Ultrahigh-purity quartz purification method and equipment

Abstract

The invention discloses an ultra-high-purity quartz purification method and equipment, which are used for extracting ultra-high-purity quartz, according to the principle of the method and the equipment, on the basis of a traditional process, quartz ore is synchronously heated and pressurized by adopting microwaves and ultrasonic waves in a roasting stage, so that the treatment efficiency of the quartz ore is effectively improved; through superposition of microwave and ultrasonic waves, penetration treatment of the fine inclusion can be effectively achieved, the fine inclusion can be fully opened during subsequent water quenching, and compared with a traditional technology, the method has the advantages that impurity removal / classification is more thorough, the reaction time is effectively shortened, energy consumption is remarkably reduced, the technological process is reduced, efficiency is improved, low carbon and environmental protection are achieved, and the effect of subsequent process treatment is better achieved; furthermore, in the acid leaching impurity removal process, a microwave and ultrasonic wave synchronous catalysis and pressurization mode is adopted, and compared with a traditional process, the reaction time can be further shortened, the energy consumption is remarkably reduced, and the impurity removal effect is improved.

Description

Technical Field

[0001] The invention relates to a purification technology of high-purity quartz, and in particular to a purification method and equipment of ultra-high-purity quartz. Background Art

[0002] Due to its unique molecular chain structure, lattice shape and lattice change law, high-purity quartz has excellent chemical stability, extremely low volume expansion coefficient, extremely high temperature resistance, high insulation and withstand voltage, low and stable ultrasonic delay performance, mechanical properties higher than ordinary glass, ultraviolet spectrum performance, visible light and near-infrared spectrum performance. According to international practice, quartz with SiO2 purity greater than 99.95% can be called high-purity quartz, and some even believe that quartz with SiO2 purity greater than 99.995% can be called high-purity quartz. However, due to the quality of raw ore, testing methods and purification technology, my country can only set the standard of high-purity quartz as SiO2 purity greater than 99.9%.

[0003] In the semiconductor field, high-purity quartz sand is one of the important strategic core raw materials for chip manufacturing. The chip manufacturing process is mainly divided into silicon wafer manufacturing-wafer manufacturing-chip manufacturing. The high-purity quartz materials used in each process mainly include quartz crucibles for pulling single crystal silicon rods in the silicon wafer manufacturing process, quartz glass diffusion tubes and supporting quartz flanges, quartz glass furnace tubes, quartz boats and other quartz glass equipment in the wafer manufacturing process, and photomask substrates used for lithography, etching and thin film deposition in the chip manufacturing process. Different quartz products have different requirements for the purity, inclusion content, and particle size of high-purity quartz sand, among which the requirements for high-purity quartz crucibles for pulling single crystal silicon are the most stringent.

[0004] In recent years, my country's photovoltaic and semiconductor industries have developed rapidly, and the consumption of high-purity quartz is huge. As an indispensable raw material for strategic high-tech industries, high-purity quartz is currently subject to the dual barriers of high-quality and stable mineral supply and purification process. my country's high-end high-purity quartz, especially with a purity greater than 99.99%, can only rely on imports (US Sibelco, Norway TQC). Therefore, improving the quartz purification process and breaking through the restrictions on high-purity quartz raw material mines are technical problems that need to be solved urgently in my country and even the world. Summary of the invention

[0005] The main technical problem to be solved by the present invention is to provide a method and equipment for purifying ultra-high purity quartz, which is conducive to the preparation of ultra-high purity quartz above 99.995% and reduces energy consumption.

[0006] In order to solve the above technical problems, the present invention provides a method for purifying ultra-high purity quartz. Based on the traditional process, the quartz ore is heated simultaneously by microwaves and ultrasound during the roasting stage, and the heating temperature is controlled at 800-900 degrees Celsius. The process is carried out in a closed cavity, and the pressure in the cavity is controlled at 1-5 Pa in the middle of roasting; and the ore is kept turned; the power ratio of microwave heating and ultrasonic heating is maintained at 1:1 to 5:1.

[0007] During implementation, in the acid leaching and impurity removal process, microwaves and ultrasound are used simultaneously for catalysis, the temperature is controlled at 50-120 degrees Celsius, the process is carried out in a closed chamber, the ore is kept turned, and the pressure in the chamber is controlled at 1-5 Pa in the middle of the acid leaching (microwaves and ultrasound have a pressurization effect); the power ratio of microwave heating and ultrasound is maintained at 1:3 to 5:1.

[0008] For roasting:

[0009] During implementation, after roasting, the quartz ore is sequentially subjected to water quenching, grinding, classification, and high-gradient iron removal, and then enters an acid leaching and impurity removal process.

[0010] A flotation process may also be performed between the classification and high gradient iron removal process to further improve the effect.

[0011] During implementation, the particle size of the quartz ore to be roasted is maintained at 0.5-3 cm in diameter.

[0012] During implementation, during the roasting stage, the pressure in the cavity is controlled at 3 Pa in the middle of the roasting, and pressure relief treatment is required in the later stage of the roasting.

[0013] In practice, the grinding stage grinds the quartz ore to a particle size of 40-160 mesh.

[0014] For pickling and impurity removal:

[0015] During implementation, after the acid leaching and impurity removal process is completed, the finished product needs to be cleaned, dried, color sorted, and chlorinated for impurity removal in sequence.

[0016] Preferably, after the acid leaching and impurity removal process is completed, a flotation is performed after the washing process and before drying.

[0017] During the implementation, the acid leaching and impurity removal process controls the pressure in the cavity to be 1-5 Pa.

[0018] Based on the ultra-high purity quartz purification method of the present invention, the following process steps can be adopted: raw ore → crushing → classification → dry iron removal → composite superconducting band roasting (i.e., the roasting process of the present invention) → water quenching → grinding → classification → flotation → high gradient iron removal → composite superconducting band complex reaction (i.e., the acid leaching impurity removal process of the present invention) → cleaning → drying → color sorting → chlorination impurity removal → cooling and packaging. Of course, the traditional process part can also be appropriately adjusted.

[0019] The present invention also provides an ultra-high purity quartz purification device, including a quartz ore roasting equipment unit, which includes a roasting cavity with a closed cover, on which a microwave heating device, an ultrasonic heating device, an air pressure regulating mechanism and an ore rolling mechanism are arranged; the inner cavity wall of the roasting cavity is made of zircon quartz or ultra-high purity quartz.

[0020] The present invention also provides an ultra-high purity quartz purification device, including a quartz acid leaching and impurity removal equipment unit, which includes an acid leaching cavity with a closed cover, and a microwave catalytic device, an ultrasonic catalytic device, an air pressure regulating mechanism and an ore disturbance mechanism are simultaneously arranged on the cavity, and the ore disturbance mechanism is used to keep the ore in a rolling state; the inner cavity wall of the acid leaching cavity is made of polyetheretherketone, polyimide or polytetrafluoroethylene.

[0021] The beneficial effects of the present invention are: a method and equipment for purifying ultra-high purity quartz. The principle of the method and equipment is that, based on the traditional process, the quartz ore is heated and pressurized by microwaves and ultrasound synchronously during the roasting stage, which effectively improves the processing efficiency of the quartz ore. The superposition of microwaves and ultrasound can effectively achieve the penetration treatment of fine inclusions, so that they can be fully opened during subsequent water quenching. Compared with the traditional process, the present invention removes / classifies impurities more thoroughly, effectively reduces the reaction time, significantly reduces energy consumption, reduces the process flow, improves efficiency, is low-carbon and environmentally friendly, and is more conducive to the effect of subsequent process treatment;

[0022] Furthermore, in the acid leaching impurity removal process, microwaves and ultrasound are used simultaneously for catalysis and pressurization, so that the effect of the agent can be fully exerted, the ultrasound further opens the remaining fine inclusions, and the impurities between the crystals can be better penetrated by the agent under the action of microwaves and ultrasound, thereby achieving a better reaction removal effect. Compared with the traditional process, the present invention can further reduce the reaction time, significantly reduce energy consumption, and improve the impurity removal effect. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] Figure 1 A schematic diagram of the unit structure of a roasting equipment according to an embodiment of the present invention;

[0024] Figure 2 The figure is a schematic diagram of the structure of an acid leaching and impurity removal equipment unit according to an embodiment of the present invention. DETAILED DESCRIPTION

[0025] The present invention will be further described in detail below through specific implementation modes in conjunction with the accompanying drawings.

[0026] The present invention discloses a method for purifying ultra-high purity quartz. Based on the traditional process (if the traditional process is to perform ultrasonic scrubbing and microwave roasting separately, the present invention combines the two processes and adjusts other process flows), the quartz ore is heated synchronously by microwave and ultrasonic waves during the roasting stage, the heating temperature is controlled at 800-900 degrees Celsius, and the pressure in the closed cavity is controlled at 1-5 Pa during the roasting process; and the ore is kept turned (the ore turning can be achieved by rotating, shaking, and vibrating the roasting cavity of the equipment, or by setting a corresponding stirring mechanism in the roasting cavity, and stirring is a relatively inferior solution); the power ratio of microwave heating and ultrasonic heating is maintained at 1:1 to 5:1 (the microwave power is kept not greater than the ultrasonic power). The inventor calls this process: composite superconducting band roasting.

[0027] The superposition of microwaves and ultrasonic waves can effectively achieve the penetration treatment of fine inclusions (which are extremely difficult to treat with traditional processes), so that they can be fully opened in the subsequent water quenching process, effectively improving the processing efficiency and quality of quartz ore. Compared with the traditional process, the impurity removal / classification of the present invention is more thorough, effectively reduces the reaction time, significantly reduces energy consumption, reduces the process flow, improves efficiency, is low-carbon and environmentally friendly, and is more conducive to the effect of subsequent process treatment; the quartz ore obtained on this basis can basically remove impurities through the traditional acid leaching impurity removal process to obtain ultra-high purity quartz of more than 99.995%.

[0028] In practice, it is preferred that the particle size of the quartz ore to be roasted is maintained at 0.5-3 cm in diameter. This particle size ensures a better treatment effect, higher treatment energy efficiency, facilitates subsequent treatment and processing flow, and avoids the final product being too fine.

[0029] During implementation, the quartz ore to be roasted can be obtained by first crushing the raw ore, then grading it, and then performing a dry iron removal. This process has a better effect on the treatment of roasted quartz ore. Of course, it can also be obtained by other existing applicable processes. For example, the ore with suitable particles can be directly subjected to a dry iron removal.

[0030] During implementation, preferably, in the roasting stage, the pressure in the cavity is controlled at about 3 Pa in the middle of the roasting, and the pressure is released in the later stage of the roasting. The pressure control in the roasting stage is adjusted and optimized as needed. The pressure of the roasting process is controlled at 3 Pa, so that the impurity removal effect is better, and the subsequent water quenching can more fully realize the impurity explosion, and has better energy efficiency.

[0031] It is preferred that, after the quartz ore is roasted in the patent solution (composite superconducting band roasting), it is sequentially subjected to water quenching, grinding, classification, high gradient iron removal, and then enters the acid leaching and impurity removal process. After these process steps, the impurities in the quartz ore are fully burst out, and after being ground and classified, the iron impurities are basically effectively removed, and other impurities are also in a fully exposed state, and subsequent acid washing can effectively achieve removal.

[0032] Preferably, a flotation can be performed between the classification and the high-gradient iron removal process to further improve the impurity removal effect, and the flotation can directly remove part of the impurities.

[0033] During implementation, the grinding process grinds the quartz ore to a particle size of 40-160 mesh. This facilitates subsequent processing, ensures the effect and maintains the consistency of the finished product. This particle size ensures a better processing effect, higher processing energy efficiency, facilitates subsequent processing and processing, and avoids the finished product being too fine. The final product has excellent performance and is particularly suitable for quartz crucible manufacturing.

[0034] During implementation, the cavity is heated for 0.1-2 hours and kept warm for 5-24 hours. Through the power control of microwave and ultrasonic waves, the two are heated synchronously to ensure that the ore can be heated to the predetermined temperature in 0.1 to 2 hours and kept warm for 5-24 hours, ensuring that the ore is fully and effectively processed and improving the processing effect. Based on the implementation of this solution, the insulation time is greatly reduced compared with the traditional process, achieving energy conservation and emission reduction and reducing production costs.

[0035] In the first embodiment of the roasting (composite superconducting band roasting) of the patented method, a quartz ore with a SiO2 purity of 99.8% and a particle size of 1 cm is placed in a closed roasting chamber, and microwave and ultrasonic waves are used for simultaneous heating. After half an hour of heating, the temperature is controlled to 830 degrees Celsius. In the middle of the process, the pressure in the closed chamber is controlled at 3 Pa; the ore is kept turning by rotating the roasting chamber of the equipment; the power ratio of microwave heating and ultrasonic heating is maintained at 1:2. The chamber is kept warm at 830° for 12 hours, and then the roasting chamber is opened by pressure relief, and the ore is poured into cold water for quenching. After completion, the ore is ground to a particle size of 40-160 mesh, and then graded, and then high-gradient iron removal is performed to remove impurities. The ore / particle obtained by this process has an iron removal rate of more than 99.98%, and the fine inclusions are basically completely exposed. Subsequent processing is extremely convenient. Even if the traditional acid leaching impurity removal process is used later, ultra-high purity quartz of more than 99.998% can be easily obtained. Energy consumption is greatly reduced and processing efficiency is greatly improved.

[0036] In the second embodiment of the roasting (composite superconducting band roasting) of the patented method, a quartz ore with a SiO2 purity of 99.8% and a particle size of 2 cm is placed in a closed roasting chamber, and microwave and ultrasonic waves are used for simultaneous heating. After half an hour of heating, the temperature is controlled to 890 degrees Celsius. In the middle of the process, the pressure in the closed chamber is controlled at 3.5 Pa; the ore is kept turning by rotating the roasting chamber of the equipment; the power ratio of microwave heating and ultrasonic heating is maintained at 1:1.5. The chamber is kept warm at 890° for 15 hours, and then the pressure is released to open the roasting chamber, and the ore is poured into cold water for quenching. After completion, the ore is ground to a particle size of 40-160 mesh, and then graded, and then high-gradient iron removal is performed to remove impurities. The ore / particle obtained by this process has an iron removal rate of more than 99.95%, and the fine inclusions are basically completely exposed. Subsequent processing is extremely convenient. Even if the traditional acid leaching impurity removal process is used later, ultra-high purity quartz of more than 99.995% can be easily obtained. Energy consumption is greatly reduced and processing efficiency is greatly improved.

[0037] The present invention discloses a method for purifying ultra-high purity quartz. In the acid leaching and impurity removal process, the microwave and ultrasonic waves are optimized to be used for simultaneous catalysis. The temperature is controlled at 50-120 degrees Celsius (microwave and ultrasonic waves have the functions of heating and pressurization at the same time). The process is carried out in a closed cavity (reactor), and the ore is kept turned (the ore turning can be achieved by rotating, shaking, and vibrating the reactor, or by setting a corresponding stirring mechanism in the reactor. Stirring is a relatively inferior solution); the pressure in the cavity is controlled at 1-5 Pa in the middle of the acid leaching; the power ratio of microwave heating and ultrasound is maintained at 1:3 to 5:1. The inventor calls this process: composite superconducting band complex extraction reaction.

[0038] The acid leaching impurity removal process uses microwaves and ultrasound to catalyze and pressurize simultaneously, so that the agent can play a more effective role. The ultrasound further opens the remaining fine inclusions, and the impurities between the crystals can be better penetrated by the agent under the action of microwaves and ultrasound, achieving a better and more thorough reaction removal effect. Compared with the traditional process, the present invention can further reduce the reaction time, significantly reduce energy consumption, and improve the impurity removal effect. In the traditional quartz purification process, the roasting is replaced by the aforementioned roasting scheme, and the acid leaching impurity removal scheme of the present invention is used to achieve the final preparation of ultra-pure quartz of more than 99.999%.

[0039] During implementation, preferably, the pressure in the chamber of the acid leaching and impurity removal process is controlled at about 3 Pa. Under this pressure, the pickling reaction can be well promoted, and the acid solution can effectively penetrate into the gaps of the ore particles in combination with microwave and ultrasonic waves, ensuring the best treatment effect and energy efficiency ratio.

[0040] During implementation, after the acid leaching and impurity removal process is completed, the finished product needs to be cleaned, dried, color sorted, and chlorinated for impurity removal in sequence. Thereby, a purer quartz material is obtained. That is, the optimized purification scheme of the present invention is: roasting (composite superconducting band roasting) - water quenching - grinding - classification - high gradient iron removal - acid leaching and impurity removal (composite superconducting band complex extraction) - cleaning - drying - color sorting - chlorination for impurity removal. As mentioned above, a flotation can also be added between the classification and high gradient iron removal processes.

[0041] Preferably, after the acid leaching and impurity removal process is completed, a flotation is performed after the cleaning process and before drying. The process can be further optimized to improve the impurity removal effect. That is, the overall process of one implementation scheme is: roasting (composite superconducting band roasting) - water quenching - grinding - classification - high gradient iron removal - acid leaching and impurity removal (composite superconducting band complex extraction) - cleaning - flotation - drying - color sorting - chlorination impurity removal. As mentioned above, a flotation can also be added between the classification and high gradient iron removal processes.

[0042] During the acid leaching and impurity removal process, the constant temperature acid leaching is maintained for 5-24 hours, and the pressure relief treatment is performed later. The constant temperature acid leaching is maintained for a certain period of time to allow the reaction to proceed fully and the impurities to be removed thoroughly. Based on the implementation of this solution, the constant temperature acid leaching time is greatly reduced compared to the traditional process, achieving energy conservation and emission reduction and reducing production costs.

[0043] The patented method, on the basis of the above-mentioned roasting (composite superconducting band roasting) of ore with SiO2 purity of more than 99.8%, is preferably carried out in sequence through water quenching, grinding, classification, and high-gradient iron removal processes, and then enters the acid leaching and impurity removal process. Example 1: In the reactor (enclosed cavity), microwaves and ultrasound are used for synchronous catalysis. The temperature is controlled at 90 degrees Celsius (heating for 0.5 hours) by microwaves and ultrasound, and the ore is kept turning (the ore turning can be achieved by rotating, shaking, and vibrating the reactor); the pressure in the cavity is controlled at 3 Pa in the middle of acid leaching; the power ratio of microwave heating and ultrasound is maintained at 1:3. Constant temperature acid leaching is maintained for 12 hours, and pressure relief treatment is performed in the later stage. Then the finished product is washed, floated, dried, color sorted, and chlorinated for impurity removal in sequence to obtain 99.9998% ultra-pure quartz.

[0044] The patented method, based on the above-mentioned roasting (composite superconducting band roasting) of ore with SiO2 purity of more than 99.8%, is preferably carried out in sequence through water quenching, grinding, classification, and high-gradient iron removal processes, and then enters the acid leaching and impurity removal process. Example 2: In the reactor (enclosed cavity), microwaves and ultrasound are used for simultaneous catalysis. The temperature is controlled at 100 degrees Celsius (heating for 1 hour) by microwaves and ultrasound, and the ore is kept turning (the ore turning can be achieved by rotating, shaking, and vibrating the reactor); the pressure in the cavity is controlled at 3.5 Pa in the middle of acid leaching; the power ratio of microwave heating and ultrasound is maintained at 1:4. Constant temperature acid leaching is maintained for 10 hours, and pressure relief treatment is performed in the later stage. Then the finished product is washed, floated, dried, color sorted, and chlorinated to remove impurities, and 99.9995% ultra-pure quartz can be obtained.

[0045] Based on the ultra-high purity quartz purification method and equipment of the present invention, the following more detailed process steps can be adopted: raw ore → crushing → classification → dry iron removal → composite superconducting band roasting (i.e., the roasting process of the present invention) → water quenching → grinding → classification → flotation (can be omitted) → high gradient iron removal → composite superconducting band complex reaction (i.e., the acid leaching impurity removal process of the present invention) → cleaning (flotation can be added once afterwards) → drying → color sorting → chlorination impurity removal → cooling and packaging. Of course, appropriate adjustments can also be made on the basis of traditional processes. And the obvious front-end process (raw ore → crushing → classification → dry iron removal) and the back-end process (cleaning → drying → color sorting → chlorination impurity removal → cooling and packaging) can be adjusted very flexibly, for example, a flotation effect will be better after cleaning and before drying; the intermediate process (water quenching → grinding → classification → flotation → high gradient iron removal) is obvious, and it can also be appropriately adjusted or process processing can be added according to needs, or part of the process can be replaced and / or repeated with the front-end / back-end process.

[0046] Through the method of the present invention and the above-mentioned process, combined with suitable domestic quartz ore, and better mixed acid ratio and parameter control, the production of ultra-high purity quartz up to 99.9998% can be achieved with high efficiency, low energy consumption, low carbon and environmental protection.

[0047] Please refer to Figure 1 , 2 The figure shows a schematic diagram of the structure of an ultra-high purity quartz purification device.

[0048] Reference Figure 1 As shown, the present invention also provides an ultra-high purity quartz purification device, including a quartz ore roasting device unit, which includes a roasting cavity with a closed cover, on which a microwave heating device 5, an ultrasonic heating device 4, an air pressure regulating mechanism 8 and an ore disturbance mechanism are arranged, and the ore disturbance mechanism is used to keep the ore in a rolling state; the inner cavity wall of the roasting cavity is made of zircon quartz or ultra-high purity quartz.

[0049] The ore disturbance mechanism can be a rotating drive mechanism, a shaking mechanism or a vibration mechanism of a roasting cavity. In the embodiment of the present patent, the preferred structure is a structure in which the roasting cavity is driven to rotate by a motor.

[0050] As shown in Figure 1, an embodiment of a quartz ore roasting equipment unit (a tubular roasting furnace for quartz impurity removal) includes an equipment support 11, on which a cylindrical metal isolation cover 6 is fixedly arranged for preventing the aforementioned microwave leakage, a U-shaped cylindrical tubular quartz reaction tube body 1 is provided in a loop in the metal isolation cover 6, the quartz reaction tube body 1 is made of high-purity zirconium quartz, the left center tail of the quartz reaction tube body 1 extends forward and is limited (only axial rotation is allowed), and a supporting mechanism is provided between the right side and the gap between the metal isolation cover 6 to ensure that the quartz reaction tube body 1 can axially rotate in the metal isolation cover 6. The quartz reaction tube body 1 is arranged horizontally and its right side is open, and a sealing cover 2 that can be opened and closed is provided at the opening, and the inner wall part of the sealing cover 2 and the quartz reaction tube body 1 forming a closed cavity is made of high-purity zirconium quartz to ensure that the container does not undergo physical changes during high-temperature treatment in the tubular roasting furnace. A telescopic rod cover opening device 3 is also provided on the equipment support 11, which drives the sealing cover 2 to open or close the opening of the quartz reaction tube body 1 when working. In addition, a sealing ring 14 made of flexible graphite is also provided on the contact surface between the quartz reaction tube body 1 and the sealing cover to further ensure the reliability of the seal between the two. An ultrasonic heating device 4 is provided at the bottom of the U-shaped structure on the left side of the quartz reaction tube body 1 and penetrates its body; the ultrasonic heating device 4 includes an ultrasonic host 4a provided on the outside of the left side of the quartz reaction tube body 1, and an ultrasonic transducer 4b located on the central axis inside the quartz reaction tube body 1, and the ultrasonic host 4a and the ultrasonic transducer 4b are connected through the tube wall. The ultrasonic transducer 4b is located on the central axis to ensure that the position of the ultrasonic transducer 4b remains unchanged when the quartz reaction tube body 1 rotates, and only rotates by itself. The ultrasonic transducer 4b adopts a zirconium transducer. A waveguide cavity 5a penetrating the metal isolation cover 6 is provided at the lower part of the quartz reaction tube body 1, and the waveguide cavity 5a is combined with a variable frequency magnetron 5b and a variable frequency power supply 5c to form a microwave heating device 5. The waveguide cavity 5a introduces microwaves into the inner cavity of the quartz reaction tube body 1 for heating, and the metal isolation cover 6 reflects the microwaves to prevent them from leaking to the outside. The waveguide cavity 5a maintains a 5mm spacing with the outer wall of the quartz reaction tube body 1 to avoid collision during rotation. The part extending from the left center tail of the quartz reaction tube body 1 to the outside of the metal isolation cover 6 cooperates with a rotating drive motor 10 through a pulley, and the quartz reaction tube body 1 is driven to rotate at a uniform speed together with the sealing cover 2, so that the ore in the quartz reaction tube body 1 is driven to keep turning continuously during ore processing. A plurality of pipelines are also arranged on the left side of the quartz reaction tube body 1, and the air pressure regulating mechanism 8, the feeding mechanism 9 and the sensor unit 7 are connected through the pipelines. The relevant pipelines rotate together when the quartz reaction tube body 1 rotates, or a pipeline mechanism supporting the corresponding rotation is set, or the structure of the quartz reaction tube body 1 can be improved (a fixed loop area is set at the bottom of the left side), or the relevant pipelines can be set to the right sealing cover 2. The sensor unit 7 is provided with a safety valve, a pressure gauge, a pressure sensor and a temperature sensor.A PLC for overall control and monitoring is also provided. The PLC also controls the microwave heating device 5 and the ultrasonic heating device 4 to adjust their power, change the temperature and pressure, etc., and drives and controls the rotary drive motor 10 to control the quartz reaction tube body 1 ore turning mechanism to work synchronously, etc. An equipment base 12 is provided directly below the equipment support 11, and a rotating tilting device 13 is provided at the lower right part of the equipment support 11. The rotating tilting device 13 is connected to the equipment base 12 and the equipment support 11 at the same time, and one end of the equipment support 11 is driven to rotate and separate from the equipment base 12 through the tilting device 13, such as. Figure 2 The whole device is tilted, and the sealing cover 2 is opened at the same time, so that the quartz ore in the quartz reaction tube body 1 can be tilted and poured out.

[0051] In one embodiment, a tubular roasting furnace for quartz impurity removal, the inner cavity volume of the quartz reaction tube body 1 is 100L. The microwave and ultrasonic combination can heat up to 800-1000 degrees, and the temperature can be adjusted by power input. The quartz reaction tube body 1 rotates during roasting, with a speed of 0-10 rpm, and the quartz ore rotates inside the equipment under the action of gravity. The air pressure regulating mechanism 8 can adjust the pressure to a maximum of only 3 MPa (the quartz reaction tube body 1 and the sealing cover 2 and the sealing ring 14 can withstand this pressure). The power supply of the microwave heating device 5 can be 380V±10V, power: 50KW, frequency: 2450+50Hz, microwave leakage: <5mW / cm. The rotary drive motor 10 adopts a high-precision stepping motor controlled by PLC. The ultrasonic heating device 4 adopts a probability of 8000W and a nominal frequency of 20kHZ.

[0052] Reference Figure 2 As shown, the present invention also provides an ultra-high purity quartz purification device, including a quartz acid leaching impurity removal equipment unit, which includes an acid leaching cavity with a closed cover, on which a microwave catalytic device 105, an ultrasonic catalytic device 104, an air pressure regulating mechanism 108 and an ore disturbance mechanism are simultaneously arranged, and the ore disturbance mechanism is used to keep the ore in a rolling state; the inner cavity wall of the acid leaching cavity is made of polyetheretherketone (PEEK), polyimide or polytetrafluoroethylene.

[0053] The ore disturbance mechanism can be a rotation drive mechanism, a shaking mechanism or a vibration mechanism of an acid leaching chamber. In the embodiment of the present patent, the preferred structure is a structure in which the acid leaching chamber is driven to rotate by a motor.

[0054] like Figure 2As shown, the quartz acid leaching and impurity removal equipment unit (a horizontal reactor) includes a horizontally placed U-shaped reactor body 101 and a quick-opening reactor cover 102 for closing the opening of the reactor body. The reactor body and the quick-opening reactor cover are detachably connected through a safety buckle (or a bolt 103), and a sealing ring 114 made of acid- and alkali-resistant polymer material is also provided on the contact surface between the reactor body and the quick-opening reactor cover. An ultrasonic catalytic device 104 penetrating the reactor body is provided at the bottom of the U-shaped structure of the reactor body 101; a microwave catalytic device 105 radiating into the tube is provided on the outer wall of the reactor body 101; a microwave isolation layer is also provided to envelop the outer wall of the reactor body to prevent the aforementioned microwave from leaking; and an ore turning mechanism is also provided to drive the processed ore in the reactor body 101 to turn over.

[0055] like Figure 2 As shown, it is preferred that the bottom edge of the horizontal reactor body 101 is at an angle of -5 to -15 degrees with the horizontal. There are three schemes to achieve the angle: 1. The two sides of the U-shaped reactor body 101 are at an angle of 10-30 degrees, and the central axis of the inner cavity tube body of the reactor body 101 is located in the horizontal plane; 2. Or the two sides of the U-shaped reactor body 101 are parallel, and the central axis of the inner cavity tube body of the reactor body 101 is at an angle of -5 to -15 degrees with the horizontal plane; 3. The reactor body 101 can also be provided with a tilting mechanism, which drives the reactor body 101 to tilt from the horizontal to an angle of -5 to -15 degrees with the horizontal during the cleaning stage (maintaining the horizontal during the conventional acid leaching and impurity removal stage).

[0056] like Figure 2 As shown, it is preferred that the ultrasonic catalytic device 104 includes an ultrasonic main unit 104a, an ultrasonic transducer head 104b and a transducer head anti-corrosion layer 104c, the ultrasonic main unit 104a is arranged on the outside of the reactor body 101, and the ultrasonic transducer head 104b penetrates the bottom center of the U-shaped structure of the reactor body 101 and is arranged on the central axis of the inner cavity tube body of the reactor body 101.

[0057] like Figure 2 As shown, during implementation, the inner wall of the reaction kettle body 101 and the inner wall of the quick-opening kettle cover 102 are made of polymer acid- and alkali-resistant materials; the anti-corrosion layer 104c is an anti-corrosion ceramic protective layer or a polymer acid- and alkali-resistant material protective layer on the surface of the ultrasonic transducer head 104b; the polymer acid- and alkali-resistant material is polyetheretherketone, polyimide or polytetrafluoroethylene.

[0058] like Figure 2 As shown, during implementation, the microwave catalytic device 105 includes a microwave variable frequency power supply 105c, a variable frequency magnetron 105b and a waveguide cavity 105a. The waveguide cavity 105a is close to the outer wall of the reactor body 101 to guide microwaves into the inner cavity of the reactor body 101.

[0059] like Figure 2 As shown, it is preferred that during implementation, the outer wall of the reactor body 101 has a cylindrical profile, and the microwave isolation layer is a metal isolation cover 106 with a cylindrical inner cavity. The metal isolation cover 106 and the waveguide cavity 105a are both kept at a distance of 3-20 mm from the outer wall of the reactor body 101.

[0060] like Figure 2 As shown, during implementation, the ore turning mechanism is a rotation drive mechanism of the reactor body 101, including a rotation drive motor 110, a transmission belt 112, and a driven disk 112 fixed at the tail of the reactor body 101; the rotation drive motor 110 rotates at a constant speed and drives the reactor body 101 to rotate at a constant speed through the transmission belt 112 and the driven disk 112, thereby driving the ore processed in the reactor body 101 to turn over.

[0061] like Figure 2 As shown, during implementation, a regulating mechanism 108 for regulating the air pressure in the reaction kettle cavity, a liquid inlet mechanism 109 for inputting acid and water, a sensor unit 107 and an inlet and outlet water mechanism 111 are also provided; the inner cavity of the reaction kettle body 101 is connected with the air pressure regulating mechanism 108, the liquid inlet mechanism 109 and the inlet and outlet water mechanism 111 respectively through pipelines with valves; the inner cavity of the reaction kettle body 101 is also connected with the sensor unit 107 through a pipeline, and the sensor unit 107 is provided with a safety valve, a pressure gauge and a pressure sensor.

[0062] like Figure 2 As shown, it is preferred that a PLC for monitoring and controlling is also provided during implementation. The PLC also controls the microwave catalytic device 105, the ultrasonic catalytic device 104 and the ore turning mechanism to work synchronously.

[0063] In one embodiment, the reactor has a volume of 150L, ​​a pressure of 3 MPa, a power supply of 220v±10v, a power of 15KW, a frequency of 2450+50Hz, and a microwave leakage control of <5mW / cm. The rotary drive motor 110 uses a stepper motor and is controlled by PLC. The reaction temperature in the reactor body is 100°C-200°C, and the wavelengths of ultrasound and microwave need to pass through quartz sand.

[0064] The invention discloses an ultra-high purity quartz purification method and equipment, which can realize the preparation of ultra-high purity quartz based on conventional quartz ore of domestic quality, and the purity of quartz can reach above 99.995%. Under the condition of better mixed acid ratio and parameter control, the preparation of ultra-high purity quartz up to 99.9998% can be realized (the purity of SiO2 of the raw ore before roasting should be controlled to above 99.8%), and it is efficient, low energy consumption, low carbon and environmentally friendly.

Claims

1. A method for purifying ultra-high purity quartz, characterized in that: Based on the traditional process, quartz ore is heated simultaneously by microwaves and ultrasound during the roasting stage. The heating temperature is controlled at 800-900 degrees Celsius. The process is carried out in a closed cavity. The pressure in the cavity is controlled at 1-5 Pa in the middle of roasting; and the ore is kept turned; the power ratio of microwave heating and ultrasonic heating is maintained at 1:1 to 5:

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2. The method for purifying ultra-high purity quartz according to claim 1, characterized in that: In the acid leaching and impurity removal process, microwave and ultrasonic waves are used simultaneously for catalysis, the temperature is controlled at 60-80 degrees Celsius, the process is carried out in a closed chamber, and the ore is kept rolling. The pressure in the chamber is controlled at 1-5 Pa in the middle stage of acid leaching; the power ratio of microwave heating and ultrasonic waves is maintained at 1:3 to 5:

1.

3. The method for purifying ultra-high purity quartz according to claim 2, characterized in that: After the acid leaching and impurity removal process is completed, the finished product needs to be cleaned, dried, color sorted, and chlorinated for impurity removal in sequence.

4. The method for purifying ultra-high purity quartz according to claim 1, 2 or 3, characterized in that: The particle size of the quartz ore to be roasted is maintained at 0.5-3 cm in diameter.

5. The method for purifying ultra-high purity quartz according to claim 1, 2 or 3, characterized in that: After roasting, the quartz ore is sequentially subjected to water quenching, grinding, classification, high-gradient iron removal, and then enters the acid leaching and impurity removal process.

6. The method for purifying ultra-high purity quartz according to claim 1, 2 or 3, characterized in that: In the roasting stage, the pressure in the cavity is controlled at 3 Pa in the middle of the roasting, and the pressure is released in the late stage of the roasting.

7. The method for purifying ultra-high purity quartz according to claim 5, characterized in that: The grinding stage grinds the quartz ore to a particle size of 40-160 mesh.

8. The method for purifying ultra-high purity quartz according to claim 2 or 3, characterized in that: In the acid leaching and impurity removal process, the pressure in the cavity is controlled at 1-5 Pa.

9. An ultra-high purity quartz purification device, characterized in that: The invention discloses a quartz ore roasting equipment unit, which comprises a roasting cavity with a closed cover, on which a microwave heating mechanism, an ultrasonic heating device, an air pressure regulating mechanism and an ore disturbance mechanism are arranged; the inner cavity wall of the roasting cavity is made of zircon quartz or ultra-high purity quartz.

10. An ultra-high purity quartz purification device, characterized in that: The invention discloses an acid leaching and impurity removal equipment unit for quartz, which comprises an acid leaching cavity with a closed cover, on which a microwave catalytic device, an ultrasonic catalytic device, an air pressure regulating mechanism and an ore disturbance mechanism are arranged at the same time; the inner cavity wall of the acid leaching cavity is made of polyetheretherketone, polyimide or polytetrafluoroethylene.

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