Horizontal reaction kettle for quartz impurity removal

Abstract

The utility model discloses a horizontal reaction kettle for quartz impurity removal, which is used for quartz purification and comprises a transverse U-shaped reaction kettle main body and a quick-opening kettle cover for closing an opening of the reaction kettle main body, and an ultrasonic catalysis device penetrating through the reaction kettle main body is arranged at the bottom in the U-shaped structure of the reaction kettle main body; the outer wall of the reaction kettle main body is provided with a microwave catalysis device radiating towards the inside of the pipe; a microwave isolating layer for enveloping the outer wall of the reaction kettle main body and preventing the microwaves from leaking is also correspondingly arranged; the ore stirring mechanism is used for driving ore processed in the reaction kettle main body to be stirred. According to the invention, microwave and ultrasonic waves are integrated, so that the reaction time can be reduced, the energy consumption is obviously reduced and the impurity removal effect is improved during equipment use.

Description

TECHNICAL FIELD

[0001] The utility model relates to a chemical reaction kettle for complexation extraction reaction (acid pickling impurity removal), especially relates to a horizontal reaction kettle for quartz impurity removal. BACKGROUND

[0002] High-purity quartz has excellent chemical stability, extremely low volume expansion coefficient, extremely high temperature resistance, high insulation withstand voltage, low and stable ultrasonic delay performance, mechanical performance higher than ordinary glass, ultraviolet spectrum performance, and visible light and near-infrared spectrum performance due to its unique molecular chain structure, lattice shape and lattice change rule.

[0003] Chip manufacturing links mainly include silicon wafer manufacturing, wafer manufacturing and chip manufacturing. High-purity quartz materials used in each process mainly include quartz crucibles for drawing single crystal silicon rods in the silicon wafer manufacturing link, quartz glass diffusion tubes and supporting quartz flanges, quartz glass furnace tubes, quartz boats and other quartz glass appliances in the wafer manufacturing link, and photomask substrates used in photolithography, etching and thin film deposition in the chip manufacturing link. Different quartz products have different requirements for the purity, inclusion content and particle size of high-purity quartz sand, among which the high-purity quartz crucible for drawing single crystal silicon has the most stringent requirements.

[0004] In recent years, China's photovoltaic and semiconductor industries have developed rapidly, and high-purity quartz consumption is huge. At present, due to the double barriers of high-quality and stable mineral source supply and purification process, it is urgent to improve the quartz purification process and break through the limitation of high-purity quartz raw material mines. Utility model content

[0005] The main technical problem to be solved by the utility model is to provide a horizontal reaction kettle for quartz impurity removal, which is used for acid pickling process for quartz impurity removal and can significantly reduce energy consumption and improve impurity removal effect.

[0006] To solve the above technical problems, the utility model provides a horizontal reaction kettle for quartz impurity removal, which comprises a horizontally arranged U-shaped reaction kettle body and a quick-opening kettle cover for closing the opening of the reaction kettle body. An ultrasonic wave catalytic device is arranged at the bottom of the U-shaped structure of the reaction kettle body and penetrates the body. A microwave catalytic device is arranged on the outer wall of the reaction kettle body and radiates into the pipe. A microwave isolation layer is also arranged on the outer wall of the reaction kettle body to prevent microwave leakage. A mineral turning mechanism is also provided to turn the ore processed in the reaction kettle body. The reaction kettle forms a sealed space, and the ore in the reaction kettle is heated and catalyzed by the microwave catalytic device and the ultrasonic wave catalytic device at the same time, which effectively promotes the efficiency and effect of acid pickling impurity removal. The closed space forms a closed pressure space, which further improves the effect.

[0007] In one embodiment, the horizontal reactor body has an inner bottom edge at an angle of -5 degrees to -15 degrees with the horizontal. This facilitates cleaning of the reactor after use. The angled cleaning liquid can flow out by itself.

[0008] In implementation, there are three methods to achieve the angle; 1. The reactor body has a U-shaped structure with two side edges at an angle of 10-30 degrees, and the central axis of the inner cavity tube of the reactor body is located on the horizontal plane; 2. The reactor body has a U-shaped structure with two side edges parallel to each other, and the central axis of the inner cavity tube of the reactor body is at an angle of -5 degrees to -15 degrees with the horizontal plane; 3. The reactor body 1 can also be provided with an inclination mechanism, which drives the reactor body 1 to be inclined at an angle of -5 degrees to -15 degrees with the horizontal during the cleaning stage (the conventional acid leaching stage maintains the horizontal state).

[0009] In one embodiment, the ultrasonic catalytic device includes an ultrasonic host, an ultrasonic transducer head, and an anti-corrosion layer of the transducer head. The ultrasonic host is arranged outside the reactor body, and the ultrasonic transducer head penetrates the center of the bottom of the U-shaped structure of the reactor body and is arranged on the central axis of the inner cavity tube of the reactor body. This arrangement ensures that the ultrasonic catalytic device is always located in the center during use, is not easily affected by the ore mode, and is uniformly and effectively heated / catalyzed.

[0010] In one embodiment, the inner cavity wall of the reactor body and the inner wall of the quick-opening cover are made of high-molecular acid and alkali resistant material; the anti-corrosion layer is a protective layer of anti-corrosion ceramic or high-molecular acid and alkali resistant material on the surface of the ultrasonic transducer head; the high-molecular acid and alkali resistant material can be polyether ether ketone, polyimide, or polytetrafluoroethylene.

[0011] In one embodiment, the microwave catalytic device includes a microwave frequency conversion power supply, a frequency conversion magnetron, and a waveguide cavity. The waveguide cavity is close to the outer wall of the reactor body to guide the microwave into the inner cavity of the reactor body. The waveguide cavity penetrates the microwave isolation layer and is close to the reactor body.

[0012] In one embodiment, the outer wall of the reactor body has a cylindrical profile, and the microwave isolation layer is a cylindrical metal isolation cover. The metal isolation cover and the waveguide cavity are both spaced apart from the outer wall of the reactor body by a distance of 3-20 millimeters.

[0013] Preferably, the waveguide cavity is spaced apart from the outer wall of the reactor body by a distance of 5 millimeters. The waveguide cavity can have a square transverse structure.

[0014] In one embodiment, the ore stirring mechanism is a rotating drive mechanism of the reactor body, which includes a rotating drive motor, a transmission belt, and a driven disc fixed to the tail of the reactor body. The rotating drive motor rotates at a constant speed and drives the reactor body to rotate at a constant speed through the transmission belt and the driven disc, thereby driving the ore processed in the reactor body to stir.

[0015] In one embodiment, an adjusting mechanism for adjusting the air pressure in the cavity of the reaction kettle, a liquid inlet mechanism for inputting acid liquid and water, a sensor unit and a deionized water inlet mechanism are further provided; the inner cavity of the reaction kettle body is in communication with the air pressure adjusting mechanism, the liquid inlet mechanism and the deionized water inlet mechanism through pipelines with valves respectively; the inner cavity of the reaction kettle body is also in communication with the sensor unit through a pipeline, and the sensor unit is provided with a safety valve, a pressure gauge and a pressure sensor.

[0016] The deionized water inlet mechanism is used in the final cleaning stage and introduces super-pure water with a high electrical resistivity of 10-18.825 mega ohms to the reaction kettle body.

[0017] In one embodiment, a PLC for monitoring and control is further provided, which controls the synchronous operation of the microwave catalytic device, the ultrasonic catalytic device and the ore tumbling mechanism, and controls the air pressure adjusting mechanism to adjust the pressure in the inner cavity of the reaction kettle body as required.

[0018] The microwave isolation layer can effectively isolate microwave leakage by using a metal isolation cover or ferrite material.

[0019] The utility model discloses a horizontal reaction kettle for quartz impurity removal, which comprises a horizontally arranged U-shaped reaction kettle body and a quick-opening kettle cover for closing the opening of the reaction kettle body, an ultrasonic catalytic device is arranged at the bottom of the U-shaped structure of the reaction kettle body and penetrates the body, a microwave catalytic device is arranged on the outer wall of the reaction kettle body and radiates into the pipe, a microwave isolation layer is arranged on the outer wall of the reaction kettle body to prevent microwave leakage, and an ore tumbling mechanism is arranged to drive the ore in the reaction kettle body to tumble. The reaction kettle forms a sealed space, and the ore in the reaction kettle is heated and catalyzed by the microwave catalytic device and the ultrasonic catalytic device, which effectively improves the efficiency and effect of acid leaching impurity removal. The sealed space forms a sealed pressure space, which further improves the effect. The patent combines microwave and ultrasonic waves, which can reduce the reaction time, significantly reduce energy consumption and improve the impurity removal effect. BRIEF DESCRIPTION OF DRAWINGS

[0020] Figure 1 The structure of one embodiment of the utility model is shown in the figure. DETAILED DESCRIPTION

[0021] The utility model will be further described in detail by specific implementation and the drawings.

[0022] The existing reaction kettle is usually heated / catalyzed by a heating pipe or microwave, and the treatment effect is not ideal. Some existing reaction kettles add an ultrasonic wave to perform auxiliary treatment, but the whole process is time-consuming and laborious, and the impurity removal effect is not obvious.

[0023] Please refer to Figure 1 The structure diagram of one embodiment of a horizontal reaction kettle for quartz impurity removal. It includes a horizontally placed U-shaped reaction kettle body 1 and a quick-opening kettle cover 2 for closing the opening of the reaction kettle body 1. The reaction kettle body 1 and the quick-opening kettle cover 2 are detachably connected by safety buckles (or bolts 3). An acid and alkali resistant high polymer sealing ring 14 is arranged on the contact surface of the reaction kettle body 1 and the quick-opening kettle cover 2 to ensure airtightness.

[0024] When implemented, as shown in Figure 1 A frequency conversion magnetron 5b (temperature control is achieved by frequency conversion) for generating microwaves is arranged at the lower part of the reaction kettle body. The frequency conversion magnetron 5a guides the microwaves into the inner cavity of the reaction kettle body 1 through a waveguide cavity 5a close to the outer wall of the reaction kettle. A microwave isolation layer 6 surrounding the outer wall of the reaction kettle body 1 is also arranged. The microwave isolation layer 6 can effectively isolate microwave leakage by using a metal isolation cover or ferrite material. When implemented, the waveguide cavity 5a can adopt a square transverse structure. The distance between the waveguide cavity 5a and the reaction kettle is maintained at about 5mm.

[0025] When implemented, when the reaction kettle body 1 is in a horizontal position, rollers can be arranged at the opening part of the reaction kettle body 1 for lifting. The microwave isolation layer / metal isolation cover 6 can also be arranged as a support shell to support the reaction kettle body 1 through a supporting mechanism to realize rotation in it.

[0026] When implemented, as shown in Figure 1 An ultrasonic device (ultrasonic catalytic device 4) penetrating the body of the reaction kettle body 1 U-shaped body is arranged at the bottom of the reaction kettle body 1 U-shaped body. The main body of the ultrasonic device (ultrasonic main machine 4a) is arranged at the outer bottom of the U-shaped body of the reaction kettle body 1, and the ultrasonic transducer head 4b is located at the middle part of the inner cavity of the reaction kettle body 1.

[0027] The patent can realize pressurization by closing the reaction kettle body 1. The microwave catalytic device 5 and the ultrasonic catalytic device 4 are superimposed to realize shorter heating and catalysis time, promote the acid liquid to fully enter the cracks of the ore, promote the opening and sufficient reaction of the fine inclusions, and greatly improve the impurity removal effect.

[0028] When the patent is implemented, the quartz reaction tube body 1 is cylindrical. Of course, in application, it can be changed to non-cylindrical and other shapes, which are also feasible on the basis of the principle of the patent, but the technical effect is worse.

[0029] When implemented, as shown in Figure 1 The reaction kettle body 1 is also provided with a rotary drive mechanism. The reaction kettle body 1 is driven by a rotary drive motor 10 to rotate at a uniform speed in use. Thus, the ore in the acid leaching reaction is kept continuously tumbling to promote the reaction. The rotation of the reaction kettle body 1 replaces the traditional stirring of acid leaching, avoiding the influence of stirring instruments on the purity of quartz sand.

[0030] In practice, as shown in the figure, outside the reactor body 1, a plurality of pipelines are also provided, which are connected to the inner cavity of the reactor body 1, and these pipelines are respectively connected to a safety valve, a pressure gauge, a pressure sensor (sensor unit 7), a gas pressure regulating mechanism 8, a liquid inlet mechanism 9 (acid liquid and water), and a deionized water inlet mechanism (final reactor cleaning, requiring ultrapure water with a resistance of 10-18.825 megaohms). Of course, the pipelines are each independently provided with a valve. Figure 1

[0031] In practice, a PLC is also provided, which has a total control function, and through the PLC, temperature, pressure, and rotating speed control and monitoring, temperature detection and control (through microwave power control), and control of the gas pressure regulating mechanism to adjust the pressure in the inner cavity of the reactor body 1 according to needs are monitored and controlled.

[0032] In practice, the ore stirring mechanism is a rotating drive mechanism of the reactor body 1, which includes a rotating drive motor 10, a transmission belt 12, and a driven disc 13 fixed at the tail of the reactor body; the rotating drive motor 10 rotates at a constant speed and drives the reactor body 1 to rotate at a constant speed through the transmission belt 12 and the driven disc 13, thereby driving the ore processed in the reactor body 1 to stir.

[0033] In practice, the reactor body 1 and the quick-opening cover 2 are connected and fixed by safety buckles or bolts 3 (as shown in the figure). Figure 1 This facilitates the formation of a sealed space and the removal of finished products after the reaction is completed.

[0034] In practice, the inner wall of the reactor and the quick-opening cover 2 are made of high-molecular high-temperature-resistant (200-300℃) materials, such as polyether ether ketone (PEEK); in addition, polyimide and polytetrafluoroethylene materials can also be used.

[0035] In practice, the outer part of the reactor body 1 can be made of the same material as the inner part, or heat-insulating materials can be combined with the inner wall of the reactor, or other composite structures can be used to increase strength.

[0036] In practice, the quick-opening cover 2 can be made of the same material as the inner wall of the reactor. Of course, the quick-opening cover 2 can also be made of polyether ether ketone, polyimide, or polytetrafluoroethylene materials on the inner wall, and heat-insulating materials or metal materials on the outer part, or heat-insulating materials and metal materials combined on the outer part. The outer wall of the quick-opening cover 2 with metal material has the advantages of sufficient support strength and microwave shielding effect. Further, to avoid metal corrosion, a layer of acid-resistant material can also be covered on the metal.

[0037] The inner core of the ultrasonic transducer head can be made of PZT lead zirconate titanate piezoelectric ceramic. However, the surface must be coated with corrosion-resistant ceramic or high-molecular acid-resistant material to avoid corrosion by acid liquid.

[0038] ​A horizontal reaction kettle for quartz impurity removal, in one embodiment, the reaction kettle volume is 15L, the use pressure is 3MPa, the power supply of the microwave catalytic mechanism 5 adopts 220v±10v, the power is 5000WV, the frequency is 2450+50Hz, the microwave leakage control is <5mW / cm. The rotary drive motor 10 adopts a stepping motor, controlled by a PLC, the reaction temperature in the reaction kettle main body is 60-200℃, and the wavelengths of the ultrasonic wave and the microwave need to pass through the quartz sand.

[0039] The patent application has better use effect and energy efficiency. The principle is that on the basis of the traditional process, the quartz ore is catalyzed and heated by microwave and ultrasonic wave simultaneously in the acid leaching impurity removal stage, the pressure is increased, the acid washing treatment efficiency of the quartz ore is effectively improved, the penetration treatment of the micro-inclusion is effectively realized by the superposition of the microwave and ultrasonic wave, the acid liquid is promoted to enter the gap, the impurities are fully reacted and removed, compared with the traditional process, the impurity removal is more thorough, the reaction time is effectively reduced, the energy consumption is significantly reduced, the process flow is reduced, the efficiency is improved, it is low-carbon and environmentally friendly, and higher-purity quartz can be obtained.

Claims

1. A horizontal reaction kettle for removing impurities from quartz, characterized in that, It includes transverse U-shaped reaction kettle body (1), and the quick open kettle cover (2) for closing the opening of the reaction kettle body (1), the ultrasonic catalytic device (4) is arranged in the U-shaped structure of the reaction kettle body (1) and the bottom of the reaction kettle body (1) is penetrated, the microwave catalytic device (5) is arranged on the outer wall of the reaction kettle body (1) and the microwave is radiated into the pipe, the microwave isolation layer is correspondingly arranged on the outer wall of the reaction kettle body (1) to prevent the leakage of the microwave, and the ore turning mechanism for driving the ore in the reaction kettle body (1) to turn is further included.

2. The horizontal reaction vessel for the removal of impurities from quartz as claimed in claim 1, wherein, The inner bottom edge of the transverse reaction kettle body (1) is at an angle of -5 degrees to -15 degrees with the horizontal.

3. The horizontal reaction vessel for the removal of impurities from quartz as claimed in claim 2, wherein The angle between the two side edges of the U-shaped reaction kettle body (1) is 10-30 degrees, and the central axis of the inner cavity tube of the reaction kettle body (1) is located on the horizontal plane; or the two side edges of the U-shaped reaction kettle body (1) are parallel, and the central axis of the inner cavity tube of the reaction kettle body (1) is at an angle of -5 degrees to -15 degrees with the horizontal plane; or the reaction kettle body (1) is further provided with an inclination mechanism, and the reaction kettle body (1) is driven to be inclined from the horizontal to an angle of -5 degrees to -15 degrees with the horizontal.

4. The horizontal reaction vessel for removing impurities from quartz according to claim 1 or 2, wherein The ultrasonic catalytic device (4) includes an ultrasonic host (4a), an ultrasonic transducer head (4b) and an anti-corrosion layer (4c) of the transducer head, the ultrasonic host (4a) is arranged outside the reaction kettle body (1), the ultrasonic transducer head (4b) penetrates the center of the bottom of the U-shaped structure of the reaction kettle body (1) and is arranged on the central axis of the inner cavity tube of the reaction kettle body (1).

5. The horizontal reaction vessel for the removal of impurities from quartz as claimed in claim 4, wherein The inner cavity wall of the reaction kettle body (1) and the inner wall of the quick open kettle cover (2) are made of high molecular acid and alkali resistant material; the anti-corrosion layer (4c) is an anti-corrosion ceramic protective layer or a high molecular acid and alkali resistant material protective layer on the surface of the ultrasonic transducer head (4b); the high molecular acid and alkali resistant material is polyether ether ketone, polyimide or polytetrafluoroethylene.

6. The horizontal reaction vessel for the removal of impurities from quartz as claimed in claim 3 wherein, The microwave catalytic device (5) includes a microwave frequency conversion power supply (5c), a frequency conversion magnetron (5b) and a waveguide cavity (5a), the waveguide cavity (5a) is close to the outer wall of the reaction kettle body (1) and guides the microwave into the inner cavity of the reaction kettle body (1).

7. The horizontal reaction vessel for the removal of impurities from quartz as claimed in claim 6 wherein, The outer wall of the reaction kettle body (1) is in a cylindrical contour, the microwave isolation layer is a cylindrical metal isolation cover (6), and the metal isolation cover (6) and the waveguide cavity (5a) are both kept at a distance of 3-20 mm from the outer wall of the reaction kettle body (1).

8. The horizontal reaction vessel for the removal of impurities from quartz as claimed in claim 1 or 2, wherein The ore turning mechanism is a rotation driving mechanism of the reaction kettle body (1), which includes a rotation driving motor (10), a transmission belt (12) and a driven disc (13) fixed at the tail of the reaction kettle body (1); the rotation driving motor (10) rotates at a constant speed and drives the reaction kettle body (1) to rotate at a constant speed through the transmission belt (12) and the driven disc (13), so as to drive the ore processed in the reaction kettle body (1) to turn.

9. The horizontal reaction vessel for the removal of impurities from quartz as claimed in claim 1 or 2, wherein There are also provided a regulating mechanism (8) for regulating the air pressure in the cavity of the reaction kettle, a liquid inlet mechanism (9) for inputting acid liquid and water, a sensor unit (7), and a deionized water inlet mechanism (11); the cavity of the reaction kettle body (1) is respectively communicated with the air pressure regulating mechanism (8), the liquid inlet mechanism (9), and the deionized water inlet mechanism (11) through pipes provided with valves; the cavity of the reaction kettle body (1) is also communicated with the sensor unit (7) through a pipe, and the sensor unit (7) is provided with a safety valve, a pressure gauge, and a pressure sensor.

10. The horizontal reaction vessel for the removal of impurities from quartz as claimed in claim 1 or 2, wherein There is also provided a PLC for monitoring and control, which also controls the microwave catalytic device (5), the ultrasonic catalytic device (4), and the ore overturning mechanism to work synchronously.

Images