Preparation process of semiconductor-grade synthetic quartz

Abstract

The invention relates to the technical field of quartz preparation, in particular to a preparation process of semiconductor-grade synthetic quartz, which comprises the following steps: SS01, preparing materials, namely putting alkali metal silicate into quartz preparation equipment and adding medium-temperature pure water for dissolving and diluting, SS02, removing impurities, namely adding an impurity removing agent into an alkali metal silicate diluted solution obtained in the step SS01, fully stirring and uniformly mixing, and preparing the semiconductor-grade synthetic quartz. After the impurity removing agent is added, the stirred solution is subjected to standing precipitation, after precipitation is completed, precipitates are filtered and separated, and finally precipitated heavy metal hydroxides and a solution to be subjected to ion exchange are separated from the solution subjected to standing precipitation. The device has the beneficial effects that when the device works, the material preparation process, the impurity removal process, the ion exchange process and the aging purification process in the quartz preparation process can be integrally realized, and the automation degree and the preparation efficiency in the quartz preparation process are effectively improved through the integrated process.

Description

Technical Field

[0001] The invention relates to the technical field of quartz preparation, in particular to a process for preparing semiconductor-grade synthetic quartz. Background Art

[0002] In the semiconductor industry, quartz is an important material, and its purity and quality have a significant impact on the performance of semiconductor devices. Traditional quartz preparation processes often have problems such as low preparation efficiency, insufficient automation, difficulty in effectively removing impurities during the preparation process, and unsatisfactory purification effects. These problems not only affect the performance of quartz materials, but also limit the development of semiconductor devices.

[0003] The patent document with publication number CN118684232A in the prior art discloses a method for preparing low-cost and high-purity synthetic quartz sand, comprising the following steps: step 1, diluting alkali metal silicate with high-purity water at 35-55°C until it is completely dissolved; wherein the alkali metal silicate includes anhydrous sodium silicate, sodium silicate pentahydrate and sodium silicate nonahydrate; step 2, adding an impurity remover to the alkali metal silicate diluted solution obtained in step 1, stirring and mixing well, the impurity remover includes CaO and Ca(OH)2, and the Ca(OH)2 added in the present invention removes heavy metal ions first by controlling the addition amount, so that it is only enough to precipitate heavy metal ions without excessive reaction with silicate, and the precipitated heavy metal hydroxide can be separated by filtration, which has no effect on subsequent ion exchange impurity removal.

[0004] Specifically, the traditional quartz preparation process usually includes steps such as material preparation, impurity removal, ion exchange, and aging purification. However, these steps are often dispersed in different equipment, making the entire preparation process cumbersome and inefficient. In addition, traditional impurity removal and purification methods may not effectively remove heavy metal ions and other impurities in the solution, thereby affecting the purity of quartz. At the same time, during the aging purification process, due to the instability of the drying conditions, the drying effect of the gel may be unsatisfactory, which in turn affects the quality of the final quartz sand.

[0005] Existing devices use cheap alkali metal silicates as alternative raw materials to significantly reduce the cost of high-purity synthetic quartz. However, the prior art lacks a dedicated integrated equipment for the material preparation process, impurity removal process, ion exchange process and aging purification process when preparing quartz. Based on this, the present invention provides a semiconductor-grade synthetic quartz preparation process to solve the problems raised in the above background technology. Summary of the invention

[0006] The present invention aims at the technical problems existing in the prior art and provides a semiconductor-grade synthetic quartz preparation process to solve the problem that the prior art lacks a dedicated integrated equipment for the material preparation process, impurity removal process, ion exchange process and aging purification process when realizing quartz preparation.

[0007] The technical solution of the present invention to solve the above technical problems is as follows: A process for preparing semiconductor-grade synthetic quartz comprises the following steps: SS01, put alkali metal silicate into quartz preparation equipment and add medium temperature pure water to dissolve and dilute; SS02, adding an impurity remover to the alkali metal silicate dilute solution obtained in step SS01, fully stirring and evenly mixing, allowing the stirred solution to settle, filtering and separating the precipitate, and separating the precipitated heavy metal hydroxide and the solution to be ion exchanged from the solution after the settling; SS03, passing the solution to be ion exchanged obtained in step SS02 into a strong acid cation exchange column, and removing calcium ions and sodium ions in the solution after the solution passes into the strong acid cation exchange column, and after the calcium ions and sodium ions are removed, a sol solution is obtained; SS04, transferring the sol solution in step SS03 into a reaction kettle, allowing the stirred sol solution to stand to obtain an initial gel, aging the obtained initial gel under the protection of an inert gas, soaking and washing the aged gel with high-purity water, drying the washed wet gel under the protection of an inert gas to obtain a dry gel, crushing the obtained dry gel, sieving after crushing, placing the crushed dry gel into a high-temperature rotary furnace for sintering, and ultra-purifying the obtained quartz sand to obtain semiconductor-grade quartz sand; The quartz preparation equipment includes a reactor, a pure water storage tank, a high-pressure gas tank and an ion exchange column. A preparation reaction mechanism is installed in the reactor. The bottom end of the reactor is connected to a three-way bottom pipe, one end of the three-way bottom pipe is connected to a first pump body, the liquid outlet end of the first pump body is connected to the liquid inlet end of the ion exchange column, a second pump body is installed on the pure water storage tank, and the liquid outlet end of the ion exchange column, the gas outlet end of the high-pressure gas tank and the liquid outlet end of the second pump body are all connected to the reactor.

[0008] Based on the above technical solution, the present invention can also be improved as follows.

[0009] Furthermore, a three-way top pipe is installed on the upper part of the reactor, a feed port is provided at the top of the three-way top pipe, the other two ends of the three-way top pipe are respectively connected to the second pump body and the liquid outlet end of the ion exchange column, and solenoid valves are provided at the connection points between the three-way top pipe and the second pump body and the ion exchange column.

[0010] Furthermore, a discharge valve is provided at one end of the three-way bottom pipe, a drain valve is connected to the bottom of the reactor, a temperature probe and a pressure relief valve are respectively installed on the top of the reactor, a spiral heating coil is installed in the reactor, and a heater is provided at the connection between the high-pressure gas tank and the reactor.

[0011] The beneficial effect of adopting the above further scheme is that when the SS01 step and the SS02 step are carried out, the alkali metal silicate is put into the reaction kettle, and the alkali metal silicate is dissolved, the impurity remover and the alkali metal silicate diluted solution are stirred and mixed, and the precipitate in the mixed solution is filtered and separated; When the SS03 step is performed, the first pump body extracts the filtered solution to be ion exchanged, and the extracted solution is sent to the ion exchange column for ion exchange. During the ion exchange, the sundries in the reactor are discharged through the drain valve, and during the ion exchange, the pure water storage tank introduces pure water into the reactor. The inner cavity and structural components of the reactor are cleaned by the introduction of pure water, and the cleaned sewage is discharged through the drain valve. After the cleaning is completed, the ion-exchanged solution is returned to the reactor. After the ion-exchanged solution is returned to the reactor, the SS04 step can be performed. During the SS04 step, inert gas is stored inside the high-pressure gas tank, and the heater is used to control the delivery temperature of the inert gas, thereby realizing the drying operation of the wet gel.

[0012] Furthermore, the reaction preparation mechanism includes a bracket installed on the top of the reactor, a vibration and stirring component installed on the bracket, and a traction rotary ring rotatably sleeved on the bracket; the vibration and stirring component is transmission-connected with a liquid vibration table that can reciprocate along the axis of the reactor, a rotatable reaction rotary frame, and a rotatable core shaft; the reaction rotary frame is rotationally connected to the liquid vibration table, a transmission bevel gear is installed on the core shaft, a group of crushing and stirring modules that are regularly distributed and transmission-connected to the transmission bevel gear are installed on the reaction rotary frame, a pressing shaft is installed on the bottom surface of the reaction rotary frame, and a group of A first crushing knife is distributed in a circular array, a rolling body is fixedly installed on the rolling shaft and at a position corresponding to the bottom of the first crushing knife, a rolling gap is provided between the rolling body and the reactor, a spiral valve leaf matching the rolling gap is installed on the rolling body, a filter element is installed at the bottom end of the rolling shaft, a silicone part is provided on the filter element, filter holes are evenly distributed on the silicone part, the bottom end of the filter element is open, the bottom end of the reactor is slidably connected to the three-way bottom pipe, a deformation component for driving the silicone part to reciprocate deformation is provided on the inner side of the filter element, and a flow control component is provided on the rolling shaft and at a position corresponding to the gap between the rolling body and the filter element.

[0013] The beneficial effect of adopting the above further scheme is that when preparing quartz sand, the first crushing knife can stir and crush the prepared raw materials. Through the rotation and vibration structure setting of the rotary mill body, the reaction efficiency, stirring effect and crushing fineness of the raw materials can be effectively improved through disturbance and pressing.

[0014] Furthermore, the vibration and stirring component includes a DC motor installed on the top of the reactor, a fixed shaft and a first convex shaft rotatably connected to the bracket, the output shaft end of the DC motor is fixedly connected to the fixed shaft, and the fixed shaft and the first convex shaft are both equipped with first bevel gears, the two first bevel gears are meshed with each other, and a protrusion is installed on the first convex shaft. A limiting wheel is rotatably installed on the liquid vibration table, and the limiting wheel is adaptably connected to the protrusion. A group of reset springs limited by the bracket are installed on the bottom surface of the liquid vibration table, and the reaction rotating frame and the core shaft are both driven by the fixed shaft.

[0015] Furthermore, a core groove is fixedly provided inside the core shaft with which the fixed shaft is slidably connected, and the cross-sections of the core groove and the fixed shaft are both regular polygons. A reverse transmission shaft is rotatably installed on the liquid vibrating table, and a reverse transmission bevel gear is installed on the reverse transmission shaft. A second bevel gear is installed on the core shaft and the reaction rotating frame, and two second bevel gears are both transmission-connected to the reverse transmission bevel gear, and the two second bevel gears are respectively arranged on both sides of the reverse transmission bevel gear.

[0016] The beneficial effect of adopting the above-mentioned further scheme is that when quartz reaction is prepared, the vibration stirring component is set to drive the vibrating liquid table to vibrate up and down and make the reaction rotary frame and the core shaft rotate at a set speed. The up and down reciprocating vibration of the vibrating liquid table is used to reciprocate the position of the first crushing knife and the rotary mill body, thereby effectively improving the crushing reaction efficiency of the preparation device and reducing the residual rate of the reaction material inside the device through vibration.

[0017] Furthermore, the crushing and mixing module includes a reciprocating stirring table slidably connected to the reaction rotary frame and a coupling rotatably connected to the reaction rotary frame, a linkage bevel gear cooperating with a transmission bevel gear is installed on the coupling, a group of traction rods are hinged between the reciprocating stirring table and the traction rotary ring, a powder stirring shaft is rotatably installed on the reciprocating stirring table, the powder stirring shaft is driven by the coupling, and a plurality of groups of second powder stirring knives distributed in a circular array are installed on the powder stirring shaft.

[0018] The beneficial effect of adopting the above further scheme is that when the material reaction operation is carried out, the reciprocating stirring table moves back and forth within the set stroke, and then realizes the dynamic point and the variable point reciprocating stirring, thereby effectively improving the reaction efficiency and reaction uniformity of the reactants.

[0019] Furthermore, a guide sleeve is rotatably installed on the reciprocating stirring table, and a connecting groove with openings at both ends and slidingly connected to the coupling shaft is fixedly opened inside the guide sleeve, and the cross-sections of the coupling shaft and the connecting groove are both regular polygons, and the cross-sections of the connecting groove and the coupling shaft are both regular polygons. A third bevel gear is installed on the guide sleeve and the powder stirring shaft, and the two third bevel gears are meshed with each other.

[0020] Furthermore, the deforming component includes a second camshaft and a reset roller rotatably connected to the filter element, and the second camshaft and the reset roller are both equipped with driven gears. A driving gear is installed at the bottom end of the core shaft, and the two driven gears are driven by the driving gear. A group of extrusion convex plates are installed on the second camshaft, and the extrusion convex plates and the reset roller are both arranged on the inner side of the silicone part, and the extrusion convex plates and the reset roller are both in contact with the silicone part.

[0021] The beneficial effect of adopting the above further scheme is that when filtering the crushed dry gel and filtering the reaction solution, the second camshaft and the reset roller rotate at a set speed, and the second camshaft is deformed to make the silicone part deform reciprocatingly, and then the filtering angle of the filter hole to the liquid is changed reciprocatingly, thereby improving the filtering efficiency of the liquid, and the blockage rate of the liquid to be filtered in the filter hole can be effectively reduced by realizing the reciprocating deformation effect of the silicone part, and the setting of the reset roller enables the silicone part to perform cyclic reset and cyclic deformation.

[0022] Furthermore, the flow control component includes a material guide cone seat installed in the reactor, a flow control cavity corresponding to the position of the guide cone seat is fixedly opened on the rolling shaft, a group of flow control valve holes distributed in a circular array are opened on the flow control cavity, and a group of breaking rods are installed on the rolling shaft and at the position corresponding to the flow control valve hole and the filter element.

[0023] The beneficial effect of adopting the above further solution is that, when in use, the processing time and processing intensity of the rotary mill on the reaction material can be effectively controlled by setting the flow control component.

[0024] The beneficial effects of the present invention are: 1. When the device is working, it can realize the material preparation process, impurity removal process, ion exchange process and aging purification process in quartz preparation in an integrated manner. Through the realization of the above-mentioned integrated process, the degree of automation and preparation efficiency of quartz preparation can be effectively improved.

[0025] 2. In the present device, when the SS01 step and the SS02 step are performed, the alkali metal silicate is put into the reactor, and the alkali metal silicate is dissolved, the impurity remover and the alkali metal silicate dilution solution are stirred and mixed, and the precipitate in the mixed solution is filtered and separated. When the SS03 step is performed, the first pump body extracts the filtered solution to be ion exchanged, and the extracted solution is sent to the ion exchange column for ion exchange. During the ion exchange, the impurities in the reactor are discharged through the drain valve. During the ion exchange, the pure water storage tank introduces pure water into the reactor. The inner cavity and structural elements of the reactor are cleaned by the introduction of pure water. The cleaned sewage is discharged through the drain valve. After the cleaning is completed, the ion-exchanged solution is returned to the reactor. After the ion-exchanged solution is returned to the reactor, the SS04 step can be performed. During the SS04 step, inert gas is stored inside the high-pressure gas tank, and the heater is used to control the delivery temperature of the inert gas, thereby realizing the drying operation of the wet gel.

[0026] 3. When preparing quartz sand in the present invention, the first crushing knife can stir and crush the prepared raw materials. Through the rotation and vibration structure of the rotary mill body, the reaction efficiency, stirring effect and crushing fineness of the raw materials can be effectively improved through disturbance and pressing. When preparing the quartz reaction, the vibration stirring component is set to drive the vibrating table to vibrate up and down and make the reaction rotary frame and the core shaft rotate at a set speed. The up and down reciprocating vibration of the vibrating table can reciprocate to change the position of the first crushing knife and the rotary mill body, thereby effectively improving the crushing reaction efficiency of the preparation device and reducing the residual rate of the reaction material inside the device through vibration.

[0027] 4. In the present invention, when filtering the crushed dry gel and the reaction solution, the second camshaft and the reset roller rotate at a set speed, and the second camshaft is deformed to make the silicone part deform back and forth, and then the filtering angle of the filter hole to the liquid is changed back and forth, thereby improving the filtering efficiency of the liquid. The reciprocating deformation effect of the silicone part can effectively reduce the blockage rate of the liquid to be filtered in the filter hole, and the setting of the reset roller allows the silicone part to be cyclically reset and cyclically deformed. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] Figure 1 It is a schematic diagram of the overall structure of a semiconductor-grade synthetic quartz preparation process of the present invention; Figure 2 For the present invention Figure 1 A schematic diagram of the structure from another perspective; Figure 3 It is a schematic diagram of the structure of the spiral heating coil and the material guide cone seat of the present invention; Figure 4 For the present invention Figure 3 A schematic diagram of the local enlarged structure at point A in the middle; Figure 5 For the present invention Figure 3 A schematic diagram of the local enlarged structure at B in the middle; Figure 6 For the present invention Figure 3 A schematic diagram of the local enlarged structure at C in the middle; Figure 7 It is a schematic diagram of the structure of the bracket and the silicone part of the present invention; Figure 8 It is a structural schematic diagram of the mandrel and the reset roller of the present invention; Fig. 9 It is a schematic diagram of the structure of the rolling shaft and the filter element of the present invention; Fig.10 It is a process flow chart of the present invention.

[0029] In the accompanying drawings, the components represented by the reference numerals are listed as follows: 1. Quartz preparation equipment; 2. Reactor; 3. Pure water storage tank; 4. High-pressure gas tank; 5. Ion exchange column; 6. Three-way bottom pipe; 7. Three-way top pipe; 8. Drain valve; 9. Spiral heating coil; 10. Heater; 11. Bracket; 12. Traction rotary ring; 13. Liquid vibrating table; 14. Reaction rotary rack; 15. Mandrel; 16. Pressing roller shaft; 17. First crushing knife; 18. Rotary roller body; 19. Spiral valve leaf; 20. Filter element; 21. Silicone part; 22 , DC motor; 23, fixed shaft; 24, first cam shaft; 25, convex block; 26, reset spring; 27, reverse shaft; 28, reciprocating stirring table; 29, coupling; 30, traction rod; 31, powder stirring shaft; 32, second powder stirring knife; 33, guide sleeve; 34, second cam shaft; 35, reset roller; 36, driving gear; 37, driven gear; 38, guide cone seat; 39, flow control valve hole; 40, limiting wheel; 41, extrusion convex plate; 42, breaking rod. DETAILED DESCRIPTION

[0030] The principles and features of the present invention are described below in conjunction with the accompanying drawings. The examples given are only used to explain the present invention and are not used to limit the scope of the present invention.

[0031] like Figure 1-10 As shown, a semiconductor-grade synthetic quartz preparation process comprises the following steps: SS01, prepare materials, put alkali metal silicate into quartz preparation equipment 1 and add medium temperature pure water to dissolve and dilute; SS02, impurity removal, adding an impurity remover to the alkali metal silicate dilute solution obtained in step SS01, fully stirring and evenly mixing, after the impurity remover is added, the stirred solution is allowed to stand for precipitation, after precipitation is complete, the precipitate is filtered and separated, and finally the precipitated heavy metal hydroxide and the solution to be ion exchanged are separated from the solution after standing for precipitation; SS03, ion exchange, passing the solution to be ion exchanged obtained in step SS02 into a strong acid cation exchange column 5, and removing calcium ions and sodium ions in the solution after the solution passes into the strong acid cation exchange column 5, and after the calcium ions and sodium ions are removed, a sol solution is obtained; SS04, aging and purification, the sol solution in step SS03 is transferred into the reactor 2, after the sol solution is transferred, it is stirred under the protection of inert gas, after stirring, the stirred sol solution is allowed to stand, after standing, the initial gel is obtained, after the initial gel is obtained, the initial gel is aged under the protection of inert gas, after aging, the aged gel is soaked and washed with high-purity water, after washing, the washed wet gel is dried under the protection of inert gas, after drying, the dry gel is obtained, after the dry gel is obtained, the obtained dry gel is crushed, after crushing, it is sieved, after sieving, the crushed dry gel is put into a high-temperature rotary furnace for sintering, after sintering, quartz sand is obtained, the obtained quartz sand is subjected to ultra-high purity purification, and then the purified semiconductor-grade quartz sand is obtained; As an embodiment, the quartz preparation equipment 1 includes a reactor 2, a pure water storage tank 3, a high-pressure gas tank 4 and an ion exchange column 5. A preparation reaction mechanism is installed in the reactor 2. The bottom end of the reactor 2 is connected to a three-way bottom pipe 6. One end of the three-way bottom pipe 6 is connected to a first pump body. The liquid outlet end of the first pump body is connected to the liquid inlet end of the ion exchange column 5. A second pump body is installed on the pure water storage tank 3. The liquid outlet end of the ion exchange column 5, the gas outlet end of the high-pressure gas tank 4 and the liquid outlet end of the second pump body are all connected to the reactor 2.

[0032] A three-way top pipe 7 is installed on the upper part of the reactor 2, and a feed port is provided at the top of the three-way top pipe 7. The other two ends of the three-way top pipe 7 are respectively connected to the second pump body and the liquid outlet end of the ion exchange column 5. Solenoid valves are provided at the connecting points between the three-way top pipe 7 and the second pump body and the ion exchange column 5.

[0033] A discharge valve is provided at one end of the three-way bottom pipe 6, a drain valve 8 is connected to the bottom of the reactor 2, a temperature probe and a pressure relief valve are respectively installed on the top of the reactor 2, a spiral heating coil 9 is installed in the reactor 2, and a heater 10 is provided at the connection point between the high-pressure gas tank 4 and the reactor 2.

[0034] When the SS01 step and the SS02 step are performed, the alkali metal silicate is put into the reaction kettle 2, and the alkali metal silicate is dissolved, the impurity remover and the alkali metal silicate diluted solution are stirred and mixed, and the precipitate in the mixed solution is filtered and separated; When the SS03 step is performed, the first pump body extracts the filtered solution to be ion exchanged, and the extracted solution is sent to the ion exchange column 5 for ion exchange. During the ion exchange, the sundries in the reactor 2 are discharged through the drain valve 8, and during the ion exchange, the pure water storage tank 3 introduces pure water into the reactor 2, and the inner cavity and structural components of the reactor 2 are cleaned by the introduction of pure water. The cleaned sewage is discharged through the drain valve 8. After the cleaning is completed, the ion-exchanged solution is returned to the reactor 2. After the ion-exchanged solution is returned to the reactor 2, the SS04 step can be performed. During the SS04 step, inert gas is stored in the high-pressure gas tank 4, and the heater 10 is used to control the delivery temperature of the inert gas, thereby realizing the drying operation of the wet gel.

[0035] As an embodiment, the preparation reaction mechanism includes a bracket 11 installed on the top of the reactor 2, a vibration and stirring component installed on the bracket 11, and a traction rotary ring 12 rotatably sleeved on the bracket 11. The vibration and stirring component is transmission-connected with a liquid vibration table 13 that can reciprocate along the axis direction of the reactor 2, a rotatable reaction rotary frame 14, and a rotatable core shaft 15. The reaction rotary frame 14 is rotationally connected to the liquid vibration table 13, and a transmission bevel gear is installed on the core shaft 15. A group of crushing and stirring modules that are regularly distributed and transmission-connected to the transmission bevel gear are installed on the reaction rotary frame 14. A crushing shaft 16 is installed on the bottom surface of the reaction rotary frame 14, and a group of A first crushing knife 17 is distributed in a circular array, and a rolling body 18 is fixedly installed on the rolling shaft 16 and at a position corresponding to the bottom of the first crushing knife 17. A rolling gap is provided between the rolling body 18 and the reactor 2, and a spiral valve leaf 19 matching the rolling gap is installed on the rolling body 18. A filter element 20 is installed at the bottom end of the rolling shaft 16, and a silicone portion 21 is provided on the filter element 20. The silicone portion 21 is evenly distributed with filter holes. The bottom end of the filter element 20 is open, and the bottom end of the reactor 2 is slidably connected to the three-way bottom pipe 6. A deformation component for driving the silicone portion 21 to reciprocate is provided on the inner side of the filter element 20, and a flow control component is provided on the rolling shaft 16 and at a position corresponding to the position between the rolling body 18 and the filter element 20.

[0036] When preparing quartz sand, the first crushing knife 17 can stir and crush the prepared raw materials. Through the rotation and vibration structure of the rotary mill 18, the reaction efficiency, stirring effect and crushing fineness of the raw materials can be effectively improved through disturbance and compression.

[0037] As an embodiment, the vibration and stirring component includes a DC motor 22 installed on the top of the reactor 2, a fixed shaft 23 and a first convex shaft 24 rotatably connected to the bracket 11, the output shaft end of the DC motor 22 is fixedly connected to the fixed shaft 23, and the fixed shaft 23 and the first convex shaft 24 are both equipped with first bevel gears, the two first bevel gears are meshed with each other, and the first convex shaft 24 is equipped with a protrusion 25. A limiting wheel 40 is rotatably installed on the liquid vibration table 13, and the limiting wheel 40 is adaptively connected to the protrusion 25. A group of reset springs 26 limited by the bracket 11 are installed on the bottom surface of the liquid vibration table 13, and the reaction rotating frame 14 and the core shaft 15 are both driven by the fixed shaft 23.

[0038] A core groove is fixedly provided inside the core shaft 15 and is slidably connected to the fixed shaft 23. The cross sections of the core groove and the fixed shaft 23 are both regular polygons. A reverse transmission shaft 27 is rotatably installed on the liquid vibrating table 13, and a reverse transmission bevel gear is installed on the reverse transmission shaft 27. Second bevel gears are installed on the core shaft 15 and the reaction rotating frame 14. The two second bevel gears are both drivingly connected to the reverse transmission bevel gears, and the two second bevel gears are respectively arranged on both sides of the reverse transmission bevel gear.

[0039] During the quartz reaction preparation, the vibrating and stirring components are set to drive the liquid vibrating table 13 to vibrate up and down and make the reaction rotating frame 14 and the core shaft 15 rotate at a set speed. The up and down reciprocating vibration of the liquid vibrating table 13 is used to reciprocate the positions of the first crushing knife 17 and the rotary mill 18, thereby effectively improving the crushing reaction efficiency of the preparation device and reducing the residual rate of the reaction material inside the device through vibration.

[0040] As an embodiment, the crushing and mixing module includes a reciprocating stirring table 28 slidably connected to the reaction rotary frame 14 and a coupling 29 rotatably connected to the reaction rotary frame 14, a linkage bevel gear that cooperates with the transmission bevel gear is installed on the coupling 29, a group of traction rods 30 are hinged between the reciprocating stirring table 28 and the traction rotary ring 12, a powder stirring shaft 31 is rotatably installed on the reciprocating stirring table 28, the powder stirring shaft 31 is driven by the coupling 29, and a plurality of groups of second powder stirring knives 32 distributed in a circular array are installed on the powder stirring shaft 31.

[0041] When the material is reacting, the reciprocating stirring table 28 moves back and forth within a set stroke, thereby realizing reciprocating stirring at the moving point and the changing point, thereby effectively improving the reaction efficiency and reaction uniformity of the reactants.

[0042] A guide sleeve 33 is rotatably mounted on the reciprocating stirring table 28, and a coupling groove with openings at both ends and slidably connected to the coupling shaft 29 is fixedly opened inside the guide sleeve 33. The cross-sections of the coupling shaft 29 and the coupling groove are both regular polygons, and the cross-sections of the coupling groove and the coupling shaft 29 are both regular polygons. A third bevel gear is installed on the guide sleeve 33 and the powder stirring shaft 31, and the two third bevel gears are meshed with each other.

[0043] As an embodiment, the deforming component includes a second camshaft 34 and a reset roller 35 rotatably connected to the filter element 20, and a driven gear 37 is installed on the second camshaft 34 and the reset roller 35. A driving gear 36 is installed at the bottom end of the core shaft 15, and the two driven gears 37 are driven by the driving gear 36. A group of extrusion convex plates 41 are installed on the second camshaft 34, and the extrusion convex plates 41 and the reset roller 35 are both arranged on the inner side of the silicone part 21, and the extrusion convex plates 41 and the reset roller 35 are both in contact with the silicone part 21.

[0044] When filtering the crushed dry gel and the reaction solution, the second camshaft 34 and the reset roller 35 rotate at a set speed. The second camshaft 34 is deformed to make the silicone portion 21 deform back and forth, and then the filtering angle of the filter hole to the liquid is changed back and forth, thereby improving the filtering efficiency of the liquid. The reciprocating deformation effect of the silicone portion 21 can effectively reduce the blockage rate of the liquid to be filtered in the filter hole. The setting of the reset roller 35 allows the silicone portion 21 to perform cyclic reset and cyclic deformation.

[0045] As an embodiment, the flow control component includes a material guide cone seat 38 installed in the reactor 2, a flow control cavity corresponding to the position of the guide cone seat is fixedly opened on the rolling shaft 16, a group of flow control valve holes 39 distributed in a circular array are opened on the flow control cavity, and a group of breaking rods 42 are installed on the rolling shaft 16 and at the position corresponding to the flow control valve hole 39 and the filter element 20.

[0046] When in use, the flow control component is set to effectively control the processing time and processing intensity of the rotary mill 18 on the reaction material, and the breaking rod 42 is set to fully break up the gel after crushing and rolling.

[0047] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims

1. A process for preparing semiconductor-grade synthetic quartz, characterized in that: The following steps are involved: SS01, put alkali metal silicate into quartz preparation equipment (1) and add medium temperature pure water to dissolve and dilute; SS02, adding an impurity remover to the alkali metal silicate dilute solution obtained in step SS01, fully stirring and evenly mixing, allowing the stirred solution to settle, filtering and separating the precipitate, and separating the precipitated heavy metal hydroxide and the solution to be ion exchanged from the solution after the settling; SS03, passing the solution to be ion exchanged obtained in step SS02 into a strong acid cation exchange column (5), and removing calcium ions and sodium ions in the solution after the solution passes into the strong acid cation exchange column (5). After the calcium ions and sodium ions are removed, a sol solution is obtained; SS04, transferring the sol solution in step SS03 into a reaction kettle (2), allowing the stirred sol solution to stand to obtain an initial gel, aging the obtained initial gel under the protection of an inert gas, soaking and washing the aged gel with high-purity water, drying the washed wet gel under the protection of an inert gas to obtain a dry gel, crushing the obtained dry gel, sieving after crushing, placing the crushed dry gel into a high-temperature rotary furnace for sintering, and ultra-purifying the obtained quartz sand to obtain semiconductor-grade quartz sand; The quartz preparation equipment (1) comprises a reaction kettle (2), a pure water storage tank (3), a high-pressure gas tank (4) and an ion exchange column (5); a preparation reaction mechanism is installed in the reaction kettle (2); the bottom end of the reaction kettle (2) is connected to a three-way bottom pipe (6); one end of the three-way bottom pipe (6) is connected to a first pump body; the liquid outlet end of the first pump body is connected to the liquid inlet end of the ion exchange column (5); a second pump body is installed on the pure water storage tank (3); the liquid outlet end of the ion exchange column (5), the gas outlet end of the high-pressure gas tank (4) and the liquid outlet end of the second pump body are all connected to the reaction kettle (2).

2. A process for preparing semiconductor-grade synthetic quartz according to claim 1, characterized in that: A three-way top pipe (7) is installed on the upper part of the reaction kettle (2), a feed port is provided at the top end of the three-way top pipe (7), the other two ends of the three-way top pipe (7) are respectively connected to the second pump body and the liquid outlet end of the ion exchange column (5), and electromagnetic valves are provided at the connection points between the three-way top pipe (7) and the second pump body and the ion exchange column (5).

3. A process for preparing semiconductor-grade synthetic quartz according to claim 1, characterized in that: A discharge valve is provided at one end of the three-way bottom pipe (6), a drain valve (8) is connected to the bottom of the reactor (2), a temperature probe and a pressure relief valve are respectively installed on the top of the reactor (2), a spiral heating coil (9) is installed in the reactor (2), and a heater (10) is provided at the connection point between the high-pressure gas tank (4) and the reactor (2).

4. A process for preparing semiconductor-grade synthetic quartz according to claim 1, characterized in that: The preparation reaction mechanism comprises a bracket (11) mounted on the top of the reaction kettle (2), a vibration and stirring generating component mounted on the bracket (11), and a traction rotating ring (12) rotatably sleeved on the bracket (11); the vibration and stirring generating component is transmission-connected to a liquid vibration table (13) that can reciprocate along the axis of the reaction kettle (2), a rotatable reaction rotating frame (14), and a rotatable core shaft (15); the reaction rotating frame (14) is rotationally connected to the liquid vibration table (13); a transmission bevel gear is mounted on the core shaft (15); a group of regularly distributed crushing and stirring modules that are transmission-connected to the transmission bevel gear are mounted on the reaction rotating frame (14); a pressing shaft (16) is mounted on the bottom surface of the reaction rotating frame (14); a group of first crushing knives distributed in a circumferential array are mounted on the pressing shaft (16) (17), a rolling body (18) is fixedly mounted on the rolling shaft (16) and at a position corresponding to the bottom of the first crushing knife (17), a rolling gap is provided between the rolling body (18) and the reactor (2), a spiral valve leaf (19) matched with the rolling gap is installed on the rolling body (18), a filter element (20) is installed at the bottom end of the rolling shaft (16), a silicone portion (21) is provided on the filter element (20), filter holes are evenly distributed on the silicone portion (21), the bottom end of the filter element (20) is open, the bottom end of the reactor (2) is slidably connected to the three-way bottom pipe (6), a deformation component for driving the silicone portion (21) to reciprocate and deform is provided on the inner side of the filter element (20), and a flow control component is provided on the rolling shaft (16) and at a position corresponding to the gap between the rolling body (18) and the filter element (20).

5. A process for preparing semiconductor-grade synthetic quartz according to claim 4, characterized in that: The vibration and stirring component comprises a DC motor (22) mounted on the top of the reaction kettle (2), a fixed shaft (23) rotatably connected to the bracket (11), and a first convex shaft (24); the output shaft end of the DC motor (22) is fixedly connected to the fixed shaft (23); first bevel gears are mounted on the fixed shaft (23) and the first convex shaft (24); the two first bevel gears are meshed with each other; a convex block (25) is mounted on the first convex shaft (24); a limiting wheel (40) is rotatably mounted on the liquid vibrating table (13); the limiting wheel (40) is adaptively connected to the convex block (25); a group of return springs (26) limited by the bracket (11) are mounted on the bottom surface of the liquid vibrating table (13); and the reaction rotating frame (14) and the core shaft (15) are both driven by the fixed shaft (23).

6. A process for preparing semiconductor-grade synthetic quartz according to claim 4, characterized in that: A core groove is fixedly provided inside the core shaft (15) and is slidably connected to the fixed shaft (23); the cross sections of the core groove and the fixed shaft (23) are both regular polygons; a reverse transmission shaft (27) is rotatably mounted on the liquid vibrating table (13); a reverse transmission bevel gear is mounted on the reverse transmission shaft (27); a second bevel gear is mounted on both the core shaft (15) and the reaction rotating frame (14); two second bevel gears are both drivingly connected to the reverse transmission bevel gear; and the two second bevel gears are respectively arranged on both sides of the reverse transmission bevel gear.

7. A process for preparing semiconductor-grade synthetic quartz according to claim 4, characterized in that: The crushing and stirring module comprises a reciprocating stirring table (28) slidably connected to a reaction rotary frame (14) and a coupling shaft (29) rotatably connected to the reaction rotary frame (14); a linkage bevel gear matched with a transmission bevel gear is mounted on the coupling shaft (29); a group of traction rods (30) are hingedly connected between the reciprocating stirring table (28) and the traction rotary ring (12); a powder stirring shaft (31) is rotatably mounted on the reciprocating stirring table (28); the powder stirring shaft (31) is driven by the coupling shaft (29); and a plurality of groups of second powder stirring knives (32) distributed in a circumferential array are mounted on the powder stirring shaft (31).

8. A process for preparing semiconductor-grade synthetic quartz according to claim 7, characterized in that: A guide sleeve (33) is rotatably mounted on the reciprocating stirring table (28); a coupling groove with two ends opened and slidably connected to the coupling shaft (29) is fixedly provided inside the guide sleeve (33); the cross-sections of the coupling shaft (29) and the coupling groove are both regular polygons; the cross-sections of the coupling groove and the coupling shaft (29) are both regular polygons; a third bevel gear is mounted on both the guide sleeve (33) and the powder stirring shaft (31); the two third bevel gears are meshed with each other.

9. A process for preparing semiconductor-grade synthetic quartz according to claim 4, characterized in that: The deforming component comprises a second camshaft (34) and a reset roller (35) rotatably connected to the filter element (20); a driven gear (37) is mounted on the second camshaft (34) and the reset roller (35); a driving gear (36) is mounted on the bottom end of the core shaft (15); the two driven gears (37) are driven by the driving gear (36); a group of extrusion convex plates (41) are mounted on the second camshaft (34); the extrusion convex plates (41) and the reset roller (35) are both arranged on the inner side of the silicone part (21); and the extrusion convex plates (41) and the reset roller (35) are both in contact with the silicone part (21).

10. A process for preparing semiconductor-grade synthetic quartz according to claim 4, characterized in that: The flow control assembly comprises a guide cone seat (38) installed in the reaction kettle (2); a flow control cavity corresponding to the position of the guide cone seat is fixedly provided on the rolling shaft (16); a group of flow control valve holes (39) distributed in a circular array are provided on the flow control cavity; and a group of breaking rods (42) are installed on the rolling shaft (16) at a position corresponding to the flow control valve hole (39) and the filter element (20).

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