CN112110637A - Impurity removal system and impurity removal process for quartz mineral powder - Google Patents

Impurity removal system and impurity removal process for quartz mineral powder Download PDF

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Publication number
CN112110637A
CN112110637A CN202010927286.3A CN202010927286A CN112110637A CN 112110637 A CN112110637 A CN 112110637A CN 202010927286 A CN202010927286 A CN 202010927286A CN 112110637 A CN112110637 A CN 112110637A
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China
Prior art keywords
temperature furnace
refractory
mineral powder
impurity removal
powder
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CN202010927286.3A
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CN112110637B (en
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沈建兴
国洪臣
晁鑫
赵祥
刘世权
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Linyi Haoquan Silicon Technology Co ltd
Qilu University of Technology
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Linyi Haoquan Silicon Technology Co ltd
Qilu University of Technology
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    • CCHEMISTRY; METALLURGY
    • C03GLASS; MINERAL OR SLAG WOOL
    • C03BMANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
    • C03B20/00Processes specially adapted for the production of quartz or fused silica articles, not otherwise provided for
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B33/00Silicon; Compounds thereof
    • C01B33/113Silicon oxides; Hydrates thereof
    • C01B33/12Silica; Hydrates thereof, e.g. lepidoic silicic acid
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/80Compositional purity

Abstract

The invention belongs to the technical field of quartz powder production, and particularly relates to a quartz mineral powder impurity removal system and an impurity removal process. The impurity removing system comprises a high-temperature furnace, a fire-resistant channel, a pickling tank, a filter and a dryer which are connected in sequence, wherein a powder feeding spray gun and a flame spray gun are arranged in the high-temperature furnace, an exhaust channel is arranged at the top of the high-temperature furnace, a discharge hole at the bottom of the high-temperature furnace is connected with the fire-resistant channel, the bottom of the fire-resistant channel is connected with a feed hole of the pickling tank, a discharge opening at the bottom of the pickling tank is connected with the filter, and a solid discharge opening at the bottom. The quartz mineral powder can be subjected to high-temperature melting, twice quenching, acid washing, filtering and drying processes in the system, so that impurity removal can be realized.

Description

Impurity removal system and impurity removal process for quartz mineral powder
Technical Field
The invention belongs to the technical field of quartz powder production, and particularly relates to a quartz mineral powder impurity removal system and an impurity removal process.
Background
The fused quartz can be used as a raw material and a coating material for producing a crucible for semiconductor polycrystalline silicon ingot casting, can also be used as a filling raw material for packaging silicon dioxide micropowder and organic materials of an integrated circuit, and can also be used as a raw material of high-purity quartz glass by further purification. Common purification processes of quartz mineral raw materials comprise high-temperature chlorination, calcination, acid washing, flotation, melting and the like, and two or more of the processes are combined for use so as to realize impurity removal and purification of the quartz mineral raw materials. Because the ore forming difference of quartz minerals is large, the impurity removal and purity extraction are still the technical bottleneck of the high-purity quartz industry. Therefore, firstly, a gas-liquid wrapping phase and a crystal or quartz ore raw material with low impurity content need to be selected; next, the existence form and state of the impurity phase in the mineral raw material are analyzed. On the basis, the technical combination is adopted in a targeted manner to realize efficient and environment-friendly impurity removal of the quartz raw material.
Disclosure of Invention
Aiming at the defects of the existing quartz mineral powder purification technology, the invention provides an impurity removal system for a quartz mineral raw material, and the purity of the quartz raw material is improved through a technological process combining high-temperature spray burning, twice quenching and acid washing.
In order to achieve the purpose, the invention adopts the following technical scheme:
a quartz mineral powder impurity removal system comprises a high-temperature furnace, a refractory channel, a pickling tank, a filter and a dryer which are connected in sequence; the high-temperature furnace is internally provided with a powder feeding spray gun and a flame spray gun, the powder feeding spray gun is positioned above the flame spray gun, the top of the high-temperature furnace is provided with an exhaust passage, a discharge hole at the bottom of the high-temperature furnace is connected with a fire-resistant passage, the bottom of the fire-resistant passage is connected with a feed inlet of a pickling tank, a discharge opening at the bottom of the pickling tank is connected with a filter, and a solid discharge opening at the bottom of the filter is connected with a dryer.
Preferably, the high-temperature furnace sequentially comprises a powder feeding area, a flame combustion area and a blanking area from top to bottom, the powder feeding area is in a truncated cone shape with a top necking, the combustion area is in a cylindrical shape, and the blanking area is in a truncated cone shape with a bottom necking.
Preferably, the inner diameter of the flame combustion zone is not less than 3 m, the height of the flame combustion zone is not less than 1 m, and the height and the temperature of the flame combustion zone can be adjusted by the position, the number, the fuel ratio and the supply quantity of the flame spray guns.
Preferably, the powder feeding spray gun is inclined to the center of the high-temperature furnace along the circumferential direction of the powder feeding area; the flame spray guns are arranged in a downward inclined mode, and the inclination angle between the flame spray guns and the horizontal line is not more than 15 degrees; the maximum powder spraying diameter range of all the powder feeding spray guns does not exceed the circumferential diameter range of the flame zone.
Preferably, a discharge port at the bottom of the high-temperature furnace is connected with a plurality of refractory passages, a refractory flashboard is arranged between the discharge port and each refractory passage, and the bottom of each refractory passage is connected with a pickling tank corresponding to the refractory passage. The channel is hollow and cylindrical, and the inner surface of the channel is smooth, so that the passing resistance of the powder in the channel can be reduced; the channel is made of alumina bricks or other high-temperature resistant materials, and can also be made of commercial alumina tubes directly. The position, close to the bottom of the high-temperature furnace, in the channel is provided with a refractory flashboard so as to facilitate the selective and time-sharing use and closing of the plurality of channels.
Preferably, a single filter and dryer may be connected to the plurality of pickling baths, or each pickling bath may correspond to a separate filter and dryer, depending on the amount of production.
Preferably, the inner surface of the refractory channel is smooth, compressed gas spray guns are obliquely arranged in the refractory channel downwards, the compressed gas spray guns are uniformly arranged along the periphery of the refractory channel, and the spray guns spray pure compressed air into the channel to rapidly cool materials falling from the high-temperature furnace for one time and play a role of blowing the materials to a pickling bath; in addition, the compressed air flow also plays a role of air sealing, so that acid gas volatilized from the pickling bath is prevented from entering a pipeline and a high-temperature furnace.
Preferably, a bubbling stirring device is arranged at the bottom of the pickling tank, the bubbling device comprises a nozzle inserted into the bottom of the pickling tank, the nozzle is connected with a compressor through a pipeline, and a gas valve is arranged on the pipeline. The pickling bath is made of acid-resistant materials, and can also be made of other inorganic materials with acid-resistant linings added inside; the bubbling stirring device can accelerate and perfect the pickling and impurity removal process.
The invention also discloses a quartz mineral powder impurity removal process, which utilizes the system to remove impurities and specifically comprises the following steps:
firstly, quartz mineral powder is blown into a flame combustion area of a high-temperature furnace from the top of the high-temperature furnace for oxyhydrogen flame combustion by a powder feeding spray gun by using purified dry compressed air as carrier gas. The quartz mineral powder is directly melted at high temperature, and is pelletized by surface tension, the solid density is increased immediately, and the quartz mineral powder begins to settle towards the lower part of the high-temperature furnace and is partially cooled in the settling process.
Further, the particles settled to the bottom of the high-temperature furnace enter a refractory channel obliquely connected with the bottom of the high-temperature furnace, are rapidly cooled by pure compressed air sprayed from the channel at one time, are driven by the compressed air flow to advance along the channel at an accelerated speed, fall into pickling solution prepared by hydrochloric acid and a small amount (1-3%) of phosphoric acid, and are subjected to further pickling and impurity removal after secondary quenching and burst. The addition of phosphoric acid aids in the dissolution of impurities on the surface of the fused silica and in the decrepitation peaks. The pickling time and the concentration of the pickling solution are determined by pretreatment experiments according to the impurity types and the contents of the raw materials.
In particular, in order to ensure that fused quartz particles sprayed and burned at different times are sufficiently pickled and decontaminated in the pickling tank, the high-temperature furnace is connected with the plurality of heat-resistant channels and the pickling tank and is selectively and sequentially opened in a time-sharing manner, namely, only part of the channels and the corresponding pickling tank in one or all the channels are opened each time, the rest channels are closed, after enough fused powder is accumulated in the pickling tank corresponding to the opened channels, the channels are closed, and then the other channels are opened to pump out the generated fused powder in the melting furnace to the other pickling tank. And after fully pickling and removing impurities from the fused quartz particles in the previous pickling tank or the previous part of the fused quartz particles in the previous pickling tank, unloading the fused quartz particles to a filtering device, filtering and separating the quartz powder from the acid liquor after the impurities are removed, and further drying the quartz powder. After the pickling tank is unloaded, the other part of the working channel can be closed, and then the corresponding channel of the pickling tank is opened again for use, so that the continuous production of the whole system is realized in a time-sharing and circulating manner.
Advantageous effects
The invention discloses a quartz mineral powder impurity removal system which is beneficial to removing low-melting-point components of quartz raw materials through a melting process; the crushing and cracking of the fused quartz are realized through air cooling and water quenching, and the impurity surface and position of the fused quartz are exposed, so that the full acid washing and impurity removal are facilitated. The bottom of the pickling tank is provided with a bubbling device to play a role in stirring materials, so that the pickling process is facilitated to be accelerated, and the materials settled at the bottom are prevented from being insufficiently contacted with acid; the combined configuration of the multiple channels and the multiple acid pools and the time-sharing working mode of selective opening and closing ensure the full performance of acid washing and impurity removal and realize the continuous performance of production.
The above description replaces the characteristics of the impurity removing system for quartz mineral powder, and also includes the characteristics of the impurity removing process using the system, and the rest of the description, which is not specifically described, adopts the known technology of the person skilled in the art.
To facilitate an understanding of the systems and processes of the present invention, the invention is further described with reference to the accompanying drawings.
Drawings
FIG. 1 is a schematic structural diagram of a quartz mineral powder impurity removal system according to embodiment 1 of the present invention;
in the figure, 1: powder feeding spray gun, 2: high-temperature furnace, 3: flame spray gun, 4: refractory shutter, 5: refractory passage, 6: exhaust passage, 7: compressed gas spray gun, 8: pickling bath, 9: bubbling stirring apparatus, 10: filter, 11: and (7) a dryer.
Detailed Description
Hereinafter, the present invention will be described in detail. Before the description is made, it should be understood that the terms used in the present specification and the appended claims should not be construed as limited to general and dictionary meanings, but interpreted based on the meanings and concepts corresponding to technical aspects of the present invention on the basis of the principle that the inventor is allowed to define terms appropriately for the best explanation. Accordingly, the description proposed herein is just a preferable example for the purpose of illustrations only, not intended to limit the scope of the invention, so it should be understood that other equivalents and modifications could be made thereto without departing from the spirit and scope of the invention.
The following examples are given by way of illustration of embodiments of the invention and are not to be construed as limiting the invention, and it will be understood by those skilled in the art that modifications may be made without departing from the spirit and scope of the invention. Unless otherwise specified, reagents and equipment used in the following examples are commercially available products.
Example 1
A quartz mineral powder impurity removal system comprises a high-temperature furnace 2, a refractory channel 5, a pickling tank 8, a filter 10 and a dryer 11 which are connected in sequence; the high-temperature furnace is internally provided with a powder feeding spray gun 1 and a flame spray gun 3, the powder feeding spray gun is positioned above the flame spray gun, the top of the high-temperature furnace is provided with an exhaust passage 6, a discharge hole at the bottom of the high-temperature furnace is connected with a fire-resistant passage 5, the bottom of the fire-resistant passage is connected with a feed inlet of a pickling tank, a discharge opening at the bottom of the pickling tank is connected with a filter, and a solid discharge opening at the bottom of the filter is connected with a dryer.
The high-temperature furnace sequentially comprises a powder feeding area, a flame combustion area and a blanking area from top to bottom, wherein the powder feeding area is in a truncated cone shape with a top necking, the combustion area is in a cylindrical shape, and the blanking area is in a truncated cone shape with a bottom necking.
The inner diameter of the flame combustion zone is not less than 3 meters, the height of the flame combustion zone is not less than 1 meter, and the height and the temperature of the flame combustion zone can be adjusted by the position, the number, the fuel ratio and the supply quantity of the flame spray guns.
The powder feeding spray gun 1 is inclined to the center of the high-temperature furnace along the circumferential direction of the powder feeding area; the flame spray gun 3 is arranged in a downward inclined mode, and the inclination angle between the flame spray gun 3 and the horizontal line is not more than 15 degrees; the maximum powder spraying diameter range of all the powder feeding spray guns does not exceed the circumferential diameter range of the flame zone.
High temperature furnace bottom discharge gate is connected with a plurality of refractory channel 5, all be provided with fire-resistant flashboard 4 between discharge gate and every refractory channel, every refractory channel bottom all connects and is equipped with the pickling tank that corresponds separately. The channel is hollow and cylindrical, and the inner surface of the channel is smooth, so that the passing resistance of the powder in the channel can be reduced; the channel is made of alumina bricks or other high-temperature resistant materials, and can also be made of commercial alumina tubes directly. The position, close to the bottom of the high-temperature furnace, in the channel is provided with a refractory flashboard so as to facilitate the selective and time-sharing use and closing of the plurality of channels.
According to the output, the multiple pickling baths can be connected with a set of filtering machine and drying machine, and each pickling bath can correspond to the respective filtering machine and drying machine.
The inner surface of the refractory channel is smooth, a compressed gas spray gun 7 is obliquely arranged in the refractory channel downwards, the compressed gas spray guns are uniformly arranged along the periphery of the refractory channel, and the spray guns spray pure compressed air into the refractory channel to rapidly cool materials falling from the high-temperature furnace for one time and play a role of blowing the materials to a pickling bath; in addition, the compressed air flow also plays a role of air sealing, so that acid gas volatilized from the pickling bath is prevented from entering a pipeline and a high-temperature furnace.
Preferably, a bubbling stirring device 9 is arranged at the bottom of the pickling tank, the bubbling device comprises a nozzle inserted into the bottom of the pickling tank, the nozzle is connected with a compressor through a pipeline, and a gas valve is arranged on the pipeline. The pickling bath is made of acid-resistant materials, and can also be made of other inorganic materials with acid-resistant linings added inside; the bubbling stirring device can accelerate and perfect the pickling and impurity removal process.
When the system is used, quartz mineral powder is used as a raw material and is sprayed into a high-temperature furnace 2 through a powder feeding spray gun 1, the quartz mineral powder is melted and spheroidized in a flame zone formed by a flame spray gun 3, and is descended to the bottom of the high-temperature furnace under the action of gravity, and then enters a refractory channel 5 opened by a refractory flashboard 4, and flue gas is discharged through an exhaust channel 6 at the top of the high-temperature furnace; the molten material is converged at an outlet at the bottom of the high-temperature furnace 2, and is accelerated to flow into the refractory channel 5 under the negative pressure formed by gas sprayed from the compressed gas spray gun 7 in the channel, and is rapidly subjected to primary air cooling and rapid cooling; the materials rapidly advance along the refractory passage 5 and finally fall into the pickling tank 8, and are stirred under the blowing bubbling action of the bubbling device 9 at the bottom of the pickling tank to promote pickling; after the pickling process is finished, discharging is carried out to the filtering machine 10 through a pipeline, and after solid-liquid separation, the materials enter the drying machine 11 for drying. In order to ensure continuous production, the high-temperature furnace 2 can be provided with two or more refractory passages 5 and corresponding pickling tanks 8, and the passages selectively work in a time-sharing and alternate mode through the opening and closing of the respective refractory gate plates 4.
Example 2
A quartz mineral powder impurity removal process utilizes the system of embodiment 1 to remove impurities, and specifically comprises the following steps:
firstly, quartz mineral powder with purity of more than 2N passes through a powder feeding spray gun, and is sprayed into a flame combustion area of a high-temperature furnace from the top of the high-temperature furnace for oxyhydrogen flame combustion by using purified dry compressed air as carrier gas. The quartz mineral powder is directly melted at high temperature, and is pelletized by surface tension, the solid density is increased immediately, and the quartz mineral powder begins to settle towards the lower part of the high-temperature furnace and is partially cooled in the settling process.
Further, the particles settled to the bottom of the high-temperature furnace enter a refractory channel obliquely connected with the bottom of the high-temperature furnace, are rapidly cooled by pure compressed air sprayed from the channel at one time, are driven by the compressed air flow to advance along the channel at an accelerated speed, fall into pickling solution prepared by hydrochloric acid and a small amount (1-3%) of phosphoric acid, and are subjected to further pickling and impurity removal after secondary quenching and burst. The addition of phosphoric acid aids in the dissolution of impurities on the surface of the fused silica and in the decrepitation peaks. The pickling time and the concentration of the pickling solution are determined by pretreatment experiments according to the impurity types and the contents of the raw materials. The purity of the quartz powder can be improved by 3-4N by the impurity removal process.
In particular, in order to ensure that fused quartz particles sprayed and burned at different times are sufficiently pickled and decontaminated in the pickling tank, the high-temperature furnace is connected with the plurality of heat-resistant channels and the pickling tank and is selectively and sequentially opened in a time-sharing manner, namely, only part of the channels and the corresponding pickling tank in one or all the channels are opened each time, the rest channels are closed, after enough fused powder is accumulated in the pickling tank corresponding to the opened channels, the channels are closed, and then the other channels are opened to pump out the generated fused powder in the melting furnace to the other pickling tank. And after fully pickling and removing impurities from the fused quartz particles in the previous pickling tank or the previous part of the fused quartz particles in the previous pickling tank, unloading the fused quartz particles to a filtering device, filtering and separating the quartz powder from the acid liquor after the impurities are removed, and further drying the quartz powder. After the pickling tank is unloaded, the other part of the working channel can be closed, and then the corresponding channel of the pickling tank is opened again for use, so that the continuous production of the whole system is realized in a time-sharing and circulating manner.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that various changes may be made and equivalents may be substituted for elements thereof; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions.

Claims (10)

1. A quartz mineral powder impurity removal system is characterized by comprising a high-temperature furnace, a refractory channel, a pickling tank, a filter and a dryer which are connected in sequence; the high-temperature furnace is internally provided with a powder feeding spray gun and a flame spray gun, the powder feeding spray gun is positioned above the flame spray gun, the top of the high-temperature furnace is provided with an exhaust passage, a discharge hole at the bottom of the high-temperature furnace is connected with a fire-resistant passage, the bottom of the fire-resistant passage is connected with a feed inlet of a pickling tank, a discharge opening at the bottom of the pickling tank is connected with a filter, and a solid discharge opening at the bottom of the filter is connected with a dryer.
2. The impurity removing system for quartz mineral powder according to claim 1, wherein the high temperature furnace comprises a powder feeding area, a flame combustion area and a blanking area from top to bottom in sequence, the powder feeding area is in a truncated cone shape with a top necking, the combustion area is in a cylinder shape, and the blanking area is in a truncated cone shape with a bottom necking; the inner diameter of the flame combustion area is not less than 3 meters, and the height of the flame combustion area is not less than 1 meter.
3. The system for removing impurities from quartz mineral powder of claim 2, wherein the powder feeding lance is arranged along the circumferential direction of the powder feeding area and inclined toward the center of the high temperature furnace; the flame spray guns are arranged in a downward inclined mode, and the inclination angle between the flame spray guns and the horizontal line is not more than 15 degrees; the maximum powder spraying diameter range of all the powder feeding spray guns does not exceed the circumferential diameter range of the flame zone.
4. The quartz mineral powder impurity removal system according to claim 1, wherein a discharge port at the bottom of the high-temperature furnace is connected with a plurality of refractory passages, a refractory gate plate is arranged between the discharge port and each refractory passage, and the bottom of each refractory passage is connected with a corresponding pickling tank.
5. The quartz mineral powder impurity removal system according to claim 4, wherein the multiple pickling baths can be connected with a set of filtering machine and drying machine, and each pickling bath can correspond to the respective filtering machine and drying machine.
6. The quartz mineral powder impurity removal system according to claim 1, wherein the inner surface of the refractory channel is smooth, compressed gas spray guns are obliquely arranged in the refractory channel downwards, and the compressed gas spray guns are uniformly arranged along the periphery of the refractory channel.
7. The quartz mineral powder impurity removal system according to claim 1, wherein a bubbling stirring device is arranged at the bottom of the pickling tank, the bubbling stirring device comprises a nozzle inserted into the bottom of the pickling tank, the nozzle is connected with a compressor through a pipeline, and a gas valve is arranged on the pipeline.
8. An impurity removal process for quartz mineral powder, which is characterized by using the system of any one of claims 1 to 7 to remove impurities, and specifically comprises the following steps: the quartz mineral powder is blown into a flame combustion area of a high-temperature furnace from the top of the high-temperature furnace for oxyhydrogen flame combustion by a powder feeding spray gun by using purified dry compressed air as carrier gas; directly melting quartz particle mineral powder under the action of high temperature, and settling the melted material towards the bottom of the high-temperature furnace; the materials settled to the bottom of the high-temperature furnace enter the fire-resistant channel through a discharge hole at the bottom of the high-temperature furnace, are rapidly cooled by pure compressed air sprayed from the fire-resistant channel for the first time, and then rapidly cooled for the second time, and then are subjected to bubbling stirring and acid washing by a bubbling stirring device at the bottom of the acid washing tank to remove impurities; finally, filtering and drying after solid-liquid separation.
9. The impurity removing process for quartz mineral powder as claimed in claim 8, wherein the temperature of the flame combustion zone is 2000-2400 ℃; the pickling solution is prepared from hydrochloric acid and 1-3% of phosphoric acid.
10. The impurity removing process for quartz mineral powder according to claim 8, wherein the material settled to the bottom of the high temperature furnace is selectively passed through a part of the refractory passage connected to the high temperature furnace in a time-sharing manner by opening and closing a refractory shutter provided on the refractory passage.
CN202010927286.3A 2020-09-07 2020-09-07 Impurity removal system and impurity removal process for quartz mineral powder Active CN112110637B (en)

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