197. Heating box IV199 is fixed on intelligent equipment rack 1; The gradient reactor II214 has an inlet XII206 at the top and an outlet XII223 at the bottom, located along its centerline. To the left of inlet XII206 are a timer V208, a temperature controller VII209, and an auxiliary material inlet III210. To the right of inlet XII206 are a pressure gauge II211, an exhaust port and waste gas treatment interface VIII212, and an ultrapure water interface VIII213. Waste liquid treatment interfaces VIII2 are located on both sides of outlet XII223. 22. Waste liquid treatment interface VIII222 is connected to waste liquid discharge channel Ⅲ219. Waste liquid discharge channel Ⅲ219 is connected to cleaning device Ⅲ221. Cleaning device Ⅲ221 is connected to gradient acid leaching tank Ⅱ220. Gradient acid leaching tank Ⅱ220 is connected to ultrapure water interface VIII213. Gradient reaction vessel Ⅱ214 is equipped with gradient acid leaching tank Ⅱ220. Gradient acid leaching tank Ⅱ220 is arranged outward from the lining Ⅲ218, stainless steel plate V217, magnetron V216 and outer shell V215 in sequence. Multifunctional rotary acid leaching tank II240 is located at the center line of multifunctional reactor II225. Inlet XIII229 is located at the top of multifunctional rotary acid leaching tank II240. Inlet XIII229 is connected to feed pipe VIII224. The left end of inlet XIII229 is connected to outlet XII223, and the right end is connected to inlet XIII229. To the left of inlet XIII229, from the outside in, are arranged the auxiliary material inlet IV226, temperature controller VIII227, and timer VI228. To the right, from the inside out, are arranged the pressure gauge IV231, exhaust port and waste gas treatment interface IX232, and ultrapure... Water interface IX233; multi-functional rotary acid leaching tank II240 has a discharge port XIII242 at the bottom; waste liquid treatment interfaces IX241 are set on both sides of the discharge port XIII242; waste liquid treatment interfaces IX241 are connected to waste liquid discharge channel IV238; waste liquid discharge channel IV238 is connected to cleaning device IV239; cleaning device IV239 is connected to ultrapure water interface IX233; multi-functional rotary acid leaching tank II240 is arranged outwards in sequence as lining IV237, stainless steel plate VI236, magnetron VI235 and furnace shell VI234; A reactor Ⅲ253 is positioned at the horizontal centerline of a vacuum microwave plasma purification furnace 243, tilted downwards at a 15-degree angle. Reactor Ⅲ253 passes through a heating box Ⅱ258. A feed inlet ⅩⅣ (return port) 244 is located at the high end of reactor Ⅲ253, and a discharge port XIII242 is located at the low end. The upper end of feed inlet ⅩⅣ (return port) 244 is connected to discharge port XIII242, and the lower end is vertically connected to the vertical end of the feed inner tube Ⅱ251 within a fixed rotating device Ⅲ247. The inclined end of the feed inner tube Ⅱ251 enters the reaction chamber Ⅲ252, with the inclination matching that of reactor Ⅲ253. The high end of reactor Ⅲ253 is connected to fixed rotating device Ⅲ248, with a sealing device Ⅲ250 at the connection point. The low end is connected to fixed rotating device Ⅳ260, with a sealing device Ⅳ259 at the connection point. The upper end of fixed rotating device Ⅲ248 is connected to the feed... The left end of the device is connected to the exhaust port and waste gas treatment interface X246 and vacuum interface Ⅲ247 from top to bottom. The right end is connected to the reactor Ⅲ253 and the lower end is connected to the support base Ⅱ249. The support base Ⅱ249 is fixed on the second layer of intelligent equipment rack 1. The left end of the fixed rotating device Ⅳ260 is connected to the reactor Ⅲ253. The right end is connected to the temperature controller IX261, inert gas and flow meter interface Ⅲ262 and reaction gas and flow meter interface Ⅲ263 from top to bottom. The lower end is connected to the discharge port XIV264 and vertically connected to the feed port XV266. The heating box Ⅱ258 is connected to the silicon carbide tube Ⅳ254, basalt fiber layer Ⅳ255 and stainless steel plate VII256 from the inside to the outside. The magnetron VII257 is installed on the stainless steel plate VII256. The heating box Ⅱ258 is fixed on the intelligent equipment rack 1. A quartz cooler 275 is installed at the horizontal centerline of the cooling furnace 265 at a downward tilt of 15 degrees. A fixed rotating device V270 is installed at the high end of the quartz cooler 275. The upper end of the fixed rotating device V270 is vertically connected to the feed port XV266. The left end is provided with a temperature controller X268 and an inert gas and flow meter interface Ⅳ269 from top to bottom. The lower end is connected to the support base Ⅲ271. The support base Ⅲ271 is fixed on the intelligent equipment frame 1. The right end of the fixed rotating device VI277 is connected to the quartz cooler 275. The right end is provided with an exhaust port and waste gas treatment interface XI278 and a vacuum interface Ⅳ279 from top to bottom. The lower end is provided with the discharge port XV280. Vacuum packaging machine 282 has a vacuum interface V281 on the top right side, a vacuum packaging interface 283 on the top center of the machine, which is vertically connected to the discharge port XV280 and vertically connected to the product vacuum packaging barrel 287. Controller I9 connects to the intelligent ore bin 10 and the raw ore mobile lifting trough washing machine 15; Controller II 20 connects to the raw ore crushing and grading integrated machine 21; Controller III 30 connects to the color sorter 29; Controller IV 43 connects to the vacuum microwave roasting furnace 44; Controller V58 connects to the gradient reactor I 62; Controller VI 77 connects to the ball mill 80 and the hydrocyclone classifier 90; Controller VII 113 connects to the magnetic separator 96; Controller VIII 123 connects to the slurry mixing tank I 119 and the flotation tank I 127; Controller IX 148 connects to the slurry mixing tank II 144 and the flotation tank II 152; Controller X 171 connects to the multi-functional reactor I 166; Controller XI 186 connects to the vacuum microwave purification furnace 184; Controller XII 207 connects to the gradient reactor II 214; Controller XIII 230 connects to... Connect to multi-functional reactor II 225; controller XIV 245 is connected to vacuum microwave plasma purification furnace 243; controller XV 267 is connected to cooling furnace 265, vacuum packaging machine 282, vacuum return barrel 284, conveyor belt IV 285, quality control 286 and product warehouse 288 respectively; controller I 9, controller II 20, controller III 30, controller IV 43, controller V58, controller VI 77, controller VII 113, controller VIII 123, controller IX 148, controller X171, controller XI 186, controller XII 207, controller XIII 230, controller XIV 245 and controller XV 267 are connected to different composite quartz sensors (temperature, pressure, time, chemical composition, etc.) according to the control process parameters; The linings of the raw ore mobile lifting tank washing machine 15 and the raw ore crushing and grading integrated machine 21 are all made of pollution-free materials; the gradient reactor I 62 and gradient reactor II 214 are equipped with gradient acid leaching tanks to achieve gradient acid leaching and cleaning; the multi-functional reactor I 166 and multi-functional reactor II 225 are equipped with multi-functional rotary acid leaching tank I 181 and multi-functional rotary acid leaching tank II 240 to achieve acid leaching, cleaning and drying. The linings of the gradient reactor I 62, multi-functional reactor I 166, gradient reactor II 214 and multi-functional reactor II 225 are all made of pollution-free, acid-resistant, high-temperature resistant and pressure-resistant high-quality materials. Both flotation cell I127 and flotation cell II152 are equipped with gas collection hoods I130 and II155 to collect waste gas, and ultrasonic devices are installed at the radial joint of flotation cell I127 and flotation cell II152. The inner wall of the reaction chamber I53 of the vacuum microwave roasting furnace 44 is provided with quartz spiral reinforcing ribs; the reactors II194 and III253 of the vacuum microwave purification furnace 184 and the vacuum microwave plasma purification furnace 243 all use high-purity, high-quality quartz tubes with internal straight reinforcing ribs; the microwave generators used in the vacuum microwave roasting furnace 44, the vacuum microwave purification furnace 184 and the vacuum microwave plasma purification furnace 243 are preferably 2.45 GHz microwave power sources, and the silicon carbide tubes used are hollow tubes; The system intelligent control center 2 is connected to the material preparation system 3, the high-purity quartz sand purification system 4, the ultra-high-purity quartz sand purification system 5, the quality control and product collection and processing system 6, the process auxiliary system 7, and the system monitoring center 8. The system monitoring center 8 is connected to monitoring systems I 299, II 300, III 301, IV 302, and V 303. Monitoring system I 299 is connected to the material preparation system 3; monitoring system II 300 is connected to the high-purity quartz sand purification system 4; monitoring system III 301 is connected to the ultra-high-purity quartz sand purification system 5; monitoring system IV 302 is connected to the quality control and product collection and processing system 6; and monitoring system V 303 is connected to the process auxiliary system 7. The power supply system... System 289 is connected to the system intelligent control center 2, material preparation system 3, high-purity quartz sand purification system 4, ultra-high-purity quartz sand purification system 5, quality control and product collection and processing system 6, process auxiliary system 7, and system monitoring center 8, respectively; vacuum system 290 is connected to vacuum interface I 45, vacuum interface II 188, vacuum interface III 247, vacuum interface IV 279, and vacuum interface V281, respectively; temperature control system 291 is connected to temperature controller I 46, temperature controller II 60, temperature controller III 126, temperature controller IV 151, temperature controller V168, temperature controller VI 202, temperature controller VII 209, temperature controller VIII 227, temperature controller IX 261, and temperature controller X 268, respectively; gas control system 292 is connected to... Connect to the following interfaces: Reactant Gas and Flow Meter Interface I54, Inert Gas and Flow Meter Interface I55, Inert Gas and Flow Meter Interface II203, Reactant Gas and Flow Meter Interface II204, Inert Gas and Flow Meter Interface III262, Reactant Gas and Flow Meter Interface III263, and Inert Gas and Flow Meter Interface IV269; Water Cooling System 293 connects to Water Cooling Outlet Interface 94 and Water Cooling Inlet Interface 95 respectively; Water Purification System 294 connects to Ultrapure Water Interface I14, Ultrapure Water Interface II65, Ultrapure Water Interface III78, Ultrapure Water Interface IV104, Ultrapure Water Interface V137, Ultrapure Water Interface VI162, Ultrapure Water Interface VII174, Ultrapure Water Interface VIII213, and Ultrapure Water Interface IX233 respectively; This process uses... Water is connected to the water purification system 294; the reagent preparation system 295 and the water purification system 294 are respectively connected to the reagent and ultrapure water addition tank I117 and the reagent and ultrapure water addition tank II142; the exhaust gas treatment system 296 is respectively connected to the exhaust port and exhaust gas treatment interface I28, exhaust port and exhaust gas treatment interface II41, exhaust port and exhaust gas treatment interface III64, exhaust port and exhaust gas treatment interface IV129, exhaust port and exhaust gas treatment interface V154, exhaust port and exhaust gas treatment interface VI173, exhaust port and exhaust gas treatment interface VII187, exhaust port and exhaust gas treatment interface VIII212, exhaust port and exhaust gas treatment interface IX232, exhaust port and exhaust gas treatment interface X246, and exhaust port and exhaust gas treatment interface XI278;Waste liquid treatment system 297 is connected to waste liquid treatment interfaces I16, II73, III85, IV111, V122, VI147, VII182, VIII222, IX241, and IX241 respectively; the treated water from waste liquid treatment system 297 can be connected to water treatment system 294; the solid waste treatment system 298 is connected to impurity tank 40 and magnetic material tank 108 respectively.
[0027] Example 2: Based on the above embodiment one, a smart manufacturing process for ultra-high purity quartz sand for semiconductors is disclosed, such as... Figure 9 As shown, the process includes the following four stages and a total of seven steps. The first stage is material preparation, including step one; the second stage is high-purity quartz purification, including steps two to five; the third stage is ultra-high-purity quartz purification, including step six; and the fourth stage is quality control and product collection and processing, including step seven. The apparatus of Example 1 is used, and the specific steps are as follows: Step 1: Raw material preparation: This includes raw ore beneficiation, raw ore storage, raw ore washing, crushing and grading, color sorting, chlorination calcination, acid leaching, and ball milling and grading to obtain qualified raw materials with a particle size of 0.1-0.3 mm, a purity of 4N or higher, and controllable impurities. Start the system intelligent control center 2 and input the material preparation process parameters: Select high-purity quartz ore quality: SiO2 mass fraction higher than 3N, total impurities <100μg / g; Preferred quality meets the reference standard: total impurity element (μg / g) <50, including Al <30, Ti <10, Na <8, K <8, Li <5, Ca <5, Fe <3, P <2 and B <1, and trace amounts of radioactive elements and gas-liquid inclusions; Reserve process parameters: ore reserve quantity: 72 hours continuous... Continued production ore consumption; Soaking process parameters: raw ore soaking agent 8%~12%H2C2O4+1%~10%HF, soaking time 4~24 hours, rinsing water pressure 1~10MPa; Crushing and grading process parameters: coarse crushing particle size 10~30mm, medium crushing particle size 5~10mm, fine crushing particle size 1~5mm; Color sorting process parameters: color sorting particle size range 0.08~5mm, color threshold: a narrow range close to white, spraying intensity: air valve pressure 0.4~0.6MPa; Chlorine Calcination process parameters: vacuum degree 0.1~0.01Pa, temperature 600~1200℃, time 1~4h, mixed gas flow rate 10~100sccm, Ar flow rate (above 5N) 10~100sccm, HCl gas flow rate (above 5N) 10~100sccm; Microwave acid leaching process parameters: gradient acid leaching is achieved by sequentially using acid leaching agents 1~3: acid leaching agent 1: H2C2O4 8~12%, acid leaching agent 2: acid ratio HF 3~10% + H2C2O4 10%. ~12%, acid leaching agent 3: acid ratio HF3~10% + H2C2O48~12% + H2SiF6, liquid-solid ratio 2:1~4:1, acid leaching pressure 0.5~1MPa, acid leaching temperature 60~120℃, acid leaching time 30~240min, ultrapure water microwave cleaning, ultrapure water quality: resistivity ≥18.2MΩ·cm, ball milling classification process parameters: ball milling feed particle size 1~5mm, ball milling time 1~6h, cyclone classification discharge particle size 0.1~0.3mm; Selected high-purity quartz ore is fed into conveyor belt I12 via ore inlet 11 by controller I9 and first transported to intelligent ore bin 10. After the ore storage is completed, it is directly transported to feed inlet I13 and metered into ore mobile lifting tank washing machine 15 at a liquid-solid ratio of 2:1. At the same time, 8% H2C2O4 + 3% HF ore soaking agent is introduced through reagent preparation system 295. After soaking for 8 hours, the rotating high-pressure rinsing water cover 16 connected to ultrapure water interface I14 is opened for repeated rinsing. Waste liquid is discharged through waste liquid treatment interface I17 and connected to waste liquid treatment system 297 for treatment to meet standards before being discharged or returned to the water treatment system for water production. The washed quartz ore flows into conveyor belt II19 through discharge outlet I18 and is transported to feed inlet II27 via the first sub-belt. Controller II20 controls the raw material to enter the raw ore crushing and grading integrated machine 21 through feed inlet II27. The raw material is crushed and graded step by step by coarse crusher 26, medium crusher 25 and fine crusher 24 to obtain raw materials with a coarse crushing particle size of 10mm, a medium crushing particle size of 5mm and a fine crushing particle size of 1mm respectively. The waste gas generated during the crushing and grading process is treated by exhaust port and waste gas treatment interface I28. The raw material that fails the crushing and grading process flows into the first and second sub-belts of conveyor belt II19 through return hopper 23 and is transported to feed inlet II27 for repeated crushing and grading until it is qualified. The qualified raw material flows into the third sub-belt of conveyor belt II19 through discharge port II22 and is transported to feed inlet III31. Controller Ⅲ30 controls 1mm raw material to enter the color sorter 29 through feed inlet Ⅲ31 and flow into vibrating feeder 32. Vibrator 32 makes the raw material flow evenly along chute 34 into the sorting area composed of light source 35, sensor 36 and signal processor 33, forming a single layer and continuous raw material flow to ensure that each raw material is accurately detected. Light source 35 illuminates the raw material, sensor 36 receives the light signal reflected or transmitted by the raw material and converts it into an electrical signal (material color and optical characteristics), which is analyzed and processed by signal processor 33. The compressed air 37 and spray valve 38 are separately executed to control the air pressure of the air valve to 0.6MPa to remove unqualified raw material into impurity box 40 and send it to waste solid treatment system 298 for processing. Qualified raw material flows into feed inlet Ⅳ42 through discharge outlet Ⅲ39. Controller IV43 controls process parameters to allow raw materials to enter the vacuum microwave roasting furnace 44 for chlorination calcination. Vacuum is drawn to a vacuum level of 0.1 Pa through vacuum interface I45. Temperature controller I4 controls the temperature at 1000℃. The flow rate of the reaction mixture is controlled at 60 cm³ / s according to the mixed gas volume ratio of HCl 90% + Ar 10% through reaction gas and flow meter interfaces I54 and I55. 3 / min, after chlorination and calcination for 2 hours, the feed is directly fed into the gradient acid leaching tank I71 through the feed inlet V57 for acid leaching; The controller V58 controls the raw materials to enter the gradient pickling tank I71 through the feed inlet V57 at a liquid-to-solid ratio of 2:1, and introduces the pickling agent through the auxiliary material inlet I61. In the first layer of the gradient pickling tank I71, pickling agent 1: H2C2O4 18% is introduced, pickling agent 2: acid ratio HF 3% + H2C2O4 8% is introduced, and pickling agent 3: acid ratio HF 3% + H2C2O4 8% + H2SiF6 is introduced. Ultrapure water is introduced into the lower layer through the ultrapure water interface II65. The pressure is controlled at 1MPa by the pressure gauge I63, the temperature is controlled at 70℃ by the temperature controller II60, and the timer I59 controls the time at 60 minutes. After the pickling is completed layer by layer, it automatically flows into the next layer. After microwave cleaning in the lower layer, it flows into the feed inlet VI75 through the discharge outlet V74. The waste liquid of each layer is discharged through the waste liquid discharge channel I70 to the waste liquid treatment interface II73 for treatment. The waste gas is treated through the exhaust port and the waste gas treatment interface III64. The raw material is controlled by the controller VI77 to enter the ball mill 80 through the feed port VI75 with a feed particle size of 1mm. Zirconium balls of different diameters are introduced into the ball mill media 82 according to the product particle size distribution. After ball milling for 6 hours, the raw material enters the cyclone chamber 91 through the discharge port VI87. The raw material with unqualified particle size enters the underflow trough 88 and flows into the return port 76 from the underflow port 89. It then enters the ball mill 80 again for repeated grinding until it is qualified. The raw material with a particle size of 0.1mm swirls to the overflow port 93 and flows into the feed pipe II 97. Step 2: High gradient magnetic separation: A vertical ring pulsating high gradient wet magnetic separator is preferred to remove magnetic impurities; Input the high-gradient magnetic separation process parameters into the system's intelligent control center 2: 1.5–2.0T background magnetic field, slurry concentration 25%–30%, pulse frequency 200–300 times / min, feed particle size controlled at -0.074mm with a percentage ≥80%, and washing water volume controlled at 1–2 m³ / min. 3 / t of ore, ensuring timely discharge of magnetic products and avoiding secondary adsorption; The controller VII113 selects a 1.6T background magnetic field, a slurry concentration of 30%, and a pulse frequency of 280 times / min. The raw material from feed pipe II97 flows through inlet VII101 along the upper yoke 100 and through rotating ring 102. Magnetic particles are adsorbed by the magnetic medium 103 and carried by rotating ring 102 to the bottom non-magnetic field zone. The flushing water volume is controlled at 2m³. 3 / t of ore is rinsed with flushing water pipe 105 and finally enters magnetic impurity box 108. The magnetic media can be prevented from being blocked by backflushing magnetic impurities and material pulsation. The pulsation separation efficiency is high. The raw material passes through the magnetic media pile under the action of gravity and pulsating fluid force, and is separated from magnetic particle impurities. It enters material pipe Ⅲ115 from discharge port VII112. Step 3: Ultrasonic flotation: The prepared slurry is subjected to two ultrasonic flotations and ultrasonic cleaning to remove gangue mineral impurities using the ultrasonic temperature-controlled flotation machine of this invention. Input the pulp conditioning and ultrasonic flotation process parameters in the system's intelligent control center 2: Primary pulp conditioning and ultrasonic flotation process parameters: Use a combined reagent system (oleic acid + dodecylamine + pH 2.5–3.5) and a microbubble flotation column (bubble diameter ≤ 50 μm) to remove silicate mineral impurities such as feldspar and mica; impeller speed 100–300 rpm; aeration rate 0.2–0.5 m³ / h. 3 / (m²·min), pulp concentration 20%~40%, ultrasonic frequency 20~40kHz, flotation temperature 30~50℃, flotation time 20~60min, ultrasonic cleaning with ultrapure water, ultrapure water quality: resistivity ≥18.2MΩ·cm; secondary pulp conditioning and ultrasonic flotation process parameters: for different mineral impurities, optimize the primary flotation reagent system, intelligently adjust the reagent dosage, adjust the pH value, ultrasonic flotation, and ultrasonic cleaning with ultrapure water to effectively remove various gangue mineral impurities; The raw material is controlled by the controller VIII123 to enter the slurry tank I119 through the inlet I116 of the slurry tank via the feed pipe III115. The flotation agent (oleic acid + dodecylamine + pH2.5 + ultrapure water) is added from the reagent and ultrapure water addition tank I117. The slurry is fully stirred and adjusted by the stirring device I120 to control the slurry concentration at 30%. The slurry enters the feed pipe IV121 through the outlet I118 of the slurry tank. The raw material is controlled by controller VIII123 to enter flotation cell I127 through feed inlet VIII124 via feed pipe IV121. Timer II125 sets the time to 60 minutes, and temperature controller III126 sets the temperature to 35℃. Motor I132 is started, and stator I135 and impeller I136 rotate at high speed, generating strong vortices and a negative pressure zone within the cell. This negative pressure forces air through air pipe I134 at a rate of 0.5 m³ / min. 3 / (m²·min), the slurry is strongly drawn in from the hollow shaft I33. The impeller I136 disperses the small bubbles of the drawn-in air and makes them evenly dispersed in the entire slurry. The ultrasonic device I138 is turned on to accelerate the stirring and ensure that the mineral impurities are in a suspended state. Under the action of the collector, the surface of the mineral impurities becomes hydrophobic, increasing the probability of collision between impurity particles and bubbles, and they adhere to the bubbles, float up, and form a bubble layer. The foam is scraped off by the scraper device I131 and sent to the collection tank I128. After the flotation is completed, ultrapure water is introduced through the ultrapure water interface V137 for ultrasonic cleaning and then enters the feed pipe V140 through the discharge port VIII139. The waste liquid is treated through the waste liquid treatment interface V122, and the waste gas from the gas collection hood I130 is treated through the exhaust port and the waste gas treatment interface IV129. Controller IX148 controls the raw material in feed pipe V140 to enter the slurry tank II144 through the inlet II141 of the slurry tank. Optimized flotation agent is added from the reagent and ultrapure water addition tank II142. The slurry is fully stirred and adjusted by the stirring device II145 to control the slurry concentration at 30%. The slurry enters VI146 through the outlet II143 of the slurry tank. The raw material is controlled by the controller IX148 to enter the flotation cell II152 through the feed inlet IX149 via the feed pipe VI146. The timer Ⅲ150 sets the time to 60 minutes, and the temperature controller Ⅳ151 sets the temperature to 35℃. The motor II157 is started, and the stator II160 and impeller II161 rotate at high speed, generating strong eddies and a negative pressure zone in the cell. The negative pressure forces air into the air pipe II159 at a rate of 0.5m³. 3 / (m²·min) The slurry is strongly drawn in from the hollow shaft II158. The impeller II161 disperses the small bubbles of the drawn-in air and makes them evenly dispersed in the entire slurry. The ultrasonic device II163 is turned on to accelerate the stirring and ensure that the mineral impurities are in a suspended state. Under the action of the collector, the surface of the mineral impurities becomes hydrophobic, increasing the probability of collision between impurity particles and bubbles. They adhere to the bubbles, float up, and form a bubble layer. The foam is scraped off by the scraper device II156 and sent to the collection tank II153. After the flotation is completed, ultrapure water is introduced through the ultrapure water interface VI162 for ultrasonic cleaning and then enters the feed pipe VII165 through the discharge port IX164. The waste liquid is treated through the waste liquid treatment interface VI147. The waste gas from the gas collection hood II155 is treated through the exhaust port and the waste gas treatment interface V154. Step 4: Microwave acid leaching: Microwave acid leaching, microwave cleaning, and microwave drying are performed using the microwave multifunctional reactor of this invention to remove impurities from the inclusions. Input the microwave acid leaching process parameters in the system intelligent control center 2: acid ratio of leaching agent: HCl 20~30% + H2C2O4 10~20% + HF 3~5%, liquid-solid ratio 2:1~4:1, acid leaching pressure 0.5~1MPa, acid leaching temperature 60~120℃, acid leaching time 30~240min, microwave cleaning with ultrapure water, ultrapure water quality: resistivity ≥18.2MΩ·cm, microwave drying temperature 100~120℃; The controller X171 controls the raw material through the feed pipe VII165 to enter the multi-functional rotary pickling tank Ⅰ181 through the feed inlet X170 at a liquid-to-solid ratio of 2:1. The pickling agent HCl30%+H2C2O420%+HF3% is introduced through the auxiliary material inlet Ⅱ167. The temperature is controlled at 70℃ by the temperature controller V168, the timer Ⅳ169 controls the time at 60 minutes, and the pressure gauge Ⅱ172 controls the pressure at 1MPa. After pickling, microwave cleaning is performed. After microwave drying at 100℃, the raw material flows into the feed inlet XI185 through the discharge outlet X183. The cleaning device Ⅱ180 introduces ultrapure water through the ultrapure water interface VII174. The waste liquid is discharged through the waste liquid discharge channel Ⅱ179 to the waste liquid treatment interface VII182 for treatment. The waste gas is treated through the exhaust port and the waste gas treatment interface VI173. Step 5: Vacuum chlorination combined with hot pressing acid leaching for fine purification: Using the vacuum microwave purification furnace of this invention in conjunction with a microwave reactor, first remove lattice impurities by vacuum microwave treatment, then directly remove burst micro-nano-scale inclusions by microwave acid leaching, followed by microwave cleaning and microwave drying to obtain high-purity quartz sand with a purity of 5N or higher. Input the chlorination process parameters into the system's intelligent control center 2: vacuum degree 0.1~0.01Pa, temperature 600~1200℃, time 30~240min, mixed gas flow rate 10~100sccm, Ar gas flow rate (above 5N) 10~100sccm, HCl gas flow rate (above 5N) 10~100sccm, environment: Class 100 cleanliness; microwave acid leaching process parameters: primary acid leaching: gradient acid leaching is achieved by sequentially using acid leaching agents 1~3: acid leaching agent 1: H2C2O 48~12%, acid leaching agent 2: acid ratio HF 3~10% + H2 C2O4 10~12%, acid leaching agent 3: acid ratio HF 3~10% + H2C2O4 8~12% + H2SiF6, secondary acid leaching: acid leaching agent acid ratio: HCl 20~30% + H2SO4 10~20% + HF 3~5%, liquid-solid ratio 2:1~4:1, acid leaching pressure 0.5~1MPa, acid leaching temperature 60~120℃, acid leaching time 30~240min, ultrapure water microwave cleaning, ultrapure water quality: resistivity ≥18.2MΩ·cm, microwave drying temperature 100~120℃, total impurities less than 8ppm; The raw material is controlled by the controller XI186 to enter the reaction chamber Ⅱ193 through the feed port XI185. The rotating device is turned on, and the vacuum is drawn to 0.01Pa through the vacuum interface Ⅱ188. The temperature is controlled at 1000℃ by the temperature controller VI202. The flow rate of the mixed gas is controlled at 50cm3 / min through the inert gas and flow meter interface Ⅱ203 and the reaction gas and flow meter interface Ⅱ204. After chlorination for 60 minutes, the gas enters the feed port XII206 through the discharge port XI205. The waste gas passes through the exhaust port and the waste gas treatment interface VII187. Controller XII207 controls the raw materials to enter the gradient pickling tank II220 through inlet XII206 at a liquid-to-solid ratio of 2:1, and introduces the pickling agent through auxiliary material inlet III210. In the gradient pickling tank II220, pickling agent 1 (H₂C₂O 48%) is introduced in the first layer, pickling agent 2 (HF 3% + H₂C₂O 48%) in the second layer, and pickling agent 3 (HF 3% + H₂C₂O 48%) in the third layer. H2C2O48%+H2SiF6, ultra-high purity water is introduced into the lower layer through ultrapure water interface VIII213, pressure is controlled at 1MPa by pressure gauge II211, timer V208 controls time at 60min / layer, and temperature is controlled at 70℃ by temperature controller VII209. After acid leaching, it automatically flows into the next layer. After microwave cleaning of the lower layer, it flows into material pipe VIII224 through discharge port XII223. Waste liquid is discharged to waste liquid treatment interface VIII222 through waste liquid discharge channel III219 for treatment. Waste gas is treated through exhaust port and waste gas treatment interface VIII212. The controller XIII230 controls the raw material through the feed pipe VIII224 to enter the multi-functional rotary acid leaching tank II240 through the feed inlet XIII229 at a liquid-to-solid ratio of 2:1. The acid leaching agent is introduced through the auxiliary material inlet IV226. The acid ratio is HCl 30% + H2SO4 20% + HF 3%. The temperature is controlled at 70℃ by the temperature controller VIII227, the timer VI228 controls the time at 60 minutes, and the pressure gauge IV231 controls the pressure at 1MPa. After acid leaching, microwave cleaning is performed. After microwave drying at 100℃, the raw material flows into the feed inlet XIV244 through the discharge outlet XIII242. The cleaning device IV239 introduces ultrapure water through the ultrapure water interface IX233. The waste liquid is discharged through the waste liquid discharge channel IV238 to the waste liquid treatment interface IX241 for treatment. The waste gas is treated through the exhaust port and the waste gas treatment interface IX232. Step Six: Plasma Fine Purification: Further fine purification is carried out using the vacuum microwave plasma purification furnace of the present invention, that is, in a high vacuum device filled with hydrogen mixed gas plasma, residual micro-nano-scale inclusions and lattice impurities are completely removed to obtain ultra-high purity quartz sand with a purity of 6N or higher. Input the plasma purification process parameters into the system intelligent control center 2: vacuum degree 10. -2 ~10 -4 Pa gas, temperature 600~1500℃, time 10~180min, mixed gas flow rate 10~150sccm, Ar flow rate above 6N 10~125sccm, H2 flow rate above 6N 10~120sccm; environment: Class 100 cleanliness, plasma excitation frequency 2.45GHz. The raw material is controlled by the controller XIV245 to enter the vacuum microwave plasma purification furnace 243 through the feed port XIV244 (return port). The fixed rotation device Ⅲ248 and the fixed rotation device Ⅳ260 are turned on, and the sealing device Ⅲ250 and the sealing device Ⅳ259 are kept in good condition. The vacuum is evacuated to 10 through the vacuum interface Ⅲ247. -2 Pa ensures that the raw material enters the reaction chamber Ⅲ252 through the feed inner pipe Ⅱ251, and the temperature is controlled at 1000℃ by the temperature controller IX261. The flow rate of the mixed gas is controlled at 80sccm through the inert gas and flow meter interface Ⅲ262 and the reaction gas and flow meter interface Ⅲ263. After purification for 60 minutes, the raw material flows into the feed inlet XV266 through the discharge port XIV264. Step 7: Quality control and product collection and processing: Finally, after vacuum cooling and quality testing, qualified products are vacuum-packed, sealed, and stored for sale. This product meets the stringent requirements of high-end fields such as semiconductors for ultra-high purity quartz sand. Input the following process parameters for quality control and product collection and processing at the system's intelligent control center 2: vacuum degree 0.1 Pa, cooling medium: argon gas above 6 N, argon gas flow rate 5-100 cm³ / h 3 / min, cooling rate 20~50℃ / min: cooling to room temperature 0~25℃, cooling environment: Class 100 cleanliness, relative humidity not exceeding 40%, product quality control: purity above 6N, impurity content below 0.1ppm, particle size and particle size distribution are formulated according to product application requirements; Controller XV267 controls the raw material to enter the cooling chamber 274 through the feed inlet XV266 and the feed inner pipe Ⅲ273. Fixed rotation devices V270 and VI277 are activated to ensure the sealing devices V272 and VI276 are intact. A vacuum of 0.1 Pa is drawn through vacuum interface Ⅳ279. The cooling temperature is controlled by temperature controller X268, maintaining a cooling rate of 20℃ / min. The flow rate of high-purity argon gas (above 5N) is controlled at 30 cm³ through inert gas and flow meter interface Ⅳ269. 3 The product is cooled to room temperature of 20-25℃ at a speed of 0.5 min. Products that pass the quality inspection enter the vacuum packaging machine 282 through the discharge port XV280. The vacuum is drawn to a vacuum degree of 0.1 Pa through the vacuum interface V281. The product vacuum packaging barrel 287 is connected to the product vacuum packaging interface 283 for vacuum packaging and then sealed and stored. The exhaust gas is treated through the exhaust port and exhaust gas treatment interface XI278.
[0028] Steps one through four are completed in a Class 1000 cleanroom environment, while steps six and seven are completed in a Class 100 cleanroom environment. All water used in steps one through six is ultrapure water with a resistivity ≥18.2 MΩ·cm. The exhaust gases generated during the processes of steps one through seven are treated to meet emission standards before being discharged. The wastewater generated is treated to meet emission standards before being discharged or returned to the water treatment system. All waste generated is treated to meet emission standards using a microwave plasma incinerator before being discharged.
[0029] Example 3: A smart manufacturing process for ultra-high purity quartz sand for semiconductors includes the following four stages and seven steps: the first stage is material preparation, including step one; the second stage is high-purity quartz purification, including steps two to five; the third stage is ultra-high purity quartz purification, including step six; and the fourth stage is quality control and product collection and processing, including step seven. The apparatus of Example 1 is used, and the specific steps are as follows: Step 1: Raw material preparation: This includes raw ore beneficiation, raw ore storage, raw ore washing, crushing and grading, color sorting, chlorination calcination, acid leaching, and ball milling and grading to obtain qualified raw materials with a particle size of 0.1-0.3 mm, a purity of 4N or higher, and controllable impurities. Start the system intelligent control center 2 and input the material preparation process parameters: Select high-purity quartz ore quality: SiO2 mass fraction higher than 3N, total impurities <100μg / g; Preferred quality meets the reference standard: total impurity element (μg / g) <50, including Al <30, Ti <10, Na <8, K <8, Li <5, Ca <5, Fe <3, P <2 and B <1, and trace amounts of radioactive elements and gas-liquid inclusions; Reserve process parameters: ore reserve quantity: 72 hours continuous... Continued production ore consumption; Soaking process parameters: raw ore soaking agent 8%~12%H2C2O4+1%~10%HF, soaking time 4~24 hours, rinsing water pressure 1~10MPa; Crushing and grading process parameters: coarse crushing particle size 10~30mm, medium crushing particle size 5~10mm, fine crushing particle size 1~5mm; Color sorting process parameters: color sorting particle size range 0.08~5mm, color threshold: a narrow range close to white, spraying intensity: air valve pressure 0.4~0.6MPa; Chlorine Calcination process parameters: vacuum degree 0.1~0.01Pa, temperature 600~1200℃, time 1~4h, mixed gas flow rate 10~100sccm, Ar flow rate (above 5N) 10~100sccm, HCl gas flow rate (above 5N) 10~100sccm; Microwave acid leaching process parameters: gradient acid leaching is achieved by sequentially using acid leaching agents 1~3: acid leaching agent 1: H2C2O4 8~12%, acid leaching agent 2: acid ratio HF 3~10% + H2C2O4 10%. ~12%, acid leaching agent 3: acid ratio HF3~10% + H2C2O48~12% + H2SiF6, liquid-solid ratio 2:1~4:1, acid leaching pressure 0.5~1MPa, acid leaching temperature 60~120℃, acid leaching time 30~240min, ultrapure water microwave cleaning, ultrapure water quality: resistivity ≥18.2MΩ·cm, ball milling classification process parameters: ball milling feed particle size 1~5mm, ball milling time 1~6h, cyclone classification discharge particle size 0.1~0.3mm; Selected high-purity quartz ore is fed into conveyor belt I12 via ore inlet 11 by controller I9 and first transported to intelligent ore bin 10. After the ore storage is completed, it is directly transported to feed inlet I13 and metered into ore mobile lifting tank washing machine 15 at a liquid-solid ratio of 3:1. At the same time, 10% H2C2O4 + 4% HF ore soaking agent is introduced through reagent preparation system 295. After soaking for 6 hours, the rotating high-pressure rinsing water cover 16 connected to ultrapure water interface I14 is opened for repeated rinsing. Waste liquid is discharged through waste liquid treatment interface I17 and connected to waste liquid treatment system 297 for treatment to meet standards before being discharged or returned to the water treatment system for water production. The washed quartz ore flows into conveyor belt II19 through discharge outlet I18 and is transported to feed inlet II27 via the first sub-belt. Controller II20 controls the raw material to enter the raw ore crushing and grading integrated machine 21 through feed inlet II27. The raw material is crushed and graded step by step by coarse crusher 26, medium crusher 25 and fine crusher 24 to obtain raw materials with a coarse crushing particle size of 20mm, a medium crushing particle size of 6mm and a fine crushing particle size of 2mm respectively. The waste gas generated during the crushing and grading process is treated by exhaust port and waste gas treatment interface I28. The raw material that fails the crushing and grading process flows into the first and second sub-belts of conveyor belt II19 through return hopper 23 and is transported to feed inlet II27 for repeated crushing and grading until it is qualified. The qualified raw material flows into the third sub-belt of conveyor belt II19 through discharge port II22 and is transported to feed inlet III31. Controller Ⅲ30 controls 2mm raw materials to enter the color sorter 29 through feed inlet Ⅲ31 and flow into the vibrating feeder 32. The vibrator 32 makes the raw materials flow evenly along the chute 34 into the sorting area composed of light source 35, sensor 36 and signal processor 33, forming a single layer and continuous raw material flow to ensure that each raw material is accurately detected. Light source 35 illuminates the raw materials, sensor 36 receives the light signal reflected or transmitted by the raw materials and converts it into an electrical signal (material color and optical characteristics), which is analyzed and processed by signal processor 33. The compressed air 37 and spray valve 38 are separately executed to control the air pressure of the air valve to 0.8MPa to remove unqualified raw materials into impurity box 40 and send them to waste solid treatment system 298 for processing. Qualified raw materials flow into feed inlet Ⅳ42 through discharge outlet Ⅲ39. Controller IV43 controls process parameters to allow raw materials to enter the vacuum microwave roasting furnace 44 for chlorination calcination. Vacuum is drawn to a vacuum level of 0.1 Pa through vacuum interface I45. Temperature controller I4 controls the temperature at 1100℃. The flow rate of the reaction mixture is controlled at 70 cm³ / s according to the mixed gas volume ratio of HCl 90% + Ar 10% through reaction gas and flow meter interfaces I54 and I55. 3 / min, after chlorination and calcination for 1.5h, it falls directly into the gradient acid leaching tank I71 through the feed inlet V57 for acid leaching; The controller V58 controls the raw materials to enter the gradient acid leaching tank I71 through the feed inlet V57 at a liquid-to-solid ratio of 3:1, and introduces the acid leaching agent through the auxiliary material inlet I61. In the first layer of the gradient acid leaching tank I71, acid leaching agent 1: H2C2O4 10% is introduced; in the second layer, acid leaching agent 2: acid ratio HF 4% + H2C2O4 10% is introduced; and in the third layer, acid leaching agent 3: acid ratio HF 4% + H2C2O4 10% + H2SiF6 is introduced. Ultrapure water is introduced into the lower layer through the ultrapure water interface II65. The pressure is controlled at 0.8MPa by the pressure gauge I63, the temperature is controlled at 80℃ by the temperature controller II60, and the timer I59 controls the time at 50 minutes. After the acid leaching is completed layer by layer, it automatically flows into the next layer. After microwave cleaning in the lower layer, it flows into the feed inlet VI75 through the discharge outlet V74. The waste liquid of each layer is discharged through the waste liquid discharge channel I70 to the waste liquid treatment interface II73 for treatment. The waste gas is treated through the exhaust port and the waste gas treatment interface III64. The raw material is controlled by the controller VI77 to enter the ball mill 80 through the feed port VI75. The feed particle size is 2mm. Zirconium balls of different diameters are introduced into the ball milling media 82 according to the product particle size distribution. After ball milling for 5 hours, the raw material enters the cyclone chamber 91 through the discharge port VI87. The raw material with unqualified particle size enters the underflow trough 88 and flows into the return port 76 from the underflow port 89. It then enters the ball mill 80 for repeated grinding until it is qualified. The raw material with a particle size of 0.2mm swirls to the overflow port 93 and flows into the feed pipe II 97. Step 2: High gradient magnetic separation: A vertical ring pulsating high gradient wet magnetic separator is preferred to remove magnetic impurities; Input the high gradient magnetic separation process parameters into the system intelligent control center 2: 1.5~2.0T background magnetic field, slurry concentration 25%~30%, pulse frequency 200~300 times / min, feed particle size controlled at -0.074mm with a proportion ≥80%, and washing water volume controlled at 1~2m³ / t ore to ensure timely discharge of magnetic products and avoid secondary adsorption; The controller VII113 selects a 1.8T background magnetic field, a slurry concentration of 27.5%, and a pulse frequency of 260 times / min. The raw material in feed pipe II97 flows through inlet VII101 along the upper yoke 100 and through rotating ring 102. Magnetic particles are adsorbed by the magnetic medium 103 and carried by rotating ring 102 to the bottom non-magnetic field zone. The flushing water volume is controlled at 1.5m³. 3 / t of ore is rinsed with flushing water pipe 105 and finally enters magnetic impurity box 108. The magnetic media can be prevented from being blocked by backflushing magnetic impurities and material pulsation. The pulsation separation efficiency is high. The raw material passes through the magnetic media pile under the action of gravity and pulsating fluid force, and is separated from magnetic particle impurities. It enters material pipe Ⅲ115 from discharge port VII112. Step 3: Ultrasonic flotation: The prepared slurry is subjected to two ultrasonic flotations and ultrasonic cleaning to remove gangue mineral impurities using the ultrasonic temperature-controlled flotation machine of this invention. Input the slurry conditioning and ultrasonic flotation process parameters in the system's intelligent control center 2: Primary slurry conditioning and ultrasonic flotation process parameters: Combined reagent system: oleic acid + dodecylamine + pH 2.5~3.5, microbubble flotation column (bubble diameter ≤50μm), impeller speed 100~300rpm, aeration rate 0.2~0.5m 3 / (m²·min), pulp concentration 20%~40%, ultrasonic frequency 20~40kHz, flotation temperature 30~50℃, flotation time 20~60min, ultrasonic cleaning with ultrapure water, ultrapure water quality: resistivity ≥18.2MΩ·cm; secondary pulp conditioning and ultrasonic flotation process parameters: for different mineral impurities, optimize the primary flotation reagent system, intelligently adjust the reagent dosage, adjust the pH value, ultrasonic flotation, ultrasonic cleaning with ultrapure water, effectively remove various gangue mineral impurities; The raw material is controlled by the controller VIII123 to enter the slurry tank I119 through the feed pipe III115 via the inlet I116 of the slurry tank. The flotation agent (oleic acid + dodecylamine + pH3.0 + ultrapure water) is added from the reagent and ultrapure water addition tank I117. The slurry is fully stirred and adjusted by the stirring device I120 to control the slurry concentration at 27.5%. The slurry enters the feed pipe IV121 through the outlet I118 of the slurry tank. The raw material is controlled by controller VIII123 to enter flotation cell I127 through feed inlet VIII124 via feed pipe IV121. Timer II125 sets the time to 50 minutes, and temperature controller III126 sets the temperature to 40℃. Motor I132 is started, and stator I135 and impeller I136 rotate at high speed, generating strong eddies and a negative pressure zone within the cell. This negative pressure forces air through air pipe I134 at a rate of 0.4 m³ / min. 3 / (m²·min), the slurry is strongly drawn in from the hollow shaft I33. The impeller I136 disperses the small bubbles of the drawn-in air and makes them evenly dispersed in the entire slurry. The ultrasonic device I138 is turned on to accelerate the stirring and ensure that the mineral impurities are in a suspended state. Under the action of the collector, the surface of the mineral impurities becomes hydrophobic, increasing the probability of collision between impurity particles and bubbles, and they adhere to the bubbles, float up, and form a bubble layer. The foam is scraped off by the scraper device I131 and sent to the collection tank I128. After the flotation is completed, ultrapure water is introduced through the ultrapure water interface V137 for ultrasonic cleaning and then enters the feed pipe V140 through the discharge port VIII139. The waste liquid is treated through the waste liquid treatment interface V122, and the waste gas from the gas collection hood I130 is treated through the exhaust port and the waste gas treatment interface IV129. The controller IX148 controls the raw material from the feed pipe V140 to enter the slurry tank II144 through the inlet II141. The optimized flotation agent is added from the reagent and ultrapure water addition tank II142. The slurry is fully stirred and sized by the stirring device II145 to control the slurry concentration at 27.5%. The slurry then enters through the outlet II143 of the slurry tank. The raw material is controlled by the controller IX148 to enter the flotation cell II152 through the feed inlet IX149 via the feed pipe VI146. The timer Ⅲ150 sets the time to 50 minutes, and the temperature controller Ⅳ151 sets the temperature to 40℃. The motor II157 is started, and the stator II160 and impeller II161 rotate at high speed, generating strong eddies and a negative pressure zone in the cell. The negative pressure forces air into the air pipe II159 at a rate of 0.4 m³ / min. 3 / (m²·min) The slurry is strongly drawn in from the hollow shaft II158. The impeller II161 disperses the small bubbles of the drawn-in air and makes them evenly dispersed in the entire slurry. The ultrasonic device II163 is turned on to accelerate the stirring and ensure that the mineral impurities are in a suspended state. Under the action of the collector, the surface of the mineral impurities becomes hydrophobic, increasing the probability of collision between impurity particles and bubbles. They adhere to the bubbles, float up, and form a bubble layer. The foam is scraped off by the scraper device II156 and sent to the collection tank II153. After the flotation is completed, ultrapure water is introduced through the ultrapure water interface VI162 for ultrasonic cleaning and then enters the feed pipe VII165 through the discharge port IX164. The waste liquid is treated through the waste liquid treatment interface VI147. The waste gas from the gas collection hood II155 is treated through the exhaust port and the waste gas treatment interface V154. Step 4: Microwave acid leaching: Microwave acid leaching, microwave cleaning, and microwave drying are performed using the microwave multifunctional reactor of this invention to remove impurities from the inclusions. Input the microwave acid leaching process parameters in the system intelligent control center 2: acid ratio of leaching agent: HCl 20~30% + H2SO4 10~20% + HF 3~5%, liquid-solid ratio 2:1~4:1, acid leaching pressure 0.5~1MPa, acid leaching temperature 60~120℃, acid leaching time 30~240min, microwave cleaning with ultrapure water, ultrapure water quality: resistivity ≥18.2MΩ·cm, microwave drying temperature 100~120℃; The controller X171 controls the raw material through the feed pipe VII165 to enter the multi-functional rotary pickling tank Ⅰ181 through the feed inlet X170 at a liquid-to-solid ratio of 3:1. The pickling agent HCl 25% + H2SO4 15% + HF 4% is introduced through the auxiliary material inlet Ⅱ167. The temperature is controlled at 80℃ by the temperature controller V168, the timer Ⅳ169 controls the time at 50 minutes, and the pressure gauge Ⅱ172 controls the pressure at 0.8MPa. After pickling, microwave cleaning is performed, and microwave drying is carried out at 100℃. After drying, the raw material flows into the feed inlet XI185 through the discharge outlet X183. The cleaning device Ⅱ180 introduces ultrapure water through the ultrapure water interface VII174. The waste liquid is discharged through the waste liquid discharge channel Ⅱ179 to the waste liquid treatment interface VII182 for treatment. The waste gas is treated through the exhaust port and the waste gas treatment interface VI173. Step 5: Vacuum chlorination combined with hot pressing acid leaching for fine purification: Using the vacuum microwave purification furnace of this invention in conjunction with a microwave reactor, first remove lattice impurities by vacuum microwave treatment, then directly remove burst micro-nano-scale inclusions by microwave acid leaching, followed by microwave cleaning and microwave drying to obtain high-purity quartz sand with a purity of 5N or higher. Input the chlorination process parameters into the system's intelligent control center 2: vacuum degree 0.1~0.01Pa, temperature 600~1200℃, time 30~240min, mixed gas flow rate 10~100sccm, Ar gas flow rate (above 5N) 10~100sccm, HCl gas flow rate (above 5N) 10~100sccm, environment: Class 100 cleanliness; microwave acid leaching process parameters: primary acid leaching: sequentially using acid leaching agents 1~3 to achieve gradient acid leaching: acid leaching agent 1: H2C2O 48~12%, Acid leaching agent 2: acid ratio HF 3~10% + H2C2O4 10~12%; acid leaching agent 3: acid ratio HF 3~10% + H2C2O4 8~12% + H2SiF6; secondary acid leaching: liquid-solid ratio 2:1~4:1; acid leaching pressure 0.5~1MPa; acid leaching temperature 60~120℃; acid leaching time 30~240min; microwave cleaning with ultrapure water; ultrapure water quality: resistivity ≥18.2MΩ·cm; microwave drying temperature 100~120℃; total impurities less than 8ppm. The raw materials are controlled to enter the reaction chamber II193 through the feed inlet XI185 via the controller XI186. The rotating device is started, and a vacuum is drawn to 0.01 Pa through the vacuum interface II188. The temperature is controlled at 1100℃ by the temperature controller VI202. The flow rate of the mixed gas is controlled at 60 cm³ through the inert gas and flow meter interface II203 and the reaction gas and flow meter interface II204. 3 / min, after chlorination for 50min, the waste gas enters the feed port XII206 through the discharge port XI205, and the waste gas passes through the exhaust port and waste gas treatment interface VII187; Controller XII207 controls the raw materials to enter the gradient pickling tank II220 through inlet XII206 at a liquid-to-solid ratio of 3:1, and introduces the pickling agent through auxiliary material inlet III210. In the first layer of gradient pickling tank II220, pickling agent 1 (H₂C₂O₄ 10%) is introduced, and in the second layer, pickling agent 2 (HF 4%+) is introduced. H2C2O4 10%, third layer introduces acid leaching agent 3: acid ratio HF 4% + H2C2O4 10% + H2SiF6, the lower layer introduces ultrapure water from ultrapure water interface VIII213, pressure gauge II211 controls the pressure to 1MPa, timer V208 controls the time to 50min / layer, temperature controller VII209 controls the temperature to 80℃, after acid leaching is completed, it automatically flows into the next layer, after microwave cleaning in the lower layer, it flows into the material pipe VIII224 through the discharge port XII223, the waste liquid is discharged to the waste liquid treatment interface VIII222 through the waste liquid discharge channel III219 for treatment, and the waste gas is treated through the exhaust port and the waste gas treatment interface VIII212; The controller XIII230 controls the raw material through feed pipe VIII224 to enter the multi-functional rotary pickling tank II240 through feed inlet XIII229 at a liquid-to-solid ratio of 3:1. The pickling agent is introduced through auxiliary material inlet IV226. The acid ratio is HCl 25% + H2SO4 15% + HF 4%. The temperature is controlled at 80℃ by temperature controller VIII227, the timer is controlled at 50 minutes by timer VI228, and the pressure is controlled at 0.8MPa by pressure gauge IV231. After pickling, microwave cleaning is performed. After microwave drying at 100℃, the material flows into feed inlet XIV244 through discharge port XIII242. Ultrapure water is introduced through ultrapure water interface IX233 by cleaning device IV239. Waste liquid is discharged through waste liquid discharge channel IV238 to waste liquid treatment interface IX241 for treatment. Waste gas is treated through exhaust port and waste gas treatment interface IX232. Step Six: Plasma Fine Purification: Further fine purification is carried out using the vacuum microwave plasma purification furnace of the present invention, that is, in a high vacuum device filled with hydrogen mixed gas plasma, residual micro-nano-scale inclusions and lattice impurities are completely removed to obtain ultra-high purity quartz sand with a purity of 6N or higher. Input the plasma purification process parameters into the system intelligent control center 2: vacuum degree 10. -2 ~10 -4 Pa gas, temperature 600~1500℃, time 10~180min, mixed gas flow rate 10~150sccm, Ar flow rate above 6N 10~125sccm, H2 flow rate above 6N 10~120sccm; environment: Class 100 cleanliness, plasma excitation frequency 2.45GHz. The raw material is controlled by the controller XIV245 to enter the vacuum microwave plasma purification furnace 243 through the feed port XIV244 (return port). The fixed rotation device Ⅲ248 and the fixed rotation device Ⅳ260 are turned on, and the sealing device Ⅲ250 and the sealing device Ⅳ259 are kept in good condition. The vacuum is evacuated to 10 through the vacuum interface Ⅲ247. -3 Pa ensures that the raw material enters the reaction chamber Ⅲ252 through the feed inner pipe Ⅱ251, and the temperature is controlled at 1100℃ by the temperature controller IX261. The flow rate of the mixed gas is controlled at 70sccm through the inert gas and flow meter interface Ⅲ262 and the reaction gas and flow meter interface Ⅲ263. After purification for 50 minutes, the raw material flows into the feed inlet XV266 through the outlet XIV264. Step 7: Quality control and product collection and processing: Finally, after vacuum cooling and quality testing, qualified products are vacuum-packed, sealed, and stored for sale. This product meets the stringent requirements of high-end fields such as semiconductors for ultra-high purity quartz sand. Input the following process parameters for quality control and product collection and processing at the system's intelligent control center 2: vacuum degree 0.1 Pa, cooling medium: argon gas above 6 N, argon gas flow rate 5-100 cm³ / h 3 / min, cooling rate 20~50℃ / min: cooling to room temperature 0~25℃, cooling environment: Class 100 cleanliness, relative humidity not exceeding 40%, product quality control: purity above 6N, impurity content below 0.1ppm, particle size and particle size distribution are formulated according to product application requirements; The controller XV267 controls the raw material to enter the cooling chamber 274 through the feed inlet XV266 and the feed inner pipe Ⅲ273. The fixed rotation device V270 and fixed rotation device VI277 are turned on to ensure that the sealing device V272 and sealing device VI276 are sealed properly. The vacuum is drawn to 0.1Pa through the vacuum interface Ⅳ279. The cooling temperature is controlled by the temperature controller X268 to maintain the cooling rate at 25℃ / min. The flow rate of high-purity argon gas above 5N is controlled at 40cm3 / min through the inert gas and flow meter interface Ⅳ269. The product is cooled to room temperature of 20~25℃. After quality inspection, qualified products enter the vacuum packaging machine 282 through the discharge port XV280. The vacuum is drawn to 0.1Pa through the vacuum interface V281. The product vacuum packaging barrel 287 is connected to the product vacuum packaging interface 283 for vacuum packaging and sealing and storage. The exhaust gas is treated through the exhaust port and exhaust gas treatment interface XI278.
[0030] Steps one through four are completed in a Class 1000 cleanroom environment, while steps six and seven are completed in a Class 100 cleanroom environment. All water used in steps one through six is ultrapure water with a resistivity ≥18.2 MΩ·cm. The exhaust gases generated during the processes of steps one through seven are treated to meet emission standards before being discharged. The wastewater generated is treated to meet emission standards before being discharged or returned to the water treatment system. All waste generated is treated to meet emission standards using a microwave plasma incinerator before being discharged.
[0031] Example 4: A smart manufacturing process for ultra-high purity quartz sand for semiconductors includes the following four stages and seven steps: the first stage is material preparation, including step one; the second stage is high-purity quartz purification, including steps two to five; the third stage is ultra-high purity quartz purification, including step six; and the fourth stage is quality control and product collection and processing, including step seven. The apparatus of Example 1 is used, and the specific steps are as follows: Step 1: Raw material preparation: This includes raw ore beneficiation, raw ore storage, raw ore washing, crushing and grading, color sorting, chlorination calcination, acid leaching, and ball milling and grading to obtain qualified raw materials with a particle size of 0.1-0.3 mm, a purity of 4N or higher, and controllable impurities. Start the intelligent control center 2 of the system and input the material preparation process parameters: Select high-purity quartz ore quality: SiO2 mass fraction higher than 3N, total impurities <100μg / g; Preferred quality meets the reference standard: total impurity elements (μg / g) <50, including Al <30, Ti <10, Na <8, K <8, Li <5, Ca <5, Fe <3, P <2 and B <1, and trace amounts of radioactive elements and gas-liquid inclusions; Reserve process parameters: ore reserve amount: ore amount for 72 hours of continuous production; Soaking and washing process parameters: ore soaking agent 8%~12%H2C2O4+1%~10%HF, soaking time 4~24 hours, rinsing water pressure 1~10MPa; Crushing and grading process parameters: coarse crushing particle size... 10-30mm, medium crushing particle size 5-10mm, fine crushing particle size 1-5mm; Color sorting process parameters: color sorting particle size range 0.08-5mm, color threshold: a narrow range close to white, spray intensity: gas valve pressure 0.4-0.6MPa; Chlorination calcination process parameters: vacuum degree 0.1-0.01Pa, temperature 600-1200℃, time 1-4h, mixed gas flow rate 10-100sccm, Ar flow rate above 5N 10-100sccm, HCl gas flow rate above 5N 10-100sccm; Microwave acid leaching process parameters: gradient acid leaching is achieved by sequentially using acid leaching agents 1-3: acid leaching agent 1: H2C2O 48-12%, acid leaching agent 2: acid ratio HF 3-10%+ H2C2O4 10~12%, acid leaching agent 3: acid ratio HF 3~10% + H2C2O4 8~12% + H2SiF6, liquid-solid ratio 2:1~4:1, acid leaching pressure 0.5~1MPa, acid leaching temperature 60~120℃, acid leaching time 30~240min, ultrapure water microwave cleaning, ultrapure water quality: resistivity ≥18.2MΩ·cm, ball milling classification process parameters: ball milling feed particle size 1~5mm, ball milling time 1~6h, cyclone classification discharge particle size 0.1~0.3mm; Selected high-purity quartz ore is fed into conveyor belt I12 via controller I9 through ore inlet 11 and first transported to intelligent ore bin 10. After the ore storage is completed, it is directly transported to feed inlet I13 and metered into ore mobile lifting tank washing machine 15 at a liquid-solid ratio of 4:1. At the same time, 12% H2C2O4 + 5% HF ore soaking agent is introduced through reagent preparation system 295. After soaking for 4 hours, the rotating high-pressure rinsing water cover 16 connected to ultrapure water interface I14 is opened for repeated rinsing. Waste liquid is discharged through waste liquid treatment interface I17 and connected to waste liquid treatment system 297 for treatment to meet standards before being discharged or returned to the water treatment system for water production. The washed quartz ore flows into conveyor belt II19 through discharge outlet I18 and is transported to feed inlet II27 via the first sub-belt. Controller II20 controls the raw material to enter the raw ore crushing and grading integrated machine 21 through feed inlet II27. The raw material is crushed and graded step by step by coarse crusher 26, medium crusher 25 and fine crusher 24 to obtain raw materials with a coarse crushing particle size of 30mm, a medium crushing particle size of 10mm and a fine crushing particle size of 3mm respectively. The waste gas generated during the crushing and grading process is treated by exhaust port and waste gas treatment interface I28. The raw material that fails the crushing and grading process flows into the first and second sub-belts of conveyor belt II19 through return hopper 23 and is transported to feed inlet II27 for repeated crushing and grading until it is qualified. The qualified raw material flows into the third sub-belt of conveyor belt II19 through discharge port II22 and is transported to feed inlet III31. Controller Ⅲ30 controls 3mm raw materials to enter the color sorter 29 through feed inlet Ⅲ31 and flow into the vibrating feeder 32. The vibrator 32 makes the raw materials flow evenly along the chute 34 into the sorting area composed of light source 35, sensor 36 and signal processor 33, forming a single layer and continuous raw material flow to ensure that each raw material is accurately detected. Light source 35 illuminates the raw materials, sensor 36 receives the light signal reflected or transmitted by the raw materials and converts it into an electrical signal (material color and optical characteristics), which is analyzed and processed by signal processor 33. The compressed air 37 and spray valve 38 are separately executed to control the air pressure of the air valve to 1MPa to remove unqualified raw materials into impurity box 40 and send them to waste solid treatment system 298 for processing. Qualified raw materials flow into feed inlet Ⅳ42 through discharge outlet Ⅲ39. Controller IV43 controls process parameters to guide the raw materials into the vacuum microwave roasting furnace 44 for chlorination calcination. Vacuum is drawn to a vacuum level of 0.1 Pa through vacuum interface I45. Temperature controller I4 controls the temperature at 1200℃. The flow rate of the reaction mixture is controlled at 80 cm³ / s according to the mixed gas volume ratio of HCl 90% + Ar 10% through reaction gas and flow meter interfaces I54 and I55. 3 / min, after chlorination and calcination for 1 hour, the feed is directly fed into the gradient acid leaching tank I71 through the feed inlet V57 for acid leaching; The controller V58 controls the raw materials to enter the gradient pickling tank I71 through the feed inlet V57 at a liquid-to-solid ratio of 4:1, and introduces the pickling agent through the auxiliary material inlet I61. In the first layer of the gradient pickling tank I71, pickling agent 1: H2C2O4 12% is introduced; in the second layer, pickling agent 2: acid ratio HF 5% + H2C2O4 12% is introduced; and in the third layer, pickling agent 3: acid ratio HF 5% + H2C2O4 12% + H2SiF6 is introduced. Ultrapure water is introduced into the lower layer through the ultrapure water interface II65. The pressure is controlled at 0.6MPa by the pressure gauge I63, the temperature is controlled at 90℃ by the temperature controller II60, and the timer I59 controls the time at 40 minutes. After pickling is completed layer by layer, the raw materials automatically flow into the next layer. After microwave cleaning in the lower layer, the raw materials flow into the feed inlet VI75 through the discharge outlet V74. The waste liquid of each layer is discharged through the waste liquid discharge channel I70 to the waste liquid treatment interface II73 for treatment. The waste gas is treated through the exhaust port and the waste gas treatment interface III64. The raw material is controlled by the controller VI77 to enter the ball mill 80 through the feed port VI75. The feed particle size is 3mm. Zirconium balls of different diameters are introduced into the ball milling media 82 according to the product particle size distribution. After ball milling for 4 hours, the raw material enters the cyclone chamber 91 through the discharge port VI87. The raw material with unqualified particle size enters the underflow trough 88 and flows into the return port 76 from the underflow port 89. It then enters the ball mill 80 for repeated grinding until it is qualified. The raw material with a particle size of 0.3mm swirls to the overflow port 93 and flows into the feed pipe II 97. Step 2: High gradient magnetic separation: A vertical ring pulsating high gradient wet magnetic separator is preferred to remove magnetic impurities; Input the high-gradient magnetic separation process parameters into the system's intelligent control center 2: 1.5–2.0T background magnetic field, slurry concentration 25%–30%, pulse frequency 200–300 times / min, feed particle size controlled at -0.074mm with a percentage ≥80%, and washing water volume controlled at 1–2 m³ / min. 3 / t of ore, ensuring timely discharge of magnetic products and avoiding secondary adsorption; The controller VII113 selects a 2.0T background magnetic field, a slurry concentration of 25%, and a pulse frequency of 280 times / min. The raw material from feed pipe II97 flows through inlet VII101 along the upper yoke 100 and through rotating ring 102. Magnetic particles are adsorbed by the magnetic medium 103 and carried by rotating ring 102 to the bottom non-magnetic field zone. The flushing water volume is controlled at 1m³. 3 / t of ore is rinsed with flushing water pipe 105 and finally enters magnetic impurity box 108. The magnetic media can be prevented from being blocked by backflushing magnetic impurities and material pulsation. The pulsation separation efficiency is high. The raw material passes through the magnetic media pile under the action of gravity and pulsating fluid force, and is separated from magnetic particle impurities. It enters material pipe Ⅲ115 from discharge port VII112. Step 3: Ultrasonic flotation: The prepared slurry is subjected to two ultrasonic flotations and ultrasonic cleaning to remove gangue mineral impurities using the ultrasonic temperature-controlled flotation machine of this invention. Input the pulp conditioning and ultrasonic flotation process parameters in the system's intelligent control center 2: Primary pulp conditioning and ultrasonic flotation process parameters: Use a combined reagent system (oleic acid + dodecylamine + 2.5~pH 3.5) and a microbubble flotation column (bubble diameter ≤50μm) to remove silicate mineral impurities such as feldspar and mica; impeller speed 100~300rpm; aeration rate 0.2~0.5m³. 3 / (m²·min), pulp concentration 20%~40%, ultrasonic frequency 20~40kHz, flotation temperature 30~50℃, flotation time 20~60min, ultrasonic cleaning with ultrapure water, ultrapure water quality: resistivity ≥18.2MΩ·cm; secondary pulp conditioning and ultrasonic flotation process parameters: for different mineral impurities, optimize the primary flotation reagent system, intelligently adjust the reagent dosage, adjust the pH value, ultrasonic flotation, and ultrasonic cleaning with ultrapure water to effectively remove various gangue mineral impurities; The raw material is controlled by the controller VIII123 to enter the slurry tank I119 through the inlet I116 of the slurry tank via the feed pipe III115. The flotation agent (oleic acid + dodecylamine + pH3.5 + ultrapure water) is added from the reagent and ultrapure water addition tank I117. The slurry is fully stirred and adjusted by the stirring device I120 to control the slurry concentration at 25%. The slurry enters the feed pipe IV121 through the outlet I118 of the slurry tank. The raw material is controlled by controller VIII123 to enter flotation cell I127 through feed inlet VIII124 via feed pipe IV121. Timer II125 sets the time to 40 minutes, and temperature controller III126 sets the temperature to 45℃. Motor I132 is started, and stator I135 and impeller I136 rotate at high speed, generating strong eddies and a negative pressure zone within the cell. This negative pressure forces air through air pipe I134 at a rate of 0.3 m³ / min. 3 / (m²·min), the slurry is strongly drawn in from the hollow shaft I33. The impeller I136 disperses the small bubbles of the drawn-in air and makes them evenly dispersed in the entire slurry. The ultrasonic device I138 is turned on to accelerate the stirring and ensure that the mineral impurities are in a suspended state. Under the action of the collector, the surface of the mineral impurities becomes hydrophobic, increasing the probability of collision between impurity particles and bubbles, and they adhere to the bubbles, float up, and form a bubble layer. The foam is scraped off by the scraper device I131 and sent to the collection tank I128. After the flotation is completed, ultrapure water is introduced through the ultrapure water interface V137 for ultrasonic cleaning and then enters the feed pipe V140 through the discharge port VIII139. The waste liquid is treated through the waste liquid treatment interface V122, and the waste gas from the gas collection hood I130 is treated through the exhaust port and the waste gas treatment interface IV129. Controller IX148 controls the raw material in feed pipe V140 to enter the slurry tank II144 through the inlet II141 of the slurry tank. Optimized flotation agent is added from the reagent and ultrapure water addition tank II142. The slurry is fully stirred and adjusted by the stirring device II145 to control the slurry concentration at 25%. The slurry enters VI146 through the outlet II143 of the slurry tank. The raw material is controlled by the controller IX148 to enter the flotation cell II152 through the feed inlet IX149 via the feed pipe VI146. The timer Ⅲ150 sets the time to 40 minutes, and the temperature controller Ⅳ151 sets the temperature to 45℃. The motor II157 is started, and the stator II160 and impeller II161 rotate at high speed, generating strong eddies and a negative pressure zone in the cell. The negative pressure forces air into the air pipe II159 at a rate of 0.3m³. 3 / (m²·min) The slurry is strongly drawn in from the hollow shaft II158. The impeller II161 disperses the small bubbles of the drawn-in air and makes them evenly dispersed in the entire slurry. The ultrasonic device II163 is turned on to accelerate the stirring and ensure that the mineral impurities are in a suspended state. Under the action of the collector, the surface of the mineral impurities becomes hydrophobic, increasing the probability of collision between impurity particles and bubbles. They adhere to the bubbles, float up, and form a bubble layer. The foam is scraped off by the scraper device II156 and sent to the collection tank II153. After the flotation is completed, ultrapure water is introduced through the ultrapure water interface VI162 for ultrasonic cleaning and then enters the feed pipe VII165 through the discharge port IX164. The waste liquid is treated through the waste liquid treatment interface VI147. The waste gas from the gas collection hood II155 is treated through the exhaust port and the waste gas treatment interface V154. Step 4: Microwave acid leaching: Microwave acid leaching, microwave cleaning, and microwave drying are performed using the microwave multifunctional reactor of this invention to remove impurities from the inclusions. Input the microwave acid leaching process parameters in the system intelligent control center 2: acid ratio of leaching agent: HCl 20~30% + H2SO4 10~20% + HF 3~5%, liquid-solid ratio 2:1~4:1, acid leaching pressure 0.5~1MPa, acid leaching temperature 60~120℃, acid leaching time 30~240min, microwave cleaning with ultrapure water, ultrapure water quality: resistivity ≥18.2MΩ·cm, microwave drying temperature 100~120℃; The controller X171 controls the raw material through the feed pipe VII165 to enter the multi-functional rotary pickling tank Ⅰ181 through the feed inlet X170 at a liquid-to-solid ratio of 4:1. The pickling agent HCl20%+H2SO410%+HF5% is introduced through the auxiliary material inlet Ⅱ167. The temperature is controlled at 90℃ by the temperature controller V168, the timer Ⅳ169 controls the time at 40 minutes, and the pressure gauge Ⅱ172 controls the pressure at 0.6MPa. After pickling, microwave cleaning is performed, and microwave drying is carried out at 100℃. After drying, the raw material flows into the feed inlet XI185 through the discharge outlet X183. The cleaning device Ⅱ180 introduces ultrapure water through the ultrapure water interface VII174. The waste liquid is discharged through the waste liquid discharge channel Ⅱ179 to the waste liquid treatment interface VII182 for treatment. The waste gas is treated through the exhaust port and the waste gas treatment interface VI173. Step 5: Vacuum chlorination combined with hot pressing acid leaching for fine purification: Using the vacuum microwave purification furnace of this invention in conjunction with a microwave reactor, first remove lattice impurities by vacuum microwave treatment, then directly remove burst micro-nano-scale inclusions by microwave acid leaching, followed by microwave cleaning and microwave drying to obtain high-purity quartz sand with a purity of 5N or higher. Input the chlorination process parameters into the system's intelligent control center 2: vacuum degree 0.1~0.01Pa, temperature 600~1200℃, time 30~240min, mixed gas flow rate 10~100sccm, Ar gas flow rate (above 5N) 10~100sccm, HCl gas flow rate (above 5N) 10~100sccm, environment: Class 100 cleanliness; microwave acid leaching process parameters: primary acid leaching: gradient acid leaching is achieved by sequentially using acid leaching agents 1~3: acid leaching agent 1: H2C2O 48~12%, acid leaching agent 2: acid ratio HF 3~10% + H2 C2O4 10~12%, acid leaching agent 3: acid ratio HF 3~10% + H2C2O4 8~12% + H2SiF6, secondary acid leaching: acid leaching agent acid ratio: HCl 20~30% + H2SO4 10~20% + HF 3~5%, liquid-solid ratio 2:1~4:1, acid leaching pressure 0.5~1MPa, acid leaching temperature 60~120℃, acid leaching time 30~240min, ultrapure water microwave cleaning, ultrapure water quality: resistivity ≥18.2MΩ·cm, microwave drying temperature 100~120℃, total impurities less than 8ppm; The raw materials are controlled by the controller XI186 to enter the reaction chamber Ⅱ193 through the feed port XI185. The rotating device is turned on, and the vacuum is drawn to 0.01Pa through the vacuum interface Ⅱ188. The temperature is controlled at 1200℃ by the temperature controller VI202. The flow rate of the mixed gas is controlled at 70cm3 / min through the inert gas and flow meter interface Ⅱ203 and the reaction gas and flow meter interface Ⅱ204. After chlorination for 40 minutes, the gas enters the feed port XII206 through the discharge port XI205. The waste gas passes through the exhaust port and the waste gas treatment interface VII187. Controller XII207 controls the raw materials to enter the gradient pickling tank II220 through inlet XII206 at a liquid-to-solid ratio of 4:1, and introduces the pickling agent through auxiliary material inlet III210. In the first layer of gradient pickling tank II220, pickling agent 1 (H₂C₂O₄ 12%) is introduced, and in the second layer, pickling agent 2 (HF 5%+) is introduced. H2C2O4 12%, third layer introduces acid leaching agent 3: acid ratio HF 5% + H2C2O4 12% + H2SiF6, the lower layer introduces ultrapure water from ultrapure water interface VIII213, pressure gauge II211 controls the pressure to 1MPa, timer V208 controls the time to 40min / layer, temperature controller VII209 controls the temperature to 90℃, after acid leaching is completed, it automatically flows into the next layer, after microwave cleaning in the lower layer, it flows into the material pipe VIII224 through the discharge port XII223, the waste liquid is discharged to the waste liquid treatment interface VIII222 through the waste liquid discharge channel III219 for treatment, and the waste gas is treated through the exhaust port and the waste gas treatment interface VIII212; The controller XIII230 controls the raw material through feed pipe VIII224 to enter the multi-functional rotary pickling tank II240 through feed inlet XIII229 at a liquid-to-solid ratio of 4:1. The pickling agent is introduced through auxiliary material inlet IV226. The acid ratio is HCl 20% + H2SO4 10% + HF 5%. The temperature is controlled at 90℃ by temperature controller VIII227, the timer is controlled at 40 minutes by timer VI228, and the pressure is controlled at 0.6MPa by pressure gauge IV231. After pickling, microwave cleaning is performed. After microwave drying at 100℃, the material flows into feed inlet XIV244 through discharge port XIII242. Ultrapure water is introduced through ultrapure water interface IX233 by cleaning device IV239. Waste liquid is discharged through waste liquid discharge channel IV238 to waste liquid treatment interface IX241 for treatment. Waste gas is treated through exhaust port and waste gas treatment interface IX232. Step Six: Plasma Fine Purification: Further fine purification is carried out using the vacuum microwave plasma purification furnace of the present invention, that is, in a high vacuum device filled with hydrogen mixed gas plasma, residual micro-nano-scale inclusions and lattice impurities are completely removed to obtain ultra-high purity quartz sand with a purity of 6N or higher. Input the plasma purification process parameters into the system intelligent control center 2: vacuum degree 10. -2 ~10 -4 Pa gas, temperature 600~1500℃, time 10~180min, mixed gas flow rate 10~150sccm, Ar flow rate above 6N 10~125sccm, H2 flow rate above 6N 10~120sccm; environment: Class 100 cleanliness, plasma excitation frequency 2.45GHz. The raw material is controlled by the controller XIV245 to enter the vacuum microwave plasma purification furnace 243 through the feed port XIV244 (return port). The fixed rotation device Ⅲ248 and the fixed rotation device Ⅳ260 are turned on, and the sealing device Ⅲ250 and the sealing device Ⅳ259 are kept in good condition. The vacuum is evacuated to 10 through the vacuum interface Ⅲ247. -4 Pa ensures that the raw material enters the reaction chamber Ⅲ252 through the feed inner pipe Ⅱ251, and the temperature is controlled at 1200℃ by the temperature controller IX261. The flow rate of the mixed gas is controlled at 60sccm through the inert gas and flow meter interface Ⅲ262 and the reaction gas and flow meter interface Ⅲ263. After purification for 40 minutes, the raw material flows into the feed inlet XV266 through the discharge port XIV264. Step 7: Quality control and product collection and processing: Finally, after vacuum cooling and quality testing, qualified products are vacuum-packed, sealed, and stored for sale. This product meets the stringent requirements of high-end fields such as semiconductors for ultra-high purity quartz sand. Input the following process parameters for quality control and product collection and processing at the system's intelligent control center 2: vacuum degree 0.1 Pa, cooling medium: argon gas above 6 N, argon gas flow rate 5-100 cm³ / h 3 / min, cooling rate 20~50℃ / min: cooling to room temperature 0~25℃, cooling environment: Class 100 cleanliness, relative humidity not exceeding 40%, product quality control: purity above 6N, impurity content below 0.1ppm, particle size and particle size distribution are formulated according to product application requirements; Controller XV267 controls the raw material to enter the cooling chamber 274 through the feed inlet XV266 and the feed inner pipe Ⅲ273. Fixed rotation devices V270 and VI277 are activated to ensure the sealing devices V272 and VI276 are intact. A vacuum of 0.1 Pa is drawn through vacuum interface Ⅳ279. The cooling temperature is controlled by temperature controller X268, maintaining a cooling rate of 30℃ / min. The flow rate of high-purity argon gas (above 5N) is controlled at 50 cm³ through inert gas and flow meter interface Ⅳ269. 3 The product is cooled to room temperature of 20-25℃ at a speed of 0.5 min. Products that pass the quality inspection enter the vacuum packaging machine 282 through the discharge port XV280. The vacuum is drawn to a vacuum degree of 0.1 Pa through the vacuum interface V281. The product vacuum packaging barrel 287 is connected to the product vacuum packaging interface 283 for vacuum packaging and then sealed and stored. The exhaust gas is treated through the exhaust port and exhaust gas treatment interface XI278.
[0032] Steps one through four are completed in a Class 1000 cleanroom environment, while steps six and seven are completed in a Class 100 cleanroom environment. The water used in steps one through six is ultrapure water with a resistivity ≥ 18.2 MΩ·cm. The waste gas generated during the processes of steps one through seven is treated to meet the standards before being discharged, and the wastewater generated is treated to meet the standards before being discharged or returned to the water treatment system. All waste generated is treated to meet the standards in a microwave plasma incinerator before being discharged.
[0033] The foregoing has shown and described the basic principles, main features, and advantages of the present invention. Those skilled in the art should understand that the present invention is not limited to the above embodiments. The embodiments and descriptions in the specification are merely principles of the invention. Various changes and modifications can be made to the invention without departing from its spirit and scope, and all such changes and modifications fall within the scope of the claimed invention. The scope of protection claimed by the appended claims and their equivalents is defined.
Claims
1. A smart manufacturing equipment for ultra-high purity quartz sand used in semiconductors, characterized in that, It includes an intelligent device rack (1) and a system intelligent control center (2); The intelligent control center (2) of the system includes a material preparation system (3), a high-purity quartz sand purification system (4), an ultra-high-purity quartz sand purification system (5), a quality control and product collection and processing system (6), a process auxiliary system (7), and a system monitoring center (8). The material preparation system (3) includes an intelligent ore bin (10), a raw ore mobile lifting tank washing machine (15), a raw ore crushing and grading integrated machine (21), a color sorter (29), a vacuum microwave roasting furnace (44), a gradient reactor I (62), a ball mill (80), and a hydrocyclone classifier (90). The intelligent ore bin (10) is equipped with an inlet, an outlet, a raw ore inlet (11), and a conveyor belt I (12). The raw ore mobile lifting tank washing machine (15) includes a feed inlet I (13), an ultrapure water interface I (14), a rotating high-pressure rinsing water cover (16), a waste liquid treatment interface I (17), a discharge outlet I (18), and a conveyor belt II (19). The raw ore crushing and grading integrated machine (21) includes discharge port II (22), return hopper (23), fine crushing and grading machine (24), medium crushing and grading machine (25), coarse crushing and grading machine (26), feed port II (27), exhaust port and waste gas treatment interface I (28). The color sorter (29) includes a feed inlet III (31), a vibrating feeder (32), a signal processor (33), a chute (34), a light source (35), a sensor (36), compressed air (37), a spray valve (38), a discharge outlet III (39), and an impurity box (40). The vacuum microwave roasting furnace (44) includes an exhaust port and waste gas treatment interface II (41), a feed port IV (42), a vacuum interface I (45), a temperature controller I (46), a furnace shell I (47), a magnetron I (48), a stainless steel plate I (49), a basalt fiber I (50), a silicon carbide tube I (51), a quartz tube I (52), a reaction chamber I (53), a reaction gas and flow meter interface I (54), an inert gas and flow meter interface I (55), and a discharge port IV (56). The gradient reactor I (62) includes a feed inlet V (57), a timer I (59), a temperature controller II (60), an auxiliary material inlet I (61), a pressure gauge I (63), an exhaust port and waste gas treatment interface III (64), an ultrapure water interface II (65), a furnace shell II (66), a magnetron II (67), a stainless steel plate II (68), a lining I (69), a waste liquid discharge channel I (70), a gradient acid leaching tank I (71), a cleaning device I (72), a waste liquid treatment interface II (73), and a discharge port V (74). The ball mill (80) includes a feed inlet VI (75), a return outlet (76), an ultrapure water interface Ⅲ (78), a feeding device (79), a base (81), ball milling media (82), a ball milling chamber (83), gears and a vibration device (84), a waste liquid treatment interface Ⅲ (85), a discharge device (86), and a discharge outlet VI (87). The cyclone classifier (90) includes: an underflow channel (88), an underflow outlet (89), a cyclone chamber (91), and a feed pipe I (92); The high-purity quartz sand purification system (4) includes a magnetic separator (96), a slurry tank I (119), a flotation machine I (127), a slurry tank II (144), a flotation II (152), a multi-functional reactor I (166), a vacuum microwave purification furnace (184), a gradient reactor II (214), and a multi-functional reactor II (225). The magnetic separator (96) includes a water-cooled outlet (94), a water-cooled inlet (95), a material pipe II (97), a pulsation device (98), an excitation coil (99), an iron yoke (100), a feed inlet VII (101), a rotating ring (102), a magnetic medium (103), an ultrapure water inlet IV (104), a rinsing water pipe (105), a magnetic material unloading hopper (106), rinsing water (107), a magnetic material box (108), a magnetic pole (109), a support base (110), a waste liquid treatment inlet IV (111), a discharge outlet VII (112), and a non-magnetic material hopper (114). The mixing tank I (119) includes a feed pipe III (115), a mixing tank inlet I (116), a reagent and ultrapure water addition tank I (117), a mixing tank outlet I (118), and a stirring device I (120). The flotation cell I (127) includes a feed pipe IV (121), a waste liquid treatment interface V (122), a feed inlet VIII (124), a timer II (125), a temperature controller III (126), a collection tank I (128), an exhaust port and waste gas treatment interface IV (129), a gas collection hood I (130), a scraper device I (131), a motor I (132), a hollow shaft I (133), an air pipe I (134), a stator I (135), an impeller I (136), an ultrapure water interface V (137), an ultrasonic device I (138), and a discharge port VIII (139). The mixing tank II (144) includes a feed pipe V (140), a mixing tank inlet II (141), a reagent and ultrapure water addition tank II (142), a mixing tank outlet II (143), and a stirring device II (145). The flotation cell II (152) includes a feed pipe VI (146), a waste liquid treatment interface VI (147), a feed inlet IX (149), a timer III (150), a temperature controller IV (151), a collection tank II (153), an exhaust port and waste gas treatment interface V (154), a gas collection hood II (155), a scraper device II (156), a motor II (157), a hollow shaft II (158), an air pipe II (159), a stator II (160), an impeller II (161), an ultrapure water interface VI (162), an ultrasonic device II (163), and a discharge port IX (164). The multifunctional reactor I (166) includes a feed pipe VII (165), an auxiliary material inlet II (167), a temperature controller V (168), a timer IV (169), a feed port X (170), a pressure gauge II (172), an exhaust port and waste gas treatment interface VI (173), an ultrapure water interface VII (174), a furnace shell III (175), a magnetron III (176), a stainless steel plate III (177), a lining II (178), a waste liquid discharge channel II (179), a cleaning device II (180), a multifunctional rotary acid leaching tank I (181), a waste liquid treatment interface VII (182), and a discharge port X (183). The vacuum microwave chlorination purification furnace (184) includes a feed inlet XI (185), an exhaust port and waste gas treatment interface VII (187), a vacuum interface II (188), a fixed rotating device I (189), a support I (190), a sealing device I (191), a feed inner tube II (192), a reaction chamber II (193), a quartz reactor II (194), a silicon carbide tube II (195), a basalt fiber layer II (196), a stainless steel plate IV (197), a magnetron IV (198), a heating box I (199), a sealing device II (200), a fixed rotating device II (201), a temperature controller VI (202), an inert gas and flow meter interface II (203), a reaction gas and flow meter interface II (204), and a discharge port XI (205). The gradient reactor II (214) includes a feed inlet XII (206), a timer V (208), a temperature controller VII (209), an auxiliary material inlet III (210), a pressure gauge II (211), an exhaust port and waste gas treatment interface VIII (212), an ultrapure water interface VIII (213), an outer shell V (215), a magnetron V (216), a stainless steel plate V (217), a lining III (218), a waste liquid discharge channel III (219), a gradient acid leaching tank (220), an acid leaching tank partition II (221), a waste liquid treatment interface VIII (222), and a discharge port XII (223). The multifunctional reactor II (225) includes a feed pipe VIII (224), an auxiliary material inlet IV (226), a temperature controller VIII (227), a timer VI (228), a feed inlet XIII (229), a pressure gauge IV (231), an exhaust port and waste gas treatment interface IX (232), an ultrapure water interface IX (233), a furnace shell VI (234), a magnetron VI (235), a stainless steel plate VI (236), a lining IV (237), a waste liquid discharge channel IV (238), a cleaning device IV (239), a multifunctional rotary acid leaching tank II (240), a waste liquid treatment interface IX (241), and a discharge port XIII (242); The ultra-high purity quartz sand purification system (5) includes a vacuum microwave plasma purification furnace (243). The vacuum microwave plasma purification furnace (243) includes a feed inlet XIV (return port) (244), an exhaust port and waste gas treatment interface X (246), a vacuum interface III (247), a fixed rotating device III (248), a support II (249), a sealing device III (250), a feed inner tube II (251), a reaction chamber III (252), a reactor III (253), a silicon carbide tube IV (254), a basalt fiber layer IV (255), a stainless steel plate VII (256), a magnetron VII (257), a heating box II (258), a sealing device IV (259), a fixed rotating device IV (260), a temperature controller IX (261), an inert gas and flow meter interface III (262), a reaction gas and flow meter interface III (263), and a discharge port XIV (264). The quality control and product collection and processing system (6) includes a cooling furnace (265), a vacuum packaging machine (282), a vacuum return barrel (284), a conveyor belt (285), a quality control system (286), and a product warehouse (288). The cooling furnace (265) includes a feed inlet XV (266), a temperature controller X (268), an inert gas and flow meter interface IV (269), a fixed rotating device V (270), a support III (271), a sealing device V (272), a feed inner tube III (273), a cooling chamber (274), a quartz cooler (275), a sealing device VI (276), a fixed rotating device VI (277), an exhaust port and waste gas treatment interface XI (278), a vacuum interface IV (279), and a discharge port XV (280). The vacuum packaging machine (282) includes a vacuum interface V (281), a product vacuum packaging interface (283), and a product vacuum packaging barrel (287). The process auxiliary system (7) includes a power supply system (289), a vacuum system (290), a temperature control system (291), a gas control system (292), a water cooling system (293), a water production system (294), a reagent preparation system (295), a waste gas treatment system (296), a waste liquid treatment system (297), and a solid waste treatment system (298). The monitoring system center (8) includes monitoring system I (299), monitoring system II (300), monitoring system III (301), monitoring system IV (302), and monitoring system V (303); The intelligent equipment rack (1) has five layers. The first layer has two layers, one high and one low, on the right side. The material preparation system (3) is located on the left side of the first and second layers and the left side of the third to fifth layers. The high-purity quartz sand purification system (4) is located on the right side of the third to fifth layers. The ultra-high purity quartz sand purification system (5) is located on the right side of the second layer. The quality control and product collection and processing system (6) is located on the right side of the upper and lower layers of the first layer. The process auxiliary system (7) is located on the left side of the lower layer. The system monitoring center (8) is located on the left end of the upper layer of the first layer. The intelligent ore bin (10), the raw ore mobile lifting trough washing machine (15), and the raw ore crushing and grading integrated machine (21) are arranged from right to left on the left side of the first layer; the color sorter (29) is arranged on the left side of the fifth layer; the vacuum microwave roasting furnace (44) is arranged on the left side of the fourth layer; the gradient reaction vessel I (62) is arranged on the left side of the third layer; the ball mill (80) and the cyclone classifier (90) are arranged from left to right on the left side of the second layer. The magnetic separator (96) is located on the left side of the third layer; the slurry preparation tank I (119) and slurry preparation tank II (144) are located on the left side of the fourth layer in sequence; the flotation machine I (127), flotation II (152) and multifunctional reactor I (166) are located on the right side of the fifth layer from left to right; the vacuum microwave purification furnace (184) is located on the right side of the fourth layer; the gradient reactor II (214) and multifunctional reactor II (225) are located on the right side of the third layer from left to right. The vacuum microwave plasma purification furnace (243) is located on the right side of the second layer; The cooling furnace (265) is located on the first high floor, and the conveyor belt IV (285), vacuum return barrel (284), quality control (286), vacuum packaging machine (282) and product warehouse (288) are arranged sequentially from right to left on the right side of the lower floor. The power supply system (289), vacuum system (290), temperature control system (291), gas control system (292), water cooling system (293), water production system (294), reagent preparation system (295), waste gas treatment system (296), waste liquid treatment system (297), and waste solid treatment system (298) are arranged from right to left on the left side of the first floor.
2. The intelligent manufacturing equipment for ultra-high purity quartz sand for semiconductors according to claim 1, characterized in that, It also includes controller I (9), controller II (20), controller III (30), controller IV (43), controller V (58), controller VI (77), controller VII (113), controller VIII (123), controller IX (148), controller X (171), controller XI (186), controller XII (207), controller XIII (230), controller XIV (245) and controller XV (267); The controller I (9) is connected to the intelligent mine bin (10) and the raw ore mobile lifting tank washing machine (14). The controller II (20) is connected to the raw ore crushing and grading integrated machine (21); The controller Ⅲ (30) is connected to the color sorter (29); The controller IV (43) is connected to the vacuum microwave roasting furnace (44). The controller V (58) is connected to the gradient reactor I (62); The controller VI (77) is connected to the ball mill (80) and the cyclone classifier (90). The controller VII (113) is connected to the magnetic separator (96); The controller VIII (123) is connected to the slurry preparation tank I (119) and the flotation tank I (127); The controller IX (148) is connected to the slurry preparation tank II (144) and the flotation tank II (152); The controller X (171) is connected to the multifunctional reactor I (166). The controller XI (186) is connected to the vacuum microwave purification furnace (184). The controller XII (207) is connected to the gradient reactor II (214); The controller XⅢ (230) is connected to the multifunctional reactor II (225); The controller XIV (245) is connected to the vacuum microwave plasma purification furnace (243). The controllers X and V (267) are respectively connected to the cooling furnace (265), the vacuum packaging machine (282), the vacuum return barrel (284), the conveyor belt IV (285), the quality control (286), and the product warehouse (288); The controllers I (9), II (20), III (30), IV (43), V (58), VI (77), VII (113), VIII (123), IX (148), X (171), XI (186), XII (207), XIII (230), XIV (245), and XV (267) are connected to different composite quartz sensors according to the control process parameters.
3. The intelligent manufacturing equipment for ultra-high purity quartz sand for semiconductors according to claim 1, characterized in that, The linings of the raw ore mobile lifting tank washing machine (15) and the raw ore crushing and grading integrated machine (21) are all made of non-polluting materials; the gradient reactor I (62) and gradient reactor II (214) are equipped with gradient acid leaching tanks; the multi-functional reactor I (166) and multi-functional reactor II (225) are equipped with multi-functional rotary acid leaching tank I (181) and multi-functional rotary acid leaching tank II (240). The linings of the gradient reactor I (62), multi-functional reactor I (166), gradient reactor II (214) and multi-functional reactor II (225) are all made of non-polluting, acid-resistant, high-temperature resistant and pressure-resistant high-quality materials.
4. The intelligent manufacturing equipment for ultra-high purity quartz sand for semiconductors according to claim 1, characterized in that, Both flotation cell I (127) and flotation cell II (152) are equipped with gas collection hood I (130) and gas collection hood II (155) to collect waste gas, and an ultrasonic device is installed at the radial joint of the flotation cell I (127) and flotation cell II (152).
5. The intelligent manufacturing equipment for ultra-high purity quartz sand for semiconductors according to claim 1, characterized in that, The inner wall of the reaction chamber I (53) of the vacuum microwave roasting furnace (44) is provided with quartz spiral reinforcing ribs; the reactors II (194) and III (253) of the vacuum microwave purification furnace (184) and vacuum microwave plasma purification furnace (243) all use high-purity, high-quality quartz tubes with internal straight reinforcing ribs. The microwave generators used in the vacuum microwave roasting furnace (44), vacuum microwave purification furnace (184) and vacuum microwave plasma purification furnace (243) are preferably 2.45 GHz microwave power sources, and the silicon carbide tubes used are hollow tubes.
6. The intelligent manufacturing equipment for ultra-high purity quartz sand for semiconductors according to claim 1, characterized in that, The system intelligent control center (2) is connected to the material preparation system (3), the high-purity quartz sand purification system (4), the ultra-high-purity quartz sand purification system (5), the quality control and product collection and processing system (6), the process auxiliary system (7), and the system monitoring center (8), respectively; the system monitoring center (8) is connected to the monitoring system I (299), the monitoring system II (300), the monitoring system III (301), the monitoring system IV (302), and the monitoring system V (303), respectively; the monitoring system I (299) is connected to the material preparation system (3); the monitoring system II (300) is connected to the high-purity quartz sand purification system (4); the monitoring system III (301) is connected to the ultra-high-purity quartz sand purification system (5); The monitoring system IV (302) is connected to the quality control and product collection and processing system (6), and the monitoring system V (303) is connected to the process auxiliary system (7); the power supply system (289) is connected to the system intelligent control center (2), the material preparation system (3), the high-purity quartz sand purification system (4), the ultra-high-purity quartz sand purification system (5), the quality control and product collection and processing system (6), the process auxiliary system (7), and the system monitoring center (8), respectively; the vacuum system (290) is connected to vacuum interface I (45), vacuum interface II (188), vacuum interface III (247), vacuum interface IV (279), and vacuum interface V (281), respectively; the temperature control system (291) is divided into The gas control system (292) is connected to the following temperature controllers: I (46), II (60), III (126), IV (151), V (168), VI (202), VII (209), VIII (227), IX (261), and X (268); the gas control system (292) is connected to the following interfaces: I (54), II (55), III (203), IV (204), III (262), III (263), and IV (269); The water cooling system (293) is connected to the water cooling outlet (94) and the water cooling inlet (95) respectively; the water production system (294) is connected to the ultrapure water interface I (14), ultrapure water interface II (65), ultrapure water interface III (78), ultrapure water interface IV (104), ultrapure water interface V (137), ultrapure water interface VI (162), ultrapure water interface VII (174), ultrapure water interface VIII (213), and ultrapure water interface IX (233) respectively; all water used in this process is connected to the water production system (294); the reagent preparation system (295) and the water production system (294) are connected to the reagent and ultrapure water addition tank I (117) and the reagent and ultrapure water addition tank II (142) respectively;The exhaust gas treatment system (296) is connected to exhaust port and exhaust gas treatment interface I (28), exhaust port and exhaust gas treatment interface II (41), exhaust port and exhaust gas treatment interface III (64), exhaust port and exhaust gas treatment interface IV (129), exhaust port and exhaust gas treatment interface V (154), exhaust port and exhaust gas treatment interface VI (173), exhaust port and exhaust gas treatment interface VII (187), exhaust port and exhaust gas treatment interface VIII (212), exhaust port and exhaust gas treatment interface IX (232), exhaust port and exhaust gas treatment interface X (246), and exhaust port and exhaust gas treatment interface XI (278), respectively; the waste liquid treatment The wastewater treatment system (297) is connected to wastewater treatment interfaces I (16), II (73), III (85), IV (111), V (122), VI (147), VII (182), VIII (222), IX (241), and IX (241) respectively; the wastewater treatment system (297) can connect to the water treatment system (294) after treating the water to meet the standards; the solid waste treatment system (298) is connected to the impurity tank (40) and the magnetic material tank (108) respectively.
7. A smart manufacturing process for ultra-high purity quartz sand for semiconductors, used in the smart manufacturing equipment for ultra-high purity quartz sand for semiconductors as described in any one of claims 1-6, characterized in that, The specific steps are as follows: Step 1: Raw Material Preparation: This includes raw ore selection, raw ore storage, raw ore washing, crushing and grading, color sorting, chlorination and calcination, acid leaching, and ball milling and grading. First, high-purity quartz raw ore is selected according to requirements and stored in the intelligent ore bin of this invention. It is then washed clean using the raw ore mobile lifting tank washing machine of this invention. The integrated crushing and grading machine of this invention performs coarse, medium, and fine crushing and grading to obtain raw materials with a particle size of 1-3 mm. A color sorter is preferred to remove discolored particles and impurities. The raw ore is first chlorinated and calcined using the vacuum microwave calcination furnace of this invention in conjunction with the microwave gradient reactor of this invention, followed by direct microwave acid leaching and microwave cleaning to complete the initial purification of the raw ore. Finally, a wet ball mill and a hydrocyclone classifier are preferred for ball milling and grading to obtain a particle size of 0. Qualified raw materials with a diameter of 1-0.3 mm, a purity of 4N or higher, and controllable impurities; Raw material preparation process parameters: Selected high-purity quartz ore quality: SiO2 mass fraction higher than 3N, total impurities <100μg / g; Preferred quality meets the reference standard: total impurity element (μg / g) <50, of which Al <30, Ti <10, Na <8, K <8, Li <5, Ca <5, Fe <3, P <2 and B <1, and trace amounts of radioactive elements and gas-liquid inclusions; Storage process parameters: Raw ore storage amount: ore amount for 72 hours of continuous production; Soaking process parameters: raw ore soaking agent 8%-12%H2C2O4 + 1%-10%HF, soaking time 4-2 hours 4 hours, rinsing water pressure 1-10 MPa; crushing and grading process parameters: coarse crushing particle size 10-30 mm, medium crushing particle size 5-10 mm, fine crushing particle size 1-5 mm; color sorting process parameters: color sorting particle size range 0.08-5 mm, color threshold: a narrow range close to white, spray intensity: air valve pressure 0.4-0.6 MPa; chlorination calcination process parameters: vacuum degree 0.1-0.01 Pa, temperature 600-1200℃, time 1-4 h, mixed gas flow rate 10-100 sccm, Ar flow rate above 5N 10-100 sccm, HCl gas flow rate above 5N 10-100 sccm; microwave acid leaching process parameters: Gradient acid leaching was achieved sequentially using acid leaching agents 1 to 3: Acid leaching agent 1: 8-12% H2C2O4, Acid leaching agent 2: Acid ratio 3-10% HF + 10-12% H2C2O4, Acid leaching agent 3: Acid ratio 3-10% HF + 8-12% H2C2O4 + H2SiF6, Liquid-solid ratio 2:1-4:1, Acid leaching pressure 0.5-1MPa, Acid leaching temperature 60-120℃, Acid leaching time 30-240min, Ultrapure water microwave cleaning, Ultrapure water quality: resistivity ≥18.2MΩ·cm, Ball milling classification process parameters: Ball mill feed particle size 1-5mm, Ball milling time 1-6h, Cyclone classification discharge particle size 0.1-0.3mm; Step 2: Gradient Magnetic Separation: A vertical ring pulsating high-gradient wet magnetic separator is preferred to remove magnetic impurities. High-gradient magnetic separation process parameters: 1.5–2.0T background magnetic field, slurry concentration 25%–30%, pulsation frequency 200–300 times / min, feed particle size controlled at -0.074mm (≥80%), and washing water volume controlled at 1–2 m³ / min. 3 / t of ore, ensuring timely discharge of magnetic products and avoiding secondary adsorption; Step 3: Ultrasonic Flotation: The prepared slurry is subjected to two ultrasonic flotations and ultrasonic cleaning using the ultrasonic temperature-controlled flotation machine of this invention to remove gangue mineral impurities; Slurry preparation and ultrasonic flotation process parameters: First slurry preparation and ultrasonic flotation process parameters: A combined reagent system and microbubble flotation column are used to remove silicate mineral impurities such as feldspar and mica; impeller speed is 100-300 rpm; aeration rate is 0.2-0.5 m³ / h. 3 / (m²·min), pulp concentration 20%-40%, ultrasonic frequency 20-40kHz, flotation temperature 30-50℃, flotation time 20-60min, ultrasonic cleaning with ultrapure water, ultrapure water quality: resistivity ≥18.2MΩ·cm; secondary pulp conditioning and ultrasonic flotation process parameters: for different mineral impurities, optimize the primary flotation reagent system, intelligently adjust the reagent dosage, adjust the pH value, ultrasonic flotation, and ultrasonic cleaning with ultrapure water to effectively remove various gangue mineral impurities; Step 4: Microwave acid leaching: Microwave acid leaching, microwave cleaning, and microwave drying are performed using the microwave multifunctional reactor of this invention to remove inclusions and impurities; Microwave acid leaching process parameters: Acid ratio of leaching agent: HCl 20~30% + H2SO4 10~20% + HF 3~5%, liquid-solid ratio 2:1~4:1, acid leaching pressure 0.5~1MPa, acid leaching temperature 60~120℃, acid leaching time 30~240min, microwave cleaning with ultrapure water, ultrapure water quality: resistivity ≥18.2MΩ·cm, microwave drying temperature 100~120℃; Step 5: Vacuum chlorination combined with hot pressing acid leaching for fine purification: Using the vacuum microwave purification furnace of this invention in conjunction with a microwave reactor, first remove lattice impurities by vacuum microwave treatment, then directly remove burst micro-nano-scale inclusions by microwave acid leaching, followed by microwave cleaning and microwave drying to obtain high-purity quartz sand with a purity of 5N or higher. Chlorination process parameters: Vacuum degree 0.1~0.01Pa, temperature 600~1200℃, time 30~240min, mixed gas flow rate 10~100sccm, Ar gas flow rate (above 5N) 10~100sccm, HCl gas flow rate (above 5N) 10~100sccm, environment: Class 100 cleanliness; Microwave acid leaching process parameters: Primary acid leaching: Gradual acid leaching is achieved by sequentially using acid leaching agents 1~3, acid leaching agent 1: H2C2O4 8~12%, acid leaching agent 2: acid ratio HF 3~10% + H2C2O4 10 ~12%, acid leaching agent 3: acid ratio HF 3~10% + H2C2O4 8~12% + H2SiF6, secondary acid leaching: acid leaching agent acid ratio: HCl 20~30% + H2SO4 10~20% + HF 3~5%, liquid-solid ratio 2:1~4:1, acid leaching pressure 0.5~1MPa, acid leaching temperature 60~120℃, acid leaching time 30~240min, ultrapure water microwave cleaning, ultrapure water quality: resistivity ≥18.2MΩ·cm, microwave drying temperature 100~120℃, total impurities less than 8ppm; Step Six: Plasma Fine Purification: Further fine purification using the vacuum microwave plasma purification furnace of this invention, i.e., in a high-vacuum device filled with hydrogen-mixed plasma, to completely remove residual micro-nano-scale inclusions and lattice impurities, obtaining ultra-high purity quartz sand with a purity of 6N or higher; Plasma purification process parameters: Vacuum degree 10 -2 ~10 -4 Pa gas, temperature 600~1500℃, time 10~180min, mixed gas flow rate 10~150sccm, Ar flow rate above 6N 10~125sccm, H2 flow rate above 6N 10~120sccm; environment: Class 100 cleanliness, plasma excitation frequency 2.45GHz. Step Seven: Quality Control and Product Collection and Processing: Finally, after vacuum cooling and quality inspection, qualified products are vacuum-packed, sealed, and stored for sale. This product meets the stringent requirements of ultra-high purity quartz sand in high-end fields such as semiconductors. Quality control and product collection and processing parameters: Vacuum degree 0.1 Pa, cooling medium: argon gas above 6N, argon gas flow rate 5–100 cm³ / h. 3 / min, cooling rate 20~50℃ / min: cooling to room temperature 0~25℃, cooling environment: Class 100 cleanliness, relative humidity not exceeding 40%, product quality control: purity above 6N, impurity content below 0.1ppm, particle size and particle size distribution are formulated according to product application requirements.
8. The intelligent manufacturing process for ultra-high purity quartz sand for semiconductors according to claim 7, characterized in that, Step 1: Selecting high-purity quartz ore with the following quality criteria: SiO2 mass fraction higher than 3N, total impurities (μg / g) < 100; preferred quality meets the following reference standards: total impurity elements (μg / g) < 50, including Al < 30, Ti < 10, Na < 8, K < 8, Li < 5, Ca < 5, Fe < 3, P < 2 and B < 1, and trace amounts of radioactive elements and gas-liquid inclusions; Step 1 uses the vacuum microwave calcination furnace of this invention in conjunction with a microwave reactor for chlorination calcination, followed by direct microwave acid leaching and microwave cleaning to complete the preliminary purification, improving the quality of the ore and ensuring the quality requirements of subsequent purification processes; This invention is suitable for the fine purification of pegmatite and vein quartz, solving the problem of scarcity of high-purity quartz ore.
9. The intelligent manufacturing process for ultra-high purity quartz sand for semiconductors according to claim 7, characterized in that, Steps one, four, and five involve using a microwave reactor for microwave acid leaching, microwave cleaning, and microwave drying to remove various inclusions in different forms, which can effectively avoid air pollution and improve product quality; Step two involves using a ring-type pulsating high-gradient wet magnetic separator to remove particulate weak magnetic impurities. Step three uses an ultrasonic temperature-controlled flotation machine to optimize the primary flotation reagent system for different mineral impurities, intelligently adjusting the reagent dosage and pH value, performing ultrasonic flotation and ultrasonic cleaning to effectively remove various gangue mineral impurities. Step five uses a vacuum microwave purification furnace in conjunction with a microwave reactor to remove lattice impurities through vacuum microwave treatment, while simultaneously using microwave acid leaching to precisely remove burst micro-nano-sized inclusions of various forms and distributions, followed by ultrapure water microwave cleaning and microwave drying to obtain high-purity quartz sand of 5N or higher. Step six further uses the vacuum microwave plasma purification furnace of this invention in a high-vacuum device filled with hydrogen mixed gas plasma to thoroughly remove residual micro-nano-sized inclusions and lattice impurities, obtaining ultra-high-purity quartz sand of 6N or higher. Step seven finally involves vacuum cooling to room temperature, quality inspection, and vacuum packaging and sealing of qualified products for storage and sale. Defective products can be returned to any step of this process for further processing based on quality issues.
10. The intelligent manufacturing process for ultra-high purity quartz sand for semiconductors according to claim 7, characterized in that, Steps one through four are completed in a Class 1000 cleanroom environment, and steps six and seven are completed in a Class 100 cleanroom environment. All water used in steps one through six is ultrapure water with a resistivity ≥18.2 MΩ·cm. The exhaust gas generated during the processes of steps one through seven is treated to meet standards before being discharged, and the wastewater generated is treated to meet standards before being discharged or returned to the water treatment system. All waste generated is treated in a microwave plasma incinerator to meet standards before being discharged.