High-purity quartz purification equipment, mixed acid, and purification process

Abstract

The invention discloses a high-purity quartz purification device, a mixed acid, and a purification process for preparing high-purity quartz. The roasting furnace and the reactor of the device both adopt a heating / catalytic method combining microwave and ultrasonic waves, and simultaneously have a heating and pressurizing effect, so that the treatment of quartz ore is more thorough, fine inclusions are effectively opened, and impurities are fully separated / removed under pressure, so as to obtain higher-purity high-purity quartz under the premise of saving energy consumption and improving efficiency; a large number of components of the mixed acid are replaced by organic acids with less harm and looser control, especially a large amount of hydrofluoric acid is replaced, which has a positive impact on environmental protection and safety, reduces production thresholds and costs, and effectively achieves the effect of acid leaching and impurity removal; the purification process greatly improves the efficiency and effect of quartz purification by improving the roasting and acid leaching and impurity removal processes, realizes the preparation of higher-purity high-purity quartz, and breaks the blockade of high-purity quartz technology in Europe and the United States.

Description

Technical Field

[0001] The invention relates to the field of high-purity quartz purification, and in particular to high-purity quartz purification equipment, mixed acid, and purification process. 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 high-purity quartz purification equipment, mixed acid, and purification process, which can be used for quartz purification, significantly reduce energy consumption, improve impurity removal effect and efficiency, and obtain high-purity quartz.

[0006] In order to solve the above technical problems, the present invention provides a high-purity quartz purification device, comprising a tubular roasting furnace for a roasting process and a horizontal reactor for an acid leaching impurity removal process;

[0007] The tubular roasting furnace comprises: a U-shaped quartz reaction tube body and a sealing cover for sealing the opening of the quartz reaction tube body; an ultrasonic heating device penetrating the body is arranged at the bottom of the U-shaped structure of the quartz reaction tube body; a microwave heating device radiating into the tube is arranged on the outer wall of the quartz reaction tube body, and a metal isolation cover is also arranged to envelop the outer wall of the quartz reaction tube body to prevent the microwave leakage; and a rotary drive motor is also provided to drive the quartz reaction tube body to rotate;

[0008] The horizontal reactor comprises: a horizontally placed U-shaped reactor body, and a quick-opening lid for closing the opening of the reactor body; an ultrasonic catalytic device penetrating the reactor body is arranged at the bottom of the U-shaped structure of the reactor body; a microwave catalytic device radiating into the tube is arranged on the outer wall of the reactor body; a corresponding metal isolation layer is also arranged to envelop the outer wall of the reactor body to prevent the aforementioned microwave from leaking; and a rotating motor is also included to drive the reactor body to rotate.

[0009] In one embodiment, the tubular roasting furnace: the quartz reaction tube body is horizontally arranged, and also includes an equipment bracket, a tilting device arranged at the bottom of the equipment bracket and an equipment base. All components of the tubular roasting furnace used for quartz impurity removal are arranged on the equipment bracket, and the tilting device is used to rotate and drive one end of the equipment bracket to separate from the equipment base, so that the quartz reaction tube body is tilted to pour out the ore in the tube; the horizontal reactor: the bottom edge of the horizontally placed reactor body is at an angle of -5 to -15 degrees with the horizontal.

[0010] In one embodiment, the ultrasonic heating device of the tubular roasting furnace includes an ultrasonic main unit and an ultrasonic transducer head, wherein the ultrasonic main unit is arranged on the outside of the quartz reaction tube body, and the ultrasonic transducer head penetrates the bottom center of the U-shaped structure of the quartz reaction tube body, and is arranged on the central axis of the inner cavity tube body of the quartz reaction tube body; the ultrasonic catalytic device of the horizontal reactor includes an ultrasonic main unit, an ultrasonic transducer head and a transducer head anti-corrosion layer, wherein the ultrasonic main unit is arranged on the outside of the reactor body, and the ultrasonic transducer head penetrates the bottom center of the U-shaped structure of the reactor body, and is arranged on the central axis of the inner cavity tube body of the reactor body.

[0011] In one embodiment, the inner cavity wall formed by the quartz reaction tube body and the sealing cover of the tubular roasting furnace is made of high-purity zircon quartz material; the ultrasonic transducer head adopts a zirconium transducer head or is covered with a layer of high-purity quartz / high-purity zirconium quartz layer on the basis of PZT lead zirconate titanate piezoelectric ceramic material; the inner cavity wall of the reactor body of the horizontal reactor and the inner wall of the quick-opening reactor cover are made of polymer acid and alkali resistant material; the anti-corrosion layer 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; the polymer acid and alkali resistant material is polyetheretherketone, polyimide or polytetrafluoroethylene.

[0012] In one embodiment, the microwave heating device of the tubular roasting furnace includes a microwave variable frequency power supply, a variable frequency magnetron and a waveguide cavity, and the waveguide cavity is close to the outer wall of the quartz reaction tube body to introduce microwaves into the inner cavity of the quartz reaction tube; the microwave catalytic device of the horizontal reactor includes a microwave variable frequency power supply, a variable frequency magnetron and a waveguide cavity, and the waveguide cavity is close to the outer wall of the reactor body to introduce microwaves into the inner cavity of the reactor body.

[0013] In one embodiment, the tubular roasting furnace is further provided with an air pressure regulating mechanism, a feeding mechanism and a sensor unit, and the inner cavity of the quartz reaction tube body is respectively connected to the air pressure regulating mechanism and the feeding mechanism through a pipe with a valve; the inner cavity of the quartz reaction tube body is also connected to the sensor unit through a pipe, and the sensor unit is provided with a safety valve, a pressure gauge and a pressure sensor; the horizontal reactor is also provided with a regulating mechanism for regulating the air pressure in the reactor cavity, a liquid inlet mechanism for inputting acid and water, a sensor unit and an inlet ionized water mechanism; the inner cavity of the reactor body is respectively connected to the air pressure regulating mechanism, the liquid inlet mechanism and the inlet ionized water mechanism through a pipe with a valve; the inner cavity of the reactor body is also connected to the sensor unit through a pipe, and the sensor unit is provided with a safety valve, a pressure gauge and a pressure sensor; a PLC for monitoring and controlling is also provided, and the PLC also controls the microwave catalytic device, the ultrasonic catalytic device and the rotating motor to work synchronously, and the PLC also controls the microwave heating device, the ultrasonic heating device and the rotating drive motor to work synchronously.

[0014] In one embodiment, the outer wall of the quartz reaction tube body of the tubular roasting furnace has a cylindrical profile, the metal isolation cover has a cylindrical inner cavity, and the metal isolation cover and the waveguide cavity are both spaced 3-20 mm apart from the outer wall of the quartz reaction tube body.

[0015] In one embodiment, a telescopic rod cover opening device is provided between the quartz reaction tube body and the sealing cover of the tubular roasting furnace to drive the sealing cover to open or close the opening of the quartz reaction tube body, and a sealing ring made of flexible graphite is also provided on the contact surface between the quartz reaction tube body and the sealing cover.

[0016] A high-purity quartz purification mixed acid is used in the high-purity quartz purification equipment as described above. The mixed acid is added to the horizontal reactor in the acid leaching and impurity removal process. The mixed acid contains: water, oxalic acid, aminosulfonic acid, a penetrant, citric acid and / or hydrochloric acid.

[0017] The concentration of the mixed acid is 25-35%, and the penetrant is silicate or sodium oleate.

[0018] In one embodiment, the mixed acid further comprises one or more of sulfuric acid, nitric acid, tartaric acid, fulvic acid, silicic acid, perchloric acid, benzoic acid, and hydrofluoric acid.

[0019] A high-purity quartz purification process, in which the high-purity quartz purification equipment and the high-purity quartz purification mixed acid as described above are used; the process is based on the traditional process:

[0020] In the roasting stage, the quartz ore is put into the tubular roasting furnace, and microwave and ultrasonic waves are used for simultaneous heating. 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. The ore is kept turned. The power ratio of microwave heating and ultrasonic heating is maintained at 1:1 to 5:1.

[0021] After roasting, the quartz ore is sequentially subjected to water quenching, grinding, grading, and high-gradient iron removal, and then enters the acid leaching and impurity removal process; in this process, the ore is transferred to the horizontal reactor and the mixed acid is added; in the acid leaching and impurity removal process, microwave and ultrasonic waves are used for simultaneous catalysis, the temperature is controlled at 60-80 degrees Celsius, the process is carried out in a closed cavity, and the ore is kept rolling, and the pressure in the cavity 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.

[0022] In one embodiment, the particle size of the quartz ore to be roasted is maintained at 0.5-3 cm in diameter; the quartz ore is ground to a particle size of 40-160 mesh in the grinding stage; and the pressure in the chamber of the acid leaching and impurity removal process is controlled at 1-5 Pa.

[0023] In order to solve the above technical problems, the present invention provides a high-purity quartz purification equipment, mixed acid, and purification process; the roasting furnace and reactor of the equipment both adopt a heating / catalytic method combining microwave and ultrasonic waves, and simultaneously have a heating and pressurizing effect, which can more thoroughly treat the quartz ore, effectively open fine inclusions, and fully separate / remove impurities under pressure, so as to obtain higher purity high-purity quartz while saving energy and improving efficiency; a large number of components of the mixed acid are replaced by organic acids with less harm and looser control, especially a large amount of hydrofluoric acid is replaced, which has a positive impact on environmental protection and safety, reduces production thresholds and costs, and effectively achieves the effect of acid leaching and impurity removal; the purification process greatly improves the efficiency and effect of quartz purification by improving the roasting and acid leaching and impurity removal processes, realizes the preparation of higher purity high-purity quartz, and breaks the blockade of high-purity quartz technology in Europe and the United States. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] Figure 1 This is a schematic diagram of the structure of an embodiment of a tubular roasting furnace for high-purity quartz purification equipment of the present invention;

[0025] Figure 2 for Figure 1 The schematic diagram of the principle of dumping ore during the water quenching process in the embodiment shown;

[0026] Figure 3 The present invention is a schematic diagram of the structure of a horizontal reactor of a high-purity quartz purification device. DETAILED DESCRIPTION

[0027] The present invention will be further described in detail below through specific implementation modes in conjunction with the accompanying drawings.

[0028] The invention discloses a high-purity quartz purification device, which comprises a tubular roasting furnace used in a roasting process and a horizontal reactor used in an acid leaching and impurity removal process.

[0029] In the prior art, roasting is usually heated by heating tubes or microwaves, but the treatment effect is not ideal. There are also additional steps to use ultrasonic treatment, but overall it is time-consuming and labor-intensive, and the effect improvement is not obvious. Figure 1 As shown, the present invention is a tubular roasting furnace of a high-purity quartz purification device, which includes a horizontally placed U-shaped quartz reaction tube body 1 and a sealing cover 2 for sealing the opening of the quartz reaction tube body 1. The quartz reaction tube body 1 and the sealing cover 2 are driven by a telescopic rod opening device 3 (cylinder telescopic rod, the extension body is connected to a positioning grab arm for connecting the sealing cover 2) to open or close the opening of the U-shaped quartz reaction tube body 1, so as to realize the processing process or pour out the heated ore for water quenching. 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 2. The sealing ring 14 made of graphite is not easy to age, is resistant to high temperatures, and has good sealing performance. An ultrasonic heating device 4 penetrating the main body of the quartz reaction tube 1 is arranged at the bottom of the U-shaped structure; a microwave heating device 5 radiating into the tube is arranged on the outer wall of the quartz reaction tube main body 1, and a microwave isolation layer is also arranged correspondingly to envelop the outer wall of the quartz reaction tube main body to prevent the aforementioned microwave from leaking; and an ore turning mechanism is also included for driving the processed ore in the quartz reaction tube main body 1 to turn over. By closing the quartz reaction tube main body 1, pressurization can be achieved, and the ultrasonic heating device 4 and the microwave heating device 5 have a superimposed effect, the heating time is shorter, and the opening of fine inclusions is promoted, and the subsequent water quenching and impurity removal effects are better.

[0030] When this patent is implemented, the main body 1 of the quartz reaction tube is cylindrical. Of course, it can be changed to non-cylindrical or other shapes in application, which is also feasible based on the principle of this patent, but the technical effect will be deteriorated.

[0031] Reference Figure 1 As shown, of course, in implementation, the cover opening device 3 can also be replaced by a hinge structure. Because of the high temperature and the need to quickly open the quenching water, in this case, a tool or an automatic opening device is required to open the sealing cover 2. The seal between the quartz reaction tube body 1 and the sealing cover 2 is preferably a double flange structure, which is conducive to sealing and extending the service life.

[0032] A variable frequency magnetron 5b (temperature control is achieved by frequency conversion) is arranged at the lower part of the quartz reaction tube body 1. The variable frequency magnetron 5b introduces microwaves into the inner cavity of the quartz reaction tube body 1 through a waveguide cavity 5a close to the outer wall of the quartz reaction tube body 1. A microwave isolation layer is also arranged to surround the outer wall of the quartz reaction tube body 1. The microwave isolation layer adopts a metal isolation cover 6 or a ferrite material to effectively isolate microwave leakage. During implementation, the lateral structure of the waveguide cavity 5a can be square; the distance between the waveguide cavity 5a and the metal isolation cover 6 and the quartz reaction tube body 1 is maintained at about 3-20 mm.

[0033] During implementation, the preferred distance between the waveguide cavity 5a and the quartz reaction tube body 1 is maintained at about 5 mm.

[0034] like Figure 1 As shown, an ultrasonic heating device 4 penetrating the main body of the quartz reaction tube 1 is arranged at the inner bottom of the U-shaped structure of the main body of the quartz reaction tube, an ultrasonic main unit 4a of the ultrasonic heating device 4 is arranged at the outer bottom of the main body of the quartz reaction tube 1, and an ultrasonic transducer 4b is located in the middle of the inner cavity of the main body of the quartz reaction tube, on the central axis of the U-shaped structure of the main body of the quartz reaction tube 1. The advantage of being arranged on the central axis as shown in the figure is that when the ore turning mechanism drives the main body of the quartz reaction tube 1 to rotate, the ultrasonic transducer 4b is always in the center position, reducing friction and collision with the ore.

[0035] like Figure 1 , Figure 2 As shown, when implemented, it also includes a tilting device 13 for pouring quartz out of the quartz reaction tube body 1 after calcination is completed. The aforementioned quartz reaction tube body 1 and accessories are all arranged on the tilting device 13 through the equipment bracket 11. One rotation pair of the tilting device 13 is fixed to the equipment bracket 11, and the other rotation pair is connected and fixed to the equipment base 12.

[0036] like Figure 1 As shown, the quartz reaction tube body 1 is provided with a rotation drive mechanism, and the quartz reaction tube body 1 is driven to rotate at a constant speed during use by a rotation drive motor 10. During implementation, if the quartz reaction tube body 1 is horizontal, a main shaft can be set to support the tail of the quartz reaction tube body 1, and a roller can be added to the opening of the quartz reaction tube body to lift it. The microwave isolation layer / metal isolation cover 6 can also be set as a supporting shell, and the quartz reaction tube body 1 is supported by a supporting mechanism to achieve rotation therein. It should be noted that if the quartz reaction tube body 1 adopts a rotating structure, then the telescopic rod cover opening device 3 connected to the sealing cover 2, its positioning gripping arm and the sealing cover 2 are directly in a movable relationship, that is, the telescopic rod cover opening device 3 only limits the sealing cover 2 and the quartz reaction tube body 1 to be tightly closed, but does not affect the rotation of the sealing cover 2.

[0037] like Figure 1As shown, outside the quartz reaction tube body, there are also multiple pipelines connected to the inner cavity of the quartz reaction tube body. The first pipeline is connected to the air pressure regulating mechanism 8 with a valve, and air can be injected into the quartz reaction tube body 1 or the air pressure in the quartz reaction tube body 1 can be adjusted through the air pressure regulating mechanism 8. The second pipeline is also provided with a valve, which connects the inner cavity of the quartz reaction tube body 1 with the feeding mechanism 9, and is used to input powder or particles into the inner cavity of the quartz reaction tube body 1. The third pipeline is not provided with a valve, which connects the inner cavity of the quartz reaction tube body 1 with the sensor unit 7, and the sensor unit 7 is provided with a safety valve (automatic pressure relief when the pressure is too high), a pressure gauge, a pressure sensor, etc. During implementation, the sensor unit 7 can also be provided with a temperature sensor, etc.

[0038] During implementation, a PLC is also provided to play a master control role, and the PLC controls the microwave heating device 5, the ultrasonic heating device 4 and the ore turning mechanism to work synchronously. The PLC also monitors the temperature, pressure, speed control and monitoring, temperature detection and control (by controlling the microwave power), the control of the telescopic rod opening device 3 (opening mechanism), and the control of the air pressure regulating mechanism to adjust the pressure of the inner cavity of the quartz reaction tube body as needed.

[0039] During implementation, the inner wall of the furnace of the quartz reaction tube body 1 can be made of high-purity quartz material, preferably high-purity zirconium quartz material (stronger), and the outer part can be made of the same material, or a composite structure of other thermal insulation materials can be used.

[0040] The sealing cover 2 is made of the same material as the inner wall of the reaction tube furnace. Alternatively, the inner wall may be made of the same material as the inner wall of the reaction tube furnace, and the outer part may be made of metal and / or other materials or thermal insulation materials.

[0041] During implementation, the ultrasonic transducer head 4b uses a zirconium transducer head, or covers a layer of high-purity quartz / high-purity zirconium quartz layer on the basis of PZT lead zirconate titanate piezoelectric ceramic material. Because the direct use of PZT lead zirconate titanate piezoelectric ceramics will be damaged by high temperature and high pressure and produce pollutants, a layer of high-purity quartz or high-purity zirconium quartz material layer can be compounded on its outside. The zirconium transducer head can realize automatic ultrasonic frequency tracking.

[0042] like Figure 1 , 2The preferred embodiment of a tubular roasting furnace for quartz impurity removal shown in the figure comprises 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.

[0043] In one embodiment, the tubular roasting furnace, 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.

[0044] When in use, the ore is placed in the equipment at room temperature, the pressure is manually released or the vacuum valve or air pressure regulating mechanism 8 is opened to adjust and restore the normal pressure, and the cover is opened at high temperature to pour out the material into water for quenching.

[0045] like Figure 3 As shown, the present invention is a high-purity quartz purification equipment, in which a horizontal reactor used for an acid leaching impurity removal process comprises: a horizontally placed U-shaped reactor body 101, and a quick-opening reactor cover 102 for closing the opening of the reactor body 101, an ultrasonic catalytic device 104 penetrating the reactor body is arranged at the bottom of the U-shaped structure of the reactor body 101; a microwave catalytic device 105 radiating into the tube is arranged on the outer wall of the reactor body 101; a corresponding metal isolation layer 106 is also arranged to envelop the outer wall of the reactor body to prevent the aforementioned microwave from leaking; and a rotating motor 110 is also included for driving the reactor body 101 to rotate.

[0046] During implementation, the horizontal reactor has an inner bottom edge of the horizontal reactor body 101 that is placed horizontally, and an angle of -5 to -15 degrees with the horizontal.

[0047] During implementation, the ultrasonic catalytic device 104 of the horizontal reactor 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.

[0048] During implementation, the inner wall of the reactor body 101 of the horizontal reactor and the inner wall of the quick-opening reactor 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.

[0049] During implementation, the microwave catalytic device 105 of the horizontal reactor 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.

[0050] During implementation, the horizontal reactor is also provided with a regulating mechanism 108 for regulating the air pressure in the reactor cavity, a liquid inlet mechanism 109 for inputting acid and water, a sensor unit 107 and an inlet and outlet ionized water mechanism 111; the inner cavity of the reactor body 101 is connected with the air pressure regulating mechanism 108, the liquid inlet mechanism 109 and the inlet and outlet ionized water mechanism 111 respectively through pipelines with valves; the inner cavity of the reactor 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; a PLC for monitoring and control is also provided, and the PLC also controls the microwave catalytic device 105, the ultrasonic catalytic device 104 and the rotating motor 110 to work synchronously, and the PLC also controls the microwave heating device 5, the ultrasonic heating device 4 and the rotating drive motor 10 to work synchronously.

[0051] When implementing, Figure 3 As shown, outside the reactor body 101, there are also multiple pipelines connected to the inner cavity of the reactor body 101, which are respectively connected to the safety valve, pressure gauge, pressure sensor (sensor unit 107), air pressure regulating mechanism 108, liquid inlet mechanism 109 (inlet acid and water), and deionized water inlet mechanism (ultrapure water resistivity of 10 megohms to 18.825 megohms is required for the final reactor cleaning). Of course, the pipelines are all independently provided with valves (sensor unit 107 may not be provided).

[0052] During implementation, a PLC with a general control function is also provided, through which the temperature, pressure, speed control and monitoring, temperature detection and control (by controlling the microwave power) and the air pressure regulating mechanism are controlled to adjust the pressure of the inner cavity of the reactor body 1 as needed.

[0053] When implemented Figure 3 As shown, the ore turning mechanism is a rotation driving mechanism of the reactor body 101, including a rotating motor 110, a transmission belt 112, and a driven disk 113 fixed at the tail of the reactor body 101; the rotating 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 113, thereby driving the ore processed in the reactor body 101 to turn over.

[0054] During implementation, the reactor body 101 and the quick-opening reactor cover 102 are connected by safety buckles or bolts 103 (such as Figure 3 ) is connected and fixed. It is convenient to form a closed space and take out the finished product after the reaction is completed.

[0055] During implementation, the exterior of the reactor body 101 may be made of the same material as the interior, or may be made of a heat-insulating material combined with the inner wall of the reactor, or may have other composite structures to increase strength.

[0056] During implementation, the quick-opening kettle cover 102 can be made of the same material as the inner wall of the reactor. Of course, the quick-opening kettle cover 102 can also be made of polyetheretherketone, polyimide or polytetrafluoroethylene, and the outer wall can also be made of insulation material or metal material, or the outer wall can be made of insulation material and metal material. The advantage of the metal material on the outer wall of the quick-opening kettle cover 102 is that it has sufficient supporting strength and can play a microwave shielding role. Further, in order to avoid metal corrosion, it is also possible to cover the metal with a layer of acid-resistant material.

[0057] The inner core of the ultrasonic transducer head 104c of the reactor can be made of PZT lead zirconate titanate piezoelectric ceramics, but the surface must be coated with anti-corrosion ceramics or polymer acid and alkali resistant materials to avoid being corroded by acid.

[0058] In one embodiment of a horizontal reactor, the reactor has a volume of 15L and a pressure of 3 MPa. The microwave catalytic mechanism 5 is powered by 220v±10v, 5000WV, 2450+50Hz, and the microwave leakage is controlled at <5mW / cm. The rotary drive motor 10 is a stepper motor controlled by PLC. The reaction temperature in the reactor body is between 60°C and 200°C. The wavelengths of ultrasound and microwave need to pass through quartz sand.

[0059] The present invention also discloses a high-purity quartz purification mixed acid, which is used in the high-purity quartz purification equipment as described above. The mixed acid is added to the horizontal reactor in the acid leaching and impurity removal process, and the mixed acid contains: water, oxalic acid, aminosulfonic acid, penetrant, citric acid and / or hydrochloric acid. The component can effectively remove / replace hydrofluoric acid and ensure the quartz purification effect.

[0060] During implementation, the concentration of the mixed acid is 25-35%, so that the acid has the best activity.

[0061] The penetrant is silicate or sodium oleate; these two components, when added in a mixed form, can produce a better superposition effect and ensure the acid leaching impurity removal effect.

[0062] The mixed acid also includes one or more of sulfuric acid, nitric acid, tartaric acid, fulvic acid, silicic acid, perchloric acid and benzoic acid. After adding, the effect of the mixed acid can be optimal.

[0063] The specific mixed ingredients can be:

[0064] Example 1: water, oxalic acid, aminosulfonic acid, penetrant, citric acid.

[0065] Example 2: water, oxalic acid, aminosulfonic acid, penetrant, hydrochloric acid.

[0066] Example 3: water, oxalic acid, aminosulfonic acid, osmotic agent, citric acid, hydrochloric acid.

[0067] Example 4: water, oxalic acid, aminosulfonic acid, osmotic agent, citric acid and / or hydrochloric acid, sulfuric acid.

[0068] Example 5: water, oxalic acid, aminosulfonic acid, osmotic agent, citric acid and / or hydrochloric acid, nitric acid.

[0069] Example 6: water, oxalic acid, aminosulfonic acid, osmotic agent, citric acid and / or hydrochloric acid, tartaric acid.

[0070] Example 7: water, oxalic acid, aminosulfonic acid, osmotic agent, citric acid and / or hydrochloric acid, tartaric acid, nitric acid.

[0071] Example 8: water, oxalic acid, aminosulfonic acid, osmotic agent, citric acid and / or hydrochloric acid, tartaric acid, fulvic acid.

[0072] Example 9: water, oxalic acid, aminosulfonic acid, osmotic agent, citric acid and / or hydrochloric acid, fulvic acid.

[0073] Example 10: water, oxalic acid, aminosulfonic acid, osmotic agent, citric acid and / or hydrochloric acid, fulvic acid, sulfuric acid.

[0074] Example 11: water, oxalic acid, aminosulfonic acid, osmotic agent, citric acid and / or hydrochloric acid, perchloric acid, sulfuric acid.

[0075] Example 12: water, oxalic acid, aminosulfonic acid, osmotic agent, citric acid and / or hydrochloric acid, perchloric acid.

[0076] Example 13: water, oxalic acid, aminosulfonic acid, osmotic agent, citric acid and / or hydrochloric acid, benzoic acid.

[0077] Example 14: water, oxalic acid, aminosulfonic acid, osmotic agent, citric acid and / or hydrochloric acid, sulfuric acid, nitric acid.

[0078] Example 15: water, oxalic acid, aminosulfonic acid, osmotic agent, citric acid and / or hydrochloric acid, fulvic acid, benzoic acid.

[0079] Example 16: water, oxalic acid, aminosulfonic acid, osmotic agent, citric acid and / or hydrochloric acid, perchloric acid, benzoic acid.

[0080] Example 17: Water, oxalic acid, aminosulfonic acid, osmotic agent, citric acid and / or hydrochloric acid, tartaric acid, sulfuric acid, benzoic acid.

[0081] Example 18: water, oxalic acid, aminosulfonic acid, penetrant, citric acid and / or hydrochloric acid, silicic acid, perchloric acid, benzoic acid.

[0082] Example 19: water, oxalic acid, aminosulfonic acid, penetrant, citric acid and / or hydrochloric acid, silicic acid, sulfuric acid, benzoic acid.

[0083] Example 20: water, oxalic acid, aminosulfonic acid, osmotic agent, citric acid and / or hydrochloric acid, sulfuric acid, nitric acid, tartaric acid, silicic acid, benzoic acid.

[0084] Example 21: Water, oxalic acid, aminosulfonic acid, osmotic agent, citric acid and / or hydrochloric acid, sulfuric acid, tartaric acid, silicic acid, benzoic acid.

[0085] Of course, during implementation, a small amount of hydrofluoric acid can also be added to the mixed acid of the present invention to improve the effect. However, compared with the traditional mixed acid formula, the amount of hydrofluoric acid used can be greatly reduced under the same effect.

[0086] During implementation, preferably, specifically, the molar ratio of each component in the mixed acid is: 1-7 of oxalic acid, 3-10 of aminosulfonic acid, 1-5 of penetrant, 1-5 of citric acid or hydrochloric acid, and 2-8 of other acids.

[0087] In the above-mentioned various implementations, the concentration of the mixed acid is finally controlled to be 25-35% by mixing with water, so that the acid has the best activity.

[0088] The following is a comparison of the application of the mixed acid of the present invention and the traditional mixed acid with hydrofluoric acid:

[0089] (1) Old formula (containing hydrofluoric acid): The SiO2 content of the raw ore is 99.8%. After roasting, it is sequentially quenched by water, ground, classified, and iron removed by high gradient. After the acid leaching and impurity removal is heated for 48 hours, it is sequentially washed, floated, dried, color sorted, and chlorinated to remove impurities. The SiO2 content of the finished product is 99.99%.

[0090] (2) The new formula of the present invention: the SiO2 content of the raw ore is 99.8%. After roasting, water quenching, grinding, classification, high gradient iron removal are carried out in sequence. After the acid leaching and impurity removal agent is heated for 48 hours, washing, flotation, drying, color sorting, and chlorination impurity removal are carried out in sequence. The SiO2 content of the finished product is 99.89%. It can be seen that the mixed acid of the present invention basically achieves the impurity removal effect of the traditional formula.

[0091] (3) In the test process, the SiO2 content of the raw ore was 99.8%. After roasting, it was water quenched, ground, classified, and iron removed at a high gradient. Then, it was placed in a horizontal reactor of a high-purity quartz purification device of the present invention, and microwave and ultrasonic waves were used for synchronous catalysis and pressurization to 3 Pa. After the heating agent reacted for 48 hours, it was washed, floated, dried, color sorted, and chlorinated to remove impurities. The SiO2 content of the finished product was 99.994%. It can be seen that the impurity removal effect of the mixed acid combined with the equipment of the present invention is better than that of the traditional formula and equipment.

[0092] (4) If, on the basis of (3), the calcination is also carried out in the tubular calcination furnace of a high-purity quartz purification equipment of the present invention (combined with the process described below), then the SiO2 content of the final product can reach 99.9998%.

[0093] The present invention also discloses a high-purity quartz purification process, in which the high-purity quartz purification equipment and high-purity quartz purification mixed acid as described above are used; the process is based on the traditional process:

[0094] In the roasting stage, the quartz ore is put into the tubular roasting furnace, and microwave and ultrasonic waves are used for simultaneous heating. 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. The ore is kept turned. The power ratio of microwave heating and ultrasonic heating is maintained at 1:1 to 5:1.

[0095] After roasting, the quartz ore is sequentially subjected to water quenching, grinding, grading, and high-gradient iron removal, and then enters the acid leaching and impurity removal process; in this process, the ore is transferred to the horizontal reactor and the mixed acid is added; in the acid leaching and impurity removal process, microwave and ultrasonic waves are used for simultaneous catalysis, the temperature is controlled at 60-80 degrees Celsius, the process is carried out in a closed cavity, and the ore is kept rolling, and the pressure in the cavity 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.

[0096] During roasting, microwave and ultrasonic superposition can effectively achieve 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 traditional processes, the present invention removes / classifies impurities more thoroughly, effectively reduces reaction time, significantly reduces energy consumption, reduces process flow, improves efficiency, is low-carbon and environmentally friendly, and is more conducive to the effect of subsequent process treatment; on this basis, the quartz ore obtained can basically remove impurities through traditional acid leaching impurity removal process, and obtain ultra-high purity quartz of more than 99.995%. The acid leaching impurity removal process uses microwaves and ultrasonic waves to catalyze and pressurize simultaneously, so that the agent can play a more full role, and the ultrasonic wave 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 ultrasonic waves, achieving a better and more thorough reaction removal effect. Compared with traditional processes, the present invention can further reduce reaction time, significantly reduce energy consumption, and improve impurity removal effect. In the traditional quartz purification process, the roasting is replaced by the above-mentioned roasting scheme, and the acid leaching and impurity removal scheme of the present invention is used, so that the final production of ultra-pure quartz of more than 99.999% can be achieved.

[0097] 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.

[0098] 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.

[0099] 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.

[0100] 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.

[0101] 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.

[0102] 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.

[0103] 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.

[0104] 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.

[0105] 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.

[0106] 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.

[0107] 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.

[0108] 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.

[0109] 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.

[0110] 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.

[0111] 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.

[0112] Based on the mixed acid and process of a high-purity quartz purification 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.

[0113] Through the technology of the present invention, 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.

[0114] This patent application has better use effect and energy efficiency. The principle is that on the basis of traditional technology, quartz ore is heated and pressurized simultaneously by microwaves and ultrasound during the roasting stage, which effectively improves the processing efficiency of quartz ore. The superposition of microwaves and ultrasound can effectively achieve penetration treatment of fine inclusions, so that they can be fully opened during subsequent water quenching. Compared with traditional processes, the impurity removal / classification of the present invention is more thorough, the reaction time is effectively reduced, the energy consumption is significantly reduced, the process flow is reduced, the efficiency is improved, low-carbon and environmentally friendly, and it is more conducive to the effect of subsequent process treatment.

Claims

1. A high-purity quartz purification equipment, comprising a tubular roasting furnace for a roasting process and a horizontal reactor for an acid leaching impurity removal process, characterized in that: The tubular roasting furnace comprises: a U-shaped quartz reaction tube body (1), and a sealing cover (2) for sealing the opening of the quartz reaction tube body; an ultrasonic heating device (4) penetrating the body is arranged at the bottom of the U-shaped structure of the quartz reaction tube body (1); a microwave heating device (5) radiating into the tube is arranged on the outer wall of the quartz reaction tube body (1), and a metal isolation cover (6) is also arranged to envelop the outer wall of the quartz reaction tube body to prevent the microwave from leaking; and a rotary drive motor (10) is also provided to drive the quartz reaction tube body (1) to rotate; The horizontal reactor comprises: a horizontally placed U-shaped reactor body (101), and a quick-opening lid (102) for closing the opening of the reactor body (101); an ultrasonic catalytic device (104) penetrating the reactor body is arranged at the bottom of the U-shaped structure of the reactor body (101); a microwave catalytic device (105) radiating into the tube is arranged on the outer wall of the reactor body (101); a corresponding metal isolation layer (106) is also arranged to envelop the outer wall of the reactor body to prevent the microwave from leaking; and a rotating motor (110) is also provided to drive the reactor body (101) to rotate.

2. The high-purity quartz purification equipment according to claim 1, characterized in that: The tubular roasting furnace: the quartz reaction tube body (1) is horizontally arranged, and also includes an equipment support (11), a tilting device (13) arranged at the bottom of the equipment support (11) and an equipment base (12); all components of the tubular roasting furnace for quartz impurity removal are arranged on the equipment support (11); the tilting device (13) is used to rotate and drive one end of the equipment support (11) to separate from the equipment base (12), so that the quartz reaction tube body (1) is tilted to pour out the ore in the tube; the horizontal reactor: the bottom edge of the horizontal reactor body (101) is at an angle of -5 to -15 degrees with the horizontal.

3. The high-purity quartz purification equipment according to claim 1, characterized in that: The ultrasonic heating device (4) of the tubular roasting furnace comprises an ultrasonic main unit (4a) and an ultrasonic transducer head (4b), wherein the ultrasonic main unit (4a) is arranged outside the quartz reaction tube body (1), and the ultrasonic transducer head (4b) penetrates the bottom center of the U-shaped structure of the quartz reaction tube body (1) and is arranged on the central axis of the inner cavity tube body of the quartz reaction tube body (1); the ultrasonic catalytic device (104) of the horizontal reactor comprises an ultrasonic main unit (104a), an ultrasonic transducer head (104b) and a transducer head anti-corrosion layer (104c), wherein the ultrasonic main unit (104a) is arranged outside 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).

4. The high-purity quartz purification equipment according to claim 3, characterized in that: The inner cavity wall formed by the quartz reaction tube body (1) and the sealing cover (2) of the tubular roasting furnace is made of high-purity zircon quartz material; the ultrasonic transducer head (4b) adopts a zirconium transducer head or is covered with a layer of high-purity quartz / high-purity zircon quartz layer on the basis of PZT lead zirconate titanate piezoelectric ceramic material; the inner cavity wall of the reactor body (101) of the horizontal reactor and the inner wall of the quick-opening reactor cover (102) are made of polymer acid and alkali resistant material; 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.

5. The high-purity quartz purification equipment according to any one of claims 1 to 4, characterized in that: The microwave heating device (5) of the tubular roasting furnace comprises a microwave variable frequency power supply (5c), a variable frequency magnetron (5b) and a waveguide cavity (5a), wherein the waveguide cavity (5a) is close to the outer wall of the quartz reaction tube body (1) to introduce microwaves into the inner cavity of the quartz reaction tube (1); the microwave catalytic device (105) of the horizontal reactor comprises a microwave variable frequency power supply (105c), a variable frequency magnetron (105b) and a waveguide cavity (105a), wherein the waveguide cavity (105a) is close to the outer wall of the reactor body (101) to introduce microwaves into the inner cavity of the reactor body (101).

6. The high-purity quartz purification equipment according to any one of claims 1 to 4, characterized in that: The tubular roasting furnace is also provided with a gas pressure regulating mechanism (8), a feeding mechanism (9) and a sensor unit (7); the inner cavity of the quartz reaction tube body (1) is communicated with the gas pressure regulating mechanism (8) and the feeding mechanism (9) respectively through pipelines with valves; the inner cavity of the quartz reaction tube body (1) is also communicated with the sensor unit (7) through pipelines; the sensor unit (7) is provided with a safety valve, a pressure gauge and a pressure sensor; the horizontal reactor is also provided with a regulating mechanism (108) for regulating the gas pressure in the reactor cavity, a liquid inlet mechanism (109) for inputting acid and water, a sensor unit (107) and a deionized water inlet mechanism (111); the reactor The inner cavity of the main body (101) is connected to the air pressure regulating mechanism (108), the liquid inlet mechanism (109), and the deionized water inlet mechanism (111) through pipelines with valves. The inner cavity of the reactor main body (101) is also connected to the sensor unit (107) through pipelines. The sensor unit (107) is provided with a safety valve, a pressure gauge, and a pressure sensor. A PLC for monitoring and controlling is also provided. The PLC controls the microwave catalytic device (105), the ultrasonic catalytic device (104), and the rotating motor (110) to work synchronously. The PLC controls the microwave heating device (5), the ultrasonic heating device (4), and the rotating drive motor (10) to work synchronously.

7. A high-purity quartz purification mixed acid, characterized in that: Used in the high-purity quartz purification equipment as described in any one of claims 1 to 6, the mixed acid is added to the horizontal reactor during the acid leaching and impurity removal process, and the components of the mixed acid include: water, oxalic acid, aminosulfonic acid, penetrant, citric acid and / or hydrochloric acid.

8. The high-purity quartz purification mixed acid according to claim 7, characterized in that: The concentration of the mixed acid is 25-35%, and the penetrant is silicate or sodium oleate; its components also include: one or more of sulfuric acid, nitric acid, tartaric acid, fulvic acid, silicic acid, perchloric acid, benzoic acid, and hydrofluoric acid.

9. A high-purity quartz purification process, characterized in that: The process uses the high-purity quartz purification equipment as described in any one of claims 1 to 6 and the high-purity quartz purification mixed acid as described in claims 7 to 8; the process is based on the traditional process: In the roasting stage, the quartz ore is put into the tubular roasting furnace, and microwave and ultrasonic waves are used for simultaneous heating. 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. The ore is kept turned. The power ratio of microwave heating and ultrasonic heating is maintained at 1:1 to 5:

1. After roasting, the quartz ore is sequentially subjected to water quenching, grinding, grading, and high-gradient iron removal, and then enters the acid leaching and impurity removal process; in this process, the ore is transferred to the horizontal reactor and the mixed acid is added; in the acid leaching and impurity removal process, microwave and ultrasonic waves are used for simultaneous catalysis, the temperature is controlled at 60-80 degrees Celsius, the process is carried out in a closed cavity, and the ore is kept rolling, and the pressure in the cavity 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.

10. The high-purity quartz purification process according to claim 9, characterized in that: The particle size of the quartz ore to be roasted is maintained at 0.5-3 cm in diameter; the quartz ore is ground to a particle size of 40-160 mesh in the grinding stage; and the pressure in the chamber of the acid leaching and impurity removal process is controlled at 1-5 Pa.

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