CN108658081B - Method for producing silicon tetrafluoride by using sodium fluosilicate as raw material and production equipment thereof - Google Patents
Method for producing silicon tetrafluoride by using sodium fluosilicate as raw material and production equipment thereof Download PDFInfo
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- CN108658081B CN108658081B CN201810867476.3A CN201810867476A CN108658081B CN 108658081 B CN108658081 B CN 108658081B CN 201810867476 A CN201810867476 A CN 201810867476A CN 108658081 B CN108658081 B CN 108658081B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/08—Compounds containing halogen
- C01B33/107—Halogenated silanes
- C01B33/10705—Tetrafluoride
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
Abstract
The invention relates to a method for producing silicon tetrafluoride by using sodium fluosilicate as a raw material and production equipment thereof, which mainly produces hydrogen fluoride and silicon tetrafluoride to be prepared by the reaction of sodium fluosilicate and sulfuric acid, and repeatedly utilizes and integrates the produced hydrogen fluoride gas in various aspects, so that the reaction of hydrogen fluoride and silicon dioxide further reacts to obtain the silicon tetrafluoride; the invention has the beneficial effects that: low production cost, high production efficiency and high yield.
Description
Technical Field
The invention relates to the technical field of silicon tetrafluoride production, in particular to a method for producing silicon tetrafluoride by using sodium fluosilicate as a raw material and production equipment thereof.
Background
Silicon tetrafluoride, a colorless, toxic and irritating odor, is used mainly in the synthesis of hardeners for cement and artificial marble and organosilicon compounds; in the prior art, hydrofluoric acid (HF.H2O), sulfuric acid and quartz sand (silicon dioxide) are generally adopted for chemical reaction (namely, a mixture of the hydrofluoric acid, the sulfuric acid and the quartz sand is reacted at the reaction temperature of 110-130 ℃), but the scheme for preparing silicon tetrafluoride by adopting the scheme has the following defects:
firstly, hydrofluoric acid has high price and has the defect of high production cost;
secondly, the preparation method has the defects of high energy consumption and low preparation efficiency because the silicon tetrafluoride is produced only by heating the temperature to 110-130 ℃;
(III) because the silicon tetrafluoride needs to be collected after the reaction, but the gas types produced after the reaction are more and the reaction is slower (including poor stirring effect and small contact surface during the reaction) at present, the defect of low production efficiency also exists.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention aims to provide a method for producing silicon tetrafluoride by using sodium fluosilicate as a raw material and production equipment thereof, and aims to solve the defects of unfavorable popularization, high energy consumption and low preparation efficiency in the prior art.
The technical scheme of the invention is realized as follows: a method for producing silicon tetrafluoride by using sodium fluosilicate as a raw material, which is characterized by comprising the following steps:
(1) Mixing sulfuric acid and quartz sand, adding the mixture into a pulping tank, and stirring the mixture to form slurry;
(2) Continuously adding sodium fluosilicate into the reaction kettle through nitrogen in the stirring process of the slurry;
(3) After the sodium fluosilicate is added, adding part of the slurry uniformly mixed in the pulping tank into a reaction kettle in a nitrogen protection mode, and heating the temperature in the reaction kettle to 60-100 ℃ to enable the sodium fluosilicate to react with sulfuric acid and produce silicon tetrafluoride gas and hydrogen fluoride gas;
(4) The hydrogen fluoride gas produced in the step (3) can be dissolved with sulfuric acid to produce hydrofluoric acid solution, and the produced hydrofluoric acid solution further reacts with quartz sand in a reaction kettle to generate silicon tetrafluoride gas;
(5) And (3) introducing the silicon tetrafluoride gas and the hydrogen fluoride gas produced in the step (3) and the step (4) into a washing tower for washing, drying and collecting.
Preferably, it is: the quartz sand is silicon dioxide with the purity of 97-99%, and the sulfuric acid is dilute sulfuric acid with the concentration of 80-85%.
Preferably, it is: and (3) introducing the hydrogen fluoride gas separated in the step (5) into a pulping tank to react with quartz sand and produce silicon tetrafluoride gas.
By adopting the technical scheme: firstly, reacting sodium fluosilicate with sulfuric acid in a reaction kettle to produce silicon tetrafluoride gas, hydrogen fluoride gas and sodium sulfate crystals, introducing the produced silicon tetrafluoride gas and part of hydrogen fluoride gas into a drying tower for drying, collecting the dried silicon tetrafluoride, and introducing the separated hydrogen fluoride gas into a pulping tank; secondly, hydrogen fluoride and silicon dioxide in the beating tank react, silicon tetrafluoride and water are generated by the reaction of the hydrogen fluoride and the silicon dioxide, the silicon tetrafluoride generated in the beating tank is sent into a drying tower for drying and decomposition, and the dried silicon tetrafluoride is collected; it should be noted that: part of the hydrogen fluoride gas produced in the first step reacts with silicon dioxide in the reaction kettle and generates silicon tetrafluoride gas; the silicon tetrafluoride produced and prepared by the three aspects has the advantages of high production efficiency, hydrogen fluoride generated by the reaction of sodium fluosilicate and sulfuric acid can be further utilized, and resources can be mutually assisted and complemented for integrated utilization, so that the advantage of high resource utilization rate also exists; secondly, through a nitrogen-adding protection slurry transportation mode, air can be effectively discharged, so that only three gases of nitrogen, hydrogen fluoride and silicon tetrafluoride exist in the reaction process, the decomposition efficiency of mixed gases can be improved, and the preparation efficiency of the silicon tetrafluoride is further improved; in addition, sodium fluosilicate and sulfuric acid can react at normal temperature, and the reaction is optimal at the temperature of 60-100 ℃, so that the advantages of low production efficiency and further provision are also provided; and the cost of sodium fluosilicate is lower, and hydrogen fluoride required by production can be produced in the reaction process of sodium fluosilicate and other substances (sulfuric acid), so that the production cost is reduced.
In addition, the invention also provides production equipment for producing silicon tetrafluoride by using sodium fluosilicate as a raw material, which is characterized in that: comprises a beating groove, a reaction kettle and a drying tower which are communicated with each other; a nitrogen supply device for conveying nitrogen to the pulping tank and the reaction kettle is arranged between the pulping tank and the reaction kettle.
Preferably, it is: the pulping tank comprises a tank body which is in a truncated cone shape and is hollow, the outer walls of the two sides of the tank body are respectively and symmetrically communicated with conveying pipes, the communicating ends of the conveying pipes and the tank body extend to the bottom of the tank body along the circumferential direction of the inner wall of the tank body to form conveying tanks, and the free ends of the conveying tanks extend to the space between the bottom wall of the tank body and the bottom wall of the other conveying tank; the center of the outer wall of the bottom of the tank body is concavely provided with a guide column, the outer wall of the guide column is movably connected with a rotating ring which is driven to rotate by a motor, the side wall of the tank body is provided with a first discharge hole, the outer wall of the rotating ring is fixedly connected with a stirring assembly used for stirring materials in the tank body at intervals, the inner wall of the bottom of the tank body is radially provided with a plurality of positioning grooves for the stirring assembly to axially slide at intervals, and the bottom of each positioning groove is provided with a plurality of concave parts at intervals; the drying tower is communicated with the top of the tank body through an air inlet pipe; and a heater is arranged on the side wall of the tank body.
Preferably, it is: the stirring assembly comprises a stirring disc fixedly connected with the rotating ring, a plurality of circles of stirring rings penetrating through the inner cavity of the stirring disc from top to bottom are radially arranged on the stirring disc, stirring rings matched with the inner cavities are arranged in the inner cavities, two sides of the top edge of the inner cavity are fixedly connected through stirring arches arranged in a plurality of circumferential gaps, and a plurality of stirring tips are circumferentially arranged on the top end face of each stirring ring at intervals; the bottom of the stirring disc is radially and fixedly connected with a plurality of positioning blocks which move inside the positioning grooves, and the thickness of each positioning block is equal to the height from the concave part to the top of each positioning groove.
Preferably, it is: the reaction kettle comprises a kettle body and a storage device fixed in the kettle body, a first feed inlet communicated with a first discharge hole through a material conveying pipe is formed in the side wall, close to the bottom, of the kettle body, and a second feed inlet used for feeding materials into the storage device is formed in the side wall, close to the top, of the kettle body; the material storage device comprises a material storage tank body fixedly connected with the inner wall of the kettle body, a circular opening is formed in the bottom wall of the material storage tank body, a sliding channel is formed by extending the circular opening towards the bottom direction of the kettle body, cylindrical blocks matched with the sliding channel are connected in a sliding mode, second discharge holes are formed in the circumferential direction of the side wall of each cylindrical block close to the top at intervals, a plurality of material discharge channels are formed by extending towards the bottom of each cylindrical block, one end, far away from each second discharge hole, of each material discharge channel is communicated with a material discharge pipe, each material discharge pipe is spirally wound with each other and extends towards the bottom direction of the kettle body and is arranged in a forked mode towards the circumferential inner wall direction of the kettle body, and a lifting shaft driven by a hydraulic cylinder is fixedly connected to the top of each cylindrical block; the side wall of the kettle body is provided with an exhaust port which is communicated with the drying tower through an exhaust pipe; the bottom of the kettle body is provided with a heater.
Preferably, it is: the bottom inner wall of the storage tank body is gradually sunken from the edge to the circular opening, and the bottom inner wall of the storage tank body is fixedly connected with a plurality of distributing plates from the edge of the circular opening to the edge of the bottom inner wall at intervals circumferentially, the bottom inner wall of the storage tank body is divided into a plurality of guide grooves by the plurality of distributing plates, each guide groove corresponds to each second discharge hole one to one respectively, and one side, away from the bottom inner wall of the storage tank body, of each distributing plate is fixedly connected with a guide plate with a cross section of semi-oval shape.
Preferably, it is: the discharge end of the discharge pipe can be bent and obliquely arranged.
By adopting the technical scheme: firstly, sulfuric acid and quartz sand (namely silicon dioxide) can be respectively added into the tank body through conveying pipes at two sides of the tank body, and as the conveying tanks communicated with the conveying pipes are arranged in the tank body, the materials can be conveyed to the bottom of the tank body by the conveying tanks, and the free ends of the conveying tanks respectively extend to the position between the bottom wall of the tank body and the bottom wall of the other conveying tank; after two parts of materials are mixed, the stirring assembly is driven by the motor to stir the materials, because the inner cavity is radially arranged on the stirring disc, the stirring ring is arranged on the inner cavity, and the stirring tip is arranged on the stirring ring, and because the positioning block is arranged at the bottom of the stirring disc, the positioning groove is arranged at the bottom of the groove body, and the concave part is arranged at the bottom of the positioning groove, the positioning block is made to do circular motion in the positioning groove in the process of rotation of the stirring disc, when the positioning block passes through the concave part, the bottom of the stirring disc is attached to the bottom of the groove bottom, and when the positioning block is separated from the concave part, the bottom of the stirring disc is separated from the bottom of the groove bottom, so that the stirring disc is repeatedly lifted in the process of rotation, and the stirring efficiency of the materials is improved, namely: in the process of lifting movement of the stirring disc, the stirring tip can repeatedly puncture materials, and the stirring arch can stir the materials in time after the materials are punctured, so that two materials (namely sulfuric acid and quartz sand) are very easy to be quickly fused, and the mixing uniformity efficiency of the materials is improved, and the production efficiency is improved; it should be noted that: the guide post can realize the positioning function on the rotating ring, and can prevent the rotating ring from separating from the guide post in the process of lifting movement of the stirring disc, thereby ensuring the normal stirring; secondly, before feeding materials into the storage tank body, the cylindrical block can be lifted by the hydraulic cylinder and the lifting shaft, so that the bottom edge of the cylindrical block coincides with the circular opening, sodium fluosilicate is added into the storage tank body through the second feeding port, after the sodium fluosilicate is added, the second feeding port is closed, then slurry (namely, a mixture of sulfuric acid and quartz sand) at the inner part of the tank body is added into the tank body through the material conveying pipe, after the slurry is added, the cylindrical block is put down by driving the hydraulic cylinder, and the bottom edge of the second discharging port on the cylindrical block coincides with the edge of the circular opening, so that sodium fluosilicate in the storage tank body enters the bottom of the tank body through the material discharging channel and the material discharging pipe to react with the slurry; the material in the storage tank body can be respectively conveyed to different areas at the top of the slurry, so that the reaction efficiency of sodium fluosilicate and sulfuric acid is improved, the structural strength of the material discharge pipe can be improved due to the spiral winding, the discharge end of the material discharge pipe can be bent and obliquely arranged, and the sodium fluosilicate discharged from the material discharge pipe can be added into the slurry at a certain angle, so that the contact area of the sodium fluosilicate and the sulfuric acid is improved, and the efficiency of producing silicon tetrafluoride is further improved; the bottom inner wall of the storage tank body is gradually concavely arranged from the edge to the round opening, a plurality of distributing plates fixedly connected with the bottom inner wall of the storage tank body and guide plates fixedly connected with the distributing plates are arranged, and the arrangement can prevent sodium fluosilicate from remaining in the storage tank body when the storage tank body is used for discharging materials, so that the utilization rate of resources is improved; and the speed of sodium fluosilicate entering the discharge channel can be improved, so that the production efficiency can be improved.
The invention is further provided with: the top of the tank body is communicated with a nitrogen supply device through a gas supply pipe.
Preferably, it is: the nitrogen supply device comprises a nitrogen storage tank and a heat exchanger for vaporizing liquid nitrogen inside the nitrogen storage tank into nitrogen.
By adopting the technical scheme: the nitrogen gas feeding device can be used for feeding nitrogen gas into the reaction kettle and the pulping tank, and the aim of feeding the nitrogen gas is that: the reaction kettle and the rest of air in the pulping tank are discharged, and only three gases of nitrogen, hydrogen fluoride and silicon tetrafluoride exist in the reaction process, so that the rectification efficiency can be improved, and the preparation efficiency of the silicon tetrafluoride is further improved; it should be noted that: but nitrogen gas cyclic utilization in reation kettle and the beating groove to the nitrogen gas that can complement lack through the nitrogen gas feeding device at cell body top when inside atmospheric pressure is unstable or detect impurity air, this part nitrogen gas cyclic utilization that says, namely: after the reaction of the reaction kettle is finished, hydrogen fluoride, silicon tetrafluoride and nitrogen generated can be fed into the drying tower for rectification, and as the boiling point of the nitrogen, the hydrogen fluoride and the silicon tetrafluoride are different, the silicon tetrafluoride can be separated, and the nitrogen and the hydrogen fluoride are fed into the beating tank for further reaction of the hydrogen fluoride and the silicon dioxide in the beating tank, so that the silicon tetrafluoride is produced, and the efficiency of preparing the silicon tetrafluoride is improved.
To sum up: the present invention can produce silicon tetrafluoride referred to by three aspects: firstly, reacting sodium fluosilicate with sulfuric acid in a reaction kettle to produce silicon tetrafluoride gas and hydrogen fluoride gas; secondly, introducing the hydrogen fluoride gas produced in the first step into a pulping tank to further react with silicon dioxide in the slurry to produce silicon tetrafluoride again; thirdly, the hydrogen fluoride gas produced in the reaction kettle can react with slurry in the reaction kettle to further generate silicon tetrafluoride gas; the silicon tetrafluoride gas is produced through the three aspects, so that the production efficiency of the silicon tetrafluoride is improved.
Drawings
In order to more clearly illustrate the embodiments of the invention or the technical solutions of the prior art, the drawings which are used in the description of the embodiments or the prior art will be briefly described, it being obvious that the drawings in the description below are only some embodiments of the invention, and that other drawings can be obtained according to these drawings without inventive faculty for a person skilled in the art.
FIG. 1 is a block diagram of an embodiment 2 of the present invention;
fig. 2 is a schematic view of the structure of the beating tank in fig. 1;
FIG. 3 is a cross-sectional view A-A of FIG. 2;
FIG. 4 is a schematic structural view of the reaction vessel in FIG. 1;
fig. 5 is a B-B cross-sectional view of fig. 4.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
The invention discloses a method for producing silicon tetrafluoride by using sodium fluosilicate as a raw material, which is characterized by comprising the following steps:
(1) Mixing sulfuric acid and quartz sand, adding the mixture into a pulping tank, and stirring the mixture to form slurry;
(2) Continuously adding sodium fluosilicate into the reaction kettle through nitrogen in the stirring process of the slurry;
(3) After the sodium fluosilicate is added, adding part of the slurry uniformly mixed in the pulping tank into a reaction kettle in a nitrogen protection mode, and heating the temperature in the reaction kettle to 60-100 ℃ to enable the sodium fluosilicate to react with sulfuric acid and produce silicon tetrafluoride gas and hydrogen fluoride gas;
(4) The hydrogen fluoride gas produced in the step (3) can be dissolved with sulfuric acid to produce hydrofluoric acid solution, and the produced hydrofluoric acid solution further reacts with quartz sand in a reaction kettle to generate silicon tetrafluoride gas;
(5) And (3) introducing the silicon tetrafluoride gas and the hydrogen fluoride gas produced in the step (3) and the step (4) into a washing tower for washing, drying and collecting.
In the specific embodiment of the invention, the quartz sand is silicon dioxide with the purity of 97-99%, and the sulfuric acid is dilute sulfuric acid with the concentration of 80-85%.
In an embodiment of the present invention, the hydrogen fluoride gas separated in the step (5) may be introduced into a beating tank to react with quartz sand and produce silicon tetrafluoride gas.
By adopting the technical scheme: firstly, reacting sodium fluosilicate with sulfuric acid in a reaction kettle to produce silicon tetrafluoride gas, hydrogen fluoride gas and sodium sulfate crystals, introducing the produced silicon tetrafluoride gas and part of hydrogen fluoride gas into a drying tower for drying, collecting the dried silicon tetrafluoride, and introducing the separated hydrogen fluoride gas into a pulping tank; secondly, hydrogen fluoride and silicon dioxide in the beating tank react, silicon tetrafluoride and water are generated by the reaction of the hydrogen fluoride and the silicon dioxide, the silicon tetrafluoride generated in the beating tank is sent into a drying tower for drying and decomposition, and the dried silicon tetrafluoride is collected; it should be noted that: part of the hydrogen fluoride gas produced in the first step reacts with silicon dioxide in the reaction kettle and generates silicon tetrafluoride gas; the silicon tetrafluoride produced and prepared by the three aspects has the advantages of high production efficiency, hydrogen fluoride generated by the reaction of sodium fluosilicate and sulfuric acid can be further utilized, and resources can be mutually assisted and complemented for integrated utilization, so that the advantage of high resource utilization rate also exists; secondly, through a nitrogen-adding protection slurry transportation mode, air can be effectively discharged, so that only three gases of nitrogen, hydrogen fluoride and silicon tetrafluoride exist in the reaction process, the decomposition efficiency of mixed gases can be improved, and the preparation efficiency of the silicon tetrafluoride is further improved; in addition, sodium fluosilicate and sulfuric acid can react at normal temperature, and the reaction is optimal at the temperature of 60-100 ℃, so that the advantages of low production efficiency and further provision are also provided; and the cost of sodium fluosilicate is lower, and hydrogen fluoride required by production can be produced in the reaction process of sodium fluosilicate and other substances (sulfuric acid), so that the production cost is reduced.
Example 2
As shown in fig. 1 to 5, the invention discloses a production device for producing silicon tetrafluoride by using sodium fluosilicate as a raw material, and in the specific embodiment of the invention, the production device comprises a beating tank 1, a reaction kettle 2 and a drying tower 3 which are communicated with each other; a nitrogen gas supply device 4 for supplying nitrogen gas to the beating tank 1 and the reaction kettle 2 is arranged between them.
In the specific embodiment of the present invention, the pulping tank 1 includes a hollow tank body 11 having a "truncated cone shape", two outer walls of the tank body 11 are symmetrically connected with conveying pipes 12, the communicating ends of the conveying pipes 12 and the tank body 11 extend along the circumferential direction of the inner wall of the tank body 11 to the bottom of the tank body 11 to form conveying tanks 13, and the free ends of the conveying tanks 13 extend between the bottom wall of the tank body 11 and the bottom wall of another conveying tank 13; a guide column 111 is concavely formed from the center of the outer wall of the bottom of the tank body 11 to the inside of the tank body 11, a rotating ring 113 driven to rotate by a motor 112 is movably connected to the outer wall of the guide column 111, a first discharge hole 14 is formed in the side wall of the tank body 11, stirring assemblies 15 for stirring materials in the tank body 11 are fixedly connected to the outer wall of the rotating ring 113 at intervals, positioning grooves 16 for axially sliding the stirring assemblies 15 are radially arranged on the inner wall of the bottom of the tank body 11 at intervals, and a plurality of concave parts 161 are formed in the bottom of each positioning groove 16 at intervals; the drying tower 3 is communicated with the top of the tank body 11 through an air inlet pipe 17; the side wall of the tank body 11 is provided with a heater 18.
In the embodiment of the present invention, the stirring assembly 15 includes a stirring disc 151 fixedly connected to the rotating ring 113, a plurality of rings of stirring rings 151a penetrating the stirring disc 151 from top to bottom are radially disposed on the stirring disc 151, stirring rings 151b matching the inner cavities 151a are disposed in each inner cavity 151a, two sides of a top edge of each inner cavity 151a are fixedly connected through a plurality of stirring arches 151c disposed at circumferential gaps, and a plurality of stirring tips 151d are circumferentially disposed at intervals on top end surfaces of each stirring ring 151 b; a plurality of positioning blocks 151e which are movably arranged in the positioning grooves 16 are fixedly connected to the bottom of the stirring disc 151 in the radial direction, and the thickness of each positioning block 151e is equal to the height from the concave part to the groove top of the positioning groove 16.
In the embodiment of the present invention, the reaction kettle 2 includes a kettle body 21 and a material storage device 22 fixed in the kettle body 21, a first material inlet 212 communicating with the first material outlet 14 through a material transfer pipe 211 is provided on a sidewall of the kettle body 21 near the bottom, and a second material inlet 213 for adding material into the material storage device 22 is provided on a sidewall of the kettle body 21 near the top; the material storage device 22 comprises a material storage tank body 221 fixedly connected with the inner wall of the kettle body 21, a circular opening 221a is formed in the bottom wall of the material storage tank body 221, a sliding channel 221b is formed by extending the circular opening 221a towards the bottom direction of the kettle body 21, cylindrical blocks 221c matched with the sliding channel 221b are connected in the sliding channel 221b in a sliding manner, second material outlet holes 221d are formed in the circumferential spacing mode of the side wall of the cylindrical blocks 221c close to the top, a plurality of material outlet channels 221e are formed by extending the second material outlet holes 221d towards the bottom of the cylindrical blocks 221c, material outlet pipes 221f are communicated with one end, far away from the second material outlet holes 221d, of each material outlet channel 221e, each material outlet pipe 221f is spirally wound with each other and extends towards the bottom direction of the kettle body and is arranged in a forked manner towards the circumferential inner wall direction of the kettle body, and the top of the cylindrical blocks 221c is fixedly connected with a lifting shaft 25 driven by a hydraulic cylinder 24; the side wall of the kettle body is provided with an exhaust port 26, and the exhaust port 26 is communicated with the drying tower 3 through an exhaust pipe 261; the bottom of the kettle body 21 is provided with a heater 27.
In the embodiment of the invention, the bottom inner wall of the storage tank 221 is gradually recessed from the edge to the circular opening 221a, and a plurality of material separating plates 221g are fixedly connected between the edge of the circular opening 221a and the edge of the bottom inner wall at intervals in the circumferential direction, the bottom inner wall of the storage tank 221 is divided into a plurality of material guiding grooves 221k by the plurality of material separating plates 221h, each material guiding groove 221k corresponds to each second material outlet 221d one by one, and one side of each material separating plate 221d far away from the bottom inner wall of the storage tank 221 is fixedly connected with a material guiding plate 221m with a semi-oval cross section.
In an embodiment of the present invention, the discharge end of the discharge pipe 221f may be bent and inclined.
By adopting the technical scheme: firstly, sulfuric acid and quartz sand (namely silicon dioxide) can be respectively added into the tank body through conveying pipes at two sides of the tank body, and as the conveying tanks communicated with the conveying pipes are arranged in the tank body, the materials can be conveyed to the bottom of the tank body by the conveying tanks, and the free ends of the conveying tanks respectively extend to the position between the bottom wall of the tank body and the bottom wall of the other conveying tank; after two parts of materials are mixed, the stirring assembly is driven by the motor to stir the materials, because the inner cavity is radially arranged on the stirring disc, the stirring ring is arranged on the inner cavity, and the stirring tip is arranged on the stirring ring, and because the positioning block is arranged at the bottom of the stirring disc, the positioning groove is arranged at the bottom of the groove body, and the concave part is arranged at the bottom of the positioning groove, the positioning block is made to do circular motion in the positioning groove in the process of rotation of the stirring disc, when the positioning block passes through the concave part, the bottom of the stirring disc is attached to the bottom of the groove bottom, and when the positioning block is separated from the concave part, the bottom of the stirring disc is separated from the bottom of the groove bottom, so that the stirring disc is repeatedly lifted in the process of rotation, and the stirring efficiency of the materials is improved, namely: in the process of lifting movement of the stirring disc, the stirring tip can repeatedly puncture materials, and the stirring arch can stir the materials in time after the materials are punctured, so that two materials (namely sulfuric acid and quartz sand) are very easy to be quickly fused, and the mixing uniformity efficiency of the materials is improved, and the production efficiency is improved; it should be noted that: the guide post can realize the positioning function on the rotating ring, and can prevent the rotating ring from separating from the guide post in the process of lifting movement of the stirring disc, thereby ensuring the normal stirring; secondly, before feeding materials into the storage tank body, the cylindrical block can be lifted by the hydraulic cylinder and the lifting shaft, so that the bottom edge of the cylindrical block coincides with the circular opening, sodium fluosilicate is added into the storage tank body through the second feeding port, after the sodium fluosilicate is added, the second feeding port is closed, then slurry (namely, a mixture of sulfuric acid and quartz sand) at the inner part of the tank body is added into the tank body through the material conveying pipe, after the slurry is added, the cylindrical block is put down by driving the hydraulic cylinder, and the bottom edge of the second discharging port on the cylindrical block coincides with the edge of the circular opening, so that sodium fluosilicate in the storage tank body enters the bottom of the tank body through the material discharging channel and the material discharging pipe to react with the slurry; the material in the storage tank body can be respectively conveyed to different areas at the top of the slurry, so that the reaction efficiency of sodium fluosilicate and sulfuric acid is improved, the structural strength of the material discharge pipe can be improved due to the spiral winding, the discharge end of the material discharge pipe can be bent and obliquely arranged, and the sodium fluosilicate discharged from the material discharge pipe can be added into the slurry at a certain angle due to the arrangement, so that the contact area of the sodium fluosilicate and the sulfuric acid is improved, and the efficiency of producing silicon tetrafluoride is further improved; the bottom inner wall of the storage tank body is gradually concavely arranged from the edge to the round opening, a plurality of distributing plates fixedly connected with the bottom inner wall of the storage tank body and guide plates fixedly connected with the distributing plates are arranged, and the arrangement can prevent sodium fluosilicate from remaining in the storage tank body when the storage tank body is used for discharging materials, so that the utilization rate of resources is improved; and the speed of sodium fluosilicate entering the discharge channel can be improved, so that the production efficiency can be improved.
In the embodiment of the invention, the top of the tank 11 is communicated with a nitrogen supply device 4 through a gas supply pipe 41.
In an embodiment of the present invention, the nitrogen supply device 4 may be a nitrogen storage tank 42 and a heat exchanger 43 for vaporizing liquid nitrogen inside the nitrogen storage tank 42 into nitrogen.
By adopting the technical scheme: the nitrogen gas feeding device can be used for feeding nitrogen gas into the reaction kettle and the pulping tank, and the aim of feeding the nitrogen gas is that: the reaction kettle and the rest of air in the pulping tank are discharged, and only three gases of nitrogen, hydrogen fluoride and silicon tetrafluoride exist in the reaction process, so that the rectification efficiency can be improved, and the preparation efficiency of the silicon tetrafluoride is further improved; it should be noted that: but nitrogen gas cyclic utilization in reation kettle and the beating groove to the nitrogen gas that can complement lack through the nitrogen gas feeding device at cell body top when inside atmospheric pressure is unstable or detect impurity air, this part nitrogen gas cyclic utilization that says, namely: after the reaction of the reaction kettle is finished, hydrogen fluoride, silicon tetrafluoride and nitrogen generated can be fed into the drying tower for rectification, and as the boiling point of the nitrogen, the hydrogen fluoride and the silicon tetrafluoride are different, the silicon tetrafluoride can be separated, and the nitrogen and the hydrogen fluoride are fed into the beating tank for further reaction of the hydrogen fluoride and the silicon dioxide in the beating tank, so that the silicon tetrafluoride is produced, and the efficiency of preparing the silicon tetrafluoride is improved.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, alternatives, and improvements that fall within the spirit and scope of the invention.
Claims (7)
1. A method for producing silicon tetrafluoride by using sodium fluosilicate as a raw material, which is characterized by comprising the following steps:
(1) Mixing sulfuric acid and quartz sand, adding the mixture into a pulping tank, and stirring the mixture to form slurry;
(2) Continuously adding sodium fluosilicate into the reaction kettle through nitrogen in the stirring process of the slurry;
(3) After the sodium fluosilicate is added, adding part of the slurry uniformly mixed in the pulping tank into a reaction kettle in a nitrogen protection mode, and heating the temperature in the reaction kettle to 60-100 ℃ to enable the sodium fluosilicate to react with sulfuric acid and produce silicon tetrafluoride gas and hydrogen fluoride gas;
(4) The hydrogen fluoride gas produced in the step (3) can be dissolved with sulfuric acid to produce hydrofluoric acid solution, and the produced hydrofluoric acid solution further reacts with quartz sand in a reaction kettle to generate silicon tetrafluoride gas;
(5) Introducing the silicon tetrafluoride gas and the hydrogen fluoride gas produced in the step (3) and the step (4) into a washing tower for washing, drying and collecting;
the production equipment for producing silicon tetrafluoride by using sodium fluosilicate as a raw material comprises a pulping tank, a reaction kettle and a drying tower which are communicated with each other; a nitrogen supply device for conveying nitrogen to the pulping tank and the reaction kettle is arranged between the pulping tank and the reaction kettle;
the pulping tank comprises a tank body which is in a truncated cone shape and is hollow, the outer walls of the two sides of the tank body are respectively and symmetrically communicated with conveying pipes, the communicating ends of the conveying pipes and the tank body extend to the bottom of the tank body along the circumferential direction of the inner wall of the tank body to form conveying tanks, and the free ends of the conveying tanks extend to the space between the bottom wall of the tank body and the bottom wall of the other conveying tank; the center of the outer wall of the bottom of the tank body is concavely provided with a guide column, the outer wall of the guide column is movably connected with a rotating ring which is driven to rotate by a motor, the side wall of the tank body is provided with a first discharge hole, the outer wall of the rotating ring is fixedly connected with a stirring assembly used for stirring materials in the tank body at intervals, the inner wall of the bottom of the tank body is radially provided with a plurality of positioning grooves for the stirring assembly to axially slide at intervals, and the bottom of each positioning groove is provided with a plurality of concave parts at intervals; the drying tower is communicated with the top of the tank body through an air inlet pipe; a heater is arranged on the side wall of the tank body;
the stirring assembly comprises a stirring disc fixedly connected with the rotating ring, a plurality of circles of stirring rings penetrating through the inner cavity of the stirring disc from top to bottom are radially arranged on the stirring disc, stirring rings matched with the inner cavities are arranged in the inner cavities, two sides of the top edge of the inner cavity are fixedly connected through stirring arches arranged in a plurality of circumferential gaps, and a plurality of stirring tips are circumferentially arranged on the top end face of each stirring ring at intervals; the bottom of the stirring disc is radially and fixedly connected with a plurality of positioning blocks which move inside the positioning grooves, and the thickness of each positioning block is equal to the height from the concave part to the top of each positioning groove.
2. The method for producing silicon tetrafluoride using sodium fluosilicate as a raw material according to claim 1, characterized in that: the quartz sand is silicon dioxide with the purity of 97-99%, and the sulfuric acid is sulfuric acid with the concentration of 80-85%.
3. The method for producing silicon tetrafluoride using sodium fluosilicate as a raw material according to claim 1 or 2, characterized in that: and (3) introducing the hydrogen fluoride gas separated in the step (5) into a pulping tank to react with quartz sand and produce silicon tetrafluoride gas.
4. The method for producing silicon tetrafluoride using sodium fluosilicate as a raw material according to claim 1, characterized in that: the top of the tank body is communicated with a nitrogen supply device through a gas supply pipe.
5. The method for producing silicon tetrafluoride using sodium fluosilicate as a raw material according to claim 4, wherein: the nitrogen supply device comprises a nitrogen storage tank and a heat exchanger for vaporizing liquid nitrogen inside the nitrogen storage tank into nitrogen.
6. The method for producing silicon tetrafluoride using sodium fluosilicate as a raw material according to claim 1, characterized in that: the reaction kettle comprises a kettle body and a storage device fixed in the kettle body, a first feed inlet communicated with a first discharge hole through a material conveying pipe is formed in the side wall, close to the bottom, of the kettle body, and a second feed inlet used for feeding materials into the storage device is formed in the side wall, close to the top, of the kettle body; the material storage device comprises a material storage tank body fixedly connected with the inner wall of the kettle body, a circular opening is formed in the bottom wall of the material storage tank body, a sliding channel is formed by extending the circular opening towards the bottom direction of the kettle body, cylindrical blocks matched with the sliding channel are connected in a sliding mode, second discharge holes are formed in the circumferential direction of the side wall of each cylindrical block close to the top at intervals, a plurality of material discharge channels are formed by extending towards the bottom of each cylindrical block, one end, far away from each second discharge hole, of each material discharge channel is communicated with a material discharge pipe, each material discharge pipe is spirally wound with each other and extends towards the bottom direction of the kettle body and is arranged in a forked mode towards the circumferential inner wall direction of the kettle body, and a lifting shaft driven by a hydraulic cylinder is fixedly connected to the top of each cylindrical block; the side wall of the kettle body is provided with an exhaust port which is communicated with the drying tower through an exhaust pipe; the bottom of the kettle body is provided with a heater.
7. The method for producing silicon tetrafluoride using sodium fluosilicate as a raw material according to claim 6, characterized in that: the bottom inner wall of the storage tank body is gradually sunken from the edge to the circular opening, and the bottom inner wall of the storage tank body is fixedly connected with a plurality of distributing plates from the edge of the circular opening to the edge of the bottom inner wall at intervals circumferentially, the bottom inner wall of the storage tank body is divided into a plurality of guide grooves by the plurality of distributing plates, each guide groove corresponds to each second discharge hole one to one respectively, and one side, away from the bottom inner wall of the storage tank body, of each distributing plate is fixedly connected with a guide plate with a cross section of semi-oval shape.
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