CN113292076B - Technology for smelting and recycling silicon tetrachloride slag slurry after cold hydrogenation process - Google Patents
Technology for smelting and recycling silicon tetrachloride slag slurry after cold hydrogenation process Download PDFInfo
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- CN113292076B CN113292076B CN202110676902.7A CN202110676902A CN113292076B CN 113292076 B CN113292076 B CN 113292076B CN 202110676902 A CN202110676902 A CN 202110676902A CN 113292076 B CN113292076 B CN 113292076B
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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
- C01B33/02—Silicon
- C01B33/037—Purification
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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
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
- F27B14/00—Crucible or pot furnaces
- F27B14/06—Crucible or pot furnaces heated electrically, e.g. induction crucible furnaces with or without any other source of heat
- F27B14/061—Induction furnaces
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
- F27B14/00—Crucible or pot furnaces
- F27B14/08—Details peculiar to crucible or pot furnaces
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
- F27B14/00—Crucible or pot furnaces
- F27B14/08—Details peculiar to crucible or pot furnaces
- F27B14/10—Crucibles
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
- F27B14/00—Crucible or pot furnaces
- F27B14/08—Details peculiar to crucible or pot furnaces
- F27B14/14—Arrangements of heating devices
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- Engineering & Computer Science (AREA)
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- Organic Chemistry (AREA)
- Mechanical Engineering (AREA)
- General Engineering & Computer Science (AREA)
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- Silicon Compounds (AREA)
Abstract
The invention relates to a technology for smelting and recovering silicon tetrachloride slag slurry after a cold hydrogenation process, which comprises the following steps of S1: preprocessing silicon tetrachloride slag; s2: adding sodium carbonate; s3: adding sodium metasilicate pentahydrate; s4: adding fluorite powder; s5: heating in a heating furnace; s6: filtering impurities; in order to realize the full utilization of silicon resources, silicon tetrachloride slag slurry after a cold hydrogenation process is smelted to recover the silicon resources, sodium carbonate is added to carry out slagging, sodium metasilicate pentahydrate is used as a covering agent to resist high-temperature oxidation, and fluorite powder is used to increase the fluidity of a molten silicon solution; the special graphite crucible is adopted for smelting the silicon tetrachloride slag slurry, so that the recycling of silicon resources is ensured.
Description
Technical Field
The invention relates to the technical field of smelting of silicon tetrachloride slag slurry, in particular to a technology for smelting and recovering silicon tetrachloride slag slurry after a cold hydrogenation process.
Background
The cold hydrogenation is a process system for converting a large amount of byproduct Silicon Tetrachloride (STC) generated in the reduction furnace in the production of the polycrystalline silicon into Trichlorosilane (TCS) which is a raw material for synthesizing the polycrystalline silicon; the raw materials of the process system comprise silicon powder, STC, hydrogen, HCl and the like, the reaction products comprise hydrogen, a mixture of STC and TCS, metal chloride and unreacted silicon powder, and the related reaction equation comprises Si +2H2+3SiCl4＝4SiHCl3；Si+3HCl＝SiHCl3+H2. The system separates most useful materials such as TCS, STC, hydrogen and the like through a quencher, and cools wet slurry (namely silicon tetrachloride slag slurry mainly comprising silicon powder and gold) after quenching of a hydrogenation process systemBelonging to chloride, liquid chlorosilane and hydrogen) to a slurry drying device; the slurry drying device is used for drying and heating wet slurry, evaporating chlorosilane gas and hydrogen for recovery, and neutralizing dried solid and alkali liquor.
The silicon tetrachloride slag slurry is generally prepared into hydrochloric acid and silicon slag by hydrolysis and pressure filtration, the hydrochloric acid is generally neutralized and salified by alkali and then discharged, and the silicon slag is buried, so that a large amount of water resources are wasted for treatment, the cost is high, and the silicon tetrachloride slag slurry is not environment-friendly.
Disclosure of Invention
The invention aims to solve the technical problem of providing a technology for smelting and recovering silicon tetrachloride slag slurry after a cold hydrogenation process, and can solve the problems that hydrochloric acid and silicon slag are formed by adopting hydrolysis and filter pressing in the smelting of the common silicon tetrachloride slag slurry, the treatment of byproducts is troublesome and the cost is high.
In order to solve the technical problems, the technical scheme of the invention is as follows: a technology for smelting and recovering silicon tetrachloride slag slurry after a cold hydrogenation process is characterized by comprising the following innovation points: the specific process comprises the following steps:
s1: preprocessing silicon tetrachloride slag: granulating the silicon tetrachloride slag through a granulator, and drying the granulated silicon tetrachloride slag through a dryer;
s2: adding sodium carbonate: putting the dried silicon tetrachloride slag into a heating furnace with a graphite crucible, and adding sodium carbonate into the silicon tetrachloride, wherein the mass ratio of the sodium carbonate to the silicon tetrachloride is (2-4): 100, used for realizing slagging;
s3: adding sodium metasilicate pentahydrate: and adding sodium metasilicate pentahydrate into the heating furnace again, wherein the mass ratio of the sodium metasilicate pentahydrate to the silicon tetrachloride is (14-16): 100, respectively;
s4: adding fluorite powder: adding fluorite powder into the heating furnace, wherein the mass ratio of the fluorite powder to the silicon tetrachloride is 0.8-1.2: 100, respectively; increasing the fluidity of the silicon solution;
s5: heating by a heating furnace: heating the heating furnace to 1400 ℃ and 1500 ℃ to completely melt the silicon tetrachloride slag, wherein the sodium metasilicate is lower in density than the silicon tetrachloride slag and floats on the surface of the silicon tetrachloride to serve as a covering agent, and oxygen is isolated from the surface of the molten silicon slag to resist high-temperature oxidation;
s6: impurity filtration: filtering the silicon tetrachloride slag after the addition and the reaction of the auxiliary agent are completed, and removing impurities; 50% of 90 silicon, 15% of 60-70 silicon, 10% of 50 silicon and 25% of silicon dioxide can be obtained.
Furthermore, the heating furnace with the graphite crucible in the S1 comprises a heating furnace body and a graphite inner container; the graphite inner container is arranged in the heating furnace body;
the heating furnace body is of a cylindrical structure and is provided with a cavity for accommodating the graphite inner container, the inner side wall of the heating furnace body is provided with a cavity for accommodating the water coil from top to bottom along the circumferential direction, and the cavity is internally provided with the water coil to heat the inner cavity in the heating furnace body; a guide groove matched with the graphite inner container is arranged on the inner wall of the heating furnace body along the vertical direction; the bottom end of the heating furnace body is horizontally provided with a locking plate extending out of the edge of the heating furnace body; the bottom end of the heating furnace body is provided with a discharge hole matched with the graphite inner container;
the graphite liner comprises a graphite end socket and a graphite cylinder; the graphite end socket is arranged at the top end of the graphite barrel, a tail gas outlet is arranged at the center of the graphite end socket, and a feeding hole and a temperature measuring hole are respectively arranged at two sides of the tail gas outlet; the graphite end socket is provided with a pressing plate, the outer diameter of the pressing plate is larger than that of the heating furnace body, the edge of the pressing plate is provided with a locking pull rod along the vertical direction, two ends of the locking pull rod are respectively connected to the pressing plate and the locking plate, and the graphite end socket is pressed on the graphite barrel through the matching of a bolt and the locking pull rod; the graphite cylinder body is of a cylindrical structure, the top end of the graphite cylinder body is open, and the bottom end of the graphite cylinder body is provided with a discharge hole matched with a discharge hole of the heating furnace body; the top end of the graphite cylinder body is provided with a step surface matched with the graphite end socket; and a guide block matched with the guide groove on the inner wall of the heating furnace body is arranged on the outer wall of the graphite cylinder body along the vertical direction.
Further, the graphite cylinder is formed by stacking a plurality of annular cylinder units.
Furthermore, the side of graphite head is provided with the lug, realizes hoisting the graphite head on the top of graphite barrel through hoist and mount.
The invention has the advantages that:
1) in order to realize the full utilization of silicon resources, silicon tetrachloride slag slurry after a cold hydrogenation process is smelted to recover the silicon resources, sodium carbonate is added to carry out slagging, sodium metasilicate pentahydrate is used as a covering agent to resist high-temperature oxidation, and fluorite powder is used to increase the fluidity of a molten silicon solution; the special graphite crucible is adopted for smelting the silicon tetrachloride slag slurry, so that the recycling of silicon resources is ensured.
Drawings
The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
FIG. 1 is a flow chart of a smelting recovery technology of silicon tetrachloride slag slurry after a cold hydrogenation process.
FIG. 2 is a heating furnace structure of the silicon tetrachloride slag slurry smelting recovery technology after the cold hydrogenation process.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. The components of embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations.
Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that: like reference numbers and letters refer to like items in the following figures, and thus, once an item is defined in one figure, it need not be further defined and explained in subsequent figures.
In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc. indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings or the orientations or positional relationships that the products of the present invention are conventionally placed in use, and are only used for convenience in describing the present invention and simplifying the description, but do not indicate or imply that the devices or elements referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first," "second," "third," and the like are used solely to distinguish one from another and are not to be construed as indicating or implying relative importance.
Furthermore, the terms "horizontal", "vertical" and the like do not imply that the components are required to be absolutely horizontal or pendant, but rather may be slightly inclined. For example, "horizontal" merely means that the direction is more horizontal than "vertical" and does not mean that the structure must be perfectly horizontal, but may be slightly inclined.
In the description of the present invention, it should also be noted that, unless otherwise explicitly stated or limited, the terms "disposed," "mounted," "connected," and "connected" are to be construed broadly and may be, for example, fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
The technology for smelting and recovering silicon tetrachloride slag slurry after the cold hydrogenation process shown in figure 1 comprises the following specific processes:
s1: preprocessing silicon tetrachloride slag: granulating the silicon tetrachloride slag through a granulator, and drying the granulated silicon tetrachloride slag through a dryer;
s2: adding sodium carbonate: putting the dried silicon tetrachloride slag into a heating furnace with a graphite crucible, and adding sodium carbonate into the silicon tetrachloride, wherein the mass ratio of the sodium carbonate to the silicon tetrachloride is 3: 100, used for realizing slagging;
s3: adding sodium metasilicate pentahydrate: adding sodium metasilicate pentahydrate into the heating furnace again, wherein the mass ratio of the sodium metasilicate pentahydrate to the silicon tetrachloride is 15: 100, respectively;
s4: adding fluorite powder: adding fluorite powder into the heating furnace, wherein the mass ratio of the fluorite powder to the silicon tetrachloride is 1: 100, respectively; the fluidity of the silicon solution is increased;
s5: heating by a heating furnace: heating the heating furnace to 1400-1500 ℃ to completely melt the silicon tetrachloride slag, wherein the density of the sodium metasilicate is lower than that of the silicon tetrachloride slag, so that the sodium metasilicate floats on the surface of the silicon tetrachloride to serve as a covering agent, and oxygen is isolated on the surface of the silicon slag in a molten state to resist high-temperature oxidation;
s6: impurity filtration: filtering the silicon tetrachloride slag after the addition and the reaction of the auxiliary agent are completed, and removing impurities; 50% of 90 silicon, 15% of 60-70 silicon, 10% of 50 silicon and 25% of silicon dioxide can be obtained.
As shown in fig. 2, the heating furnace with the graphite crucible in S1 includes a heating furnace body 1 and a graphite inner container 2; the graphite inner container 2 is arranged in the heating furnace body 1.
The heating furnace body 1 is of a cylindrical structure, the heating furnace body 1 is provided with a cavity for accommodating a graphite inner container, the inner side wall of the heating furnace body 1 is provided with a cavity for accommodating a water coil from top to bottom along the circumferential direction, and the cavity is internally provided with a water coil 11 for heating an inner cavity in the heating furnace body 1; a guide groove matched with the graphite inner container 2 is arranged on the inner wall of the heating furnace body 1 along the vertical direction; the bottom end of the heating furnace body 1 is horizontally provided with a locking plate 12 extending out of the edge of the heating furnace body; the bottom end of the heating furnace body 1 is provided with a discharge hole matched with the graphite liner 2.
The graphite liner 2 comprises a graphite end socket 21 and a graphite cylinder 22; the graphite end socket 21 is arranged at the top end of the graphite cylinder 22, a tail gas outlet 23 is arranged at the central position of the graphite end socket 21, and a feeding hole 24 and a temperature measuring hole 25 are respectively arranged at two sides of the tail gas outlet 23; a compression plate 26 is arranged on the graphite end socket 21, the outer diameter of the compression plate 26 is larger than that of the heating furnace body 1, a locking pull rod 27 is arranged on the edge of the compression plate 26 along the vertical direction, two ends of the locking pull rod 27 are respectively connected to the compression plate 26 and the locking plate 12, and the graphite end socket 21 is compressed on the graphite cylinder body 22 through the matching of a bolt and the locking pull rod 27; the graphite cylinder 22 is in a cylindrical structure, the top end of the graphite cylinder is open, and the bottom end of the graphite cylinder is provided with a discharge hole 221 matched with a discharge hole of the heating furnace body 1; the top end of the graphite cylinder 22 is provided with a step surface matched with the graphite end socket; and a guide block 222 matched with the guide groove on the inner wall of the heating furnace body is arranged on the outer wall of the graphite cylinder 22 along the vertical direction.
The graphite cylinder 22 is formed by stacking a plurality of annular cylinder units.
The side of graphite head 21 is provided with the lug, realizes hoisting graphite head 21 on the top of graphite barrel 22 through hoist and mount.
It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (4)
1. A technology for smelting and recovering silicon tetrachloride slag slurry after a cold hydrogenation process is characterized by comprising the following steps: the specific process comprises the following steps:
s1: preprocessing silicon tetrachloride slag: granulating the silicon tetrachloride slag through a granulator, and drying the granulated silicon tetrachloride slag through a dryer;
s2: adding sodium carbonate: putting the dried silicon tetrachloride slag into a heating furnace with a graphite crucible, and adding sodium carbonate into the silicon tetrachloride, wherein the mass ratio of the sodium carbonate to the silicon tetrachloride is (2-4): 100, used for realizing slagging;
s3: adding sodium metasilicate pentahydrate: adding sodium metasilicate pentahydrate into the heating furnace again, wherein the mass ratio of the sodium metasilicate pentahydrate to the silicon tetrachloride is 14-16: 100, respectively;
s4: adding fluorite powder: adding fluorite powder into the heating furnace, wherein the mass ratio of the fluorite powder to the silicon tetrachloride is 0.8-1.2: 100, respectively; the fluidity of the silicon solution is increased;
s5: heating by a heating furnace: heating the heating furnace to 1400 ℃ and 1500 ℃ to completely melt the silicon tetrachloride slag, wherein the sodium metasilicate is lower in density than the silicon tetrachloride slag and floats on the surface of the silicon tetrachloride to serve as a covering agent, and oxygen is isolated from the surface of the molten silicon slag to resist high-temperature oxidation;
s6: impurity filtering: filtering the silicon tetrachloride slag after the addition and the reaction of the auxiliary agent are completed, and removing impurities; 50% of 90 silicon, 15% of 60-70 silicon, 10% of 50 silicon and 25% of silicon dioxide can be obtained.
2. The technology for smelting and recovering silicon tetrachloride slag slurry after the cold hydrogenation process, as claimed in claim 1, is characterized in that: the heating furnace with the graphite crucible in the S1 comprises a heating furnace body and a graphite inner container; the graphite inner container is arranged in the heating furnace body;
the heating furnace body is of a cylindrical structure and is provided with a cavity for accommodating the graphite inner container, the inner side wall of the heating furnace body is provided with a cavity for accommodating the water coil from top to bottom along the circumferential direction, and the cavity is internally provided with the water coil to heat the inner cavity in the heating furnace body; a guide groove matched with the graphite inner container is arranged on the inner wall of the heating furnace body along the vertical direction; the bottom end of the heating furnace body is horizontally provided with a locking plate extending out of the edge of the heating furnace body; the bottom end of the heating furnace body is provided with a discharge hole matched with the graphite inner container;
the graphite liner comprises a graphite end socket and a graphite cylinder; the graphite end socket is arranged at the top end of the graphite barrel, a tail gas outlet is arranged at the center of the graphite end socket, and a feeding hole and a temperature measuring hole are respectively arranged at two sides of the tail gas outlet; the graphite end socket is provided with a pressing plate, the outer diameter of the pressing plate is larger than that of the heating furnace body, the edge of the pressing plate is provided with a locking pull rod along the vertical direction, two ends of the locking pull rod are respectively connected to the pressing plate and the locking plate, and the graphite end socket is pressed on the graphite barrel through the matching of a bolt and the locking pull rod; the graphite cylinder body is of a cylindrical structure, the top end of the graphite cylinder body is open, and the bottom end of the graphite cylinder body is provided with a discharge hole matched with a discharge hole of the heating furnace body; the top end of the graphite cylinder body is provided with a stepped surface matched with the graphite end socket; and a guide block matched with the guide groove on the inner wall of the heating furnace body is arranged on the outer wall of the graphite cylinder body along the vertical direction.
3. The technology for smelting and recovering silicon tetrachloride slag slurry after the cold hydrogenation process, as claimed in claim 2, is characterized in that: the graphite cylinder is formed by stacking a plurality of annular cylinder units.
4. The technology for smelting and recovering silicon tetrachloride slag slurry after the cold hydrogenation process, as claimed in claim 2, is characterized in that: the side of graphite head is provided with the lug, realizes hoisting the graphite head on the top of graphite barrel through hoist and mount.
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| CN202110676902.7A CN113292076B (en) | 2021-06-18 | 2021-06-18 | Technology for smelting and recycling silicon tetrachloride slag slurry after cold hydrogenation process |
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| CN202110676902.7A CN113292076B (en) | 2021-06-18 | 2021-06-18 | Technology for smelting and recycling silicon tetrachloride slag slurry after cold hydrogenation process |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101774584A (en) * | 2009-01-09 | 2010-07-14 | 华南师范大学 | Method for purifying solar-grade silicon |
| CN102344142A (en) * | 2010-07-26 | 2012-02-08 | 比亚迪股份有限公司 | Method for purifying silicon through removing boron |
| CN210486455U (en) * | 2019-09-18 | 2020-05-08 | 苏州诺曼比尔材料科技有限公司 | Graphite heating vacuum tube sintering equipment for 3D printing of medical metal implant |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101774584A (en) * | 2009-01-09 | 2010-07-14 | 华南师范大学 | Method for purifying solar-grade silicon |
| CN102344142A (en) * | 2010-07-26 | 2012-02-08 | 比亚迪股份有限公司 | Method for purifying silicon through removing boron |
| CN210486455U (en) * | 2019-09-18 | 2020-05-08 | 苏州诺曼比尔材料科技有限公司 | Graphite heating vacuum tube sintering equipment for 3D printing of medical metal implant |
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