CN117568620B - Crude tin double-pot sulfur adding and impurity removing reactor - Google Patents
Crude tin double-pot sulfur adding and impurity removing reactor Download PDFInfo
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- CN117568620B CN117568620B CN202311633932.5A CN202311633932A CN117568620B CN 117568620 B CN117568620 B CN 117568620B CN 202311633932 A CN202311633932 A CN 202311633932A CN 117568620 B CN117568620 B CN 117568620B
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- sulfur
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- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 title claims abstract description 82
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 title claims abstract description 74
- 239000011593 sulfur Substances 0.000 title claims abstract description 70
- 229910052717 sulfur Inorganic materials 0.000 title claims abstract description 70
- 239000012535 impurity Substances 0.000 title claims abstract description 21
- 238000004891 communication Methods 0.000 claims abstract description 25
- 239000000463 material Substances 0.000 claims abstract description 19
- 238000003756 stirring Methods 0.000 claims abstract description 16
- 230000007246 mechanism Effects 0.000 claims description 3
- 239000007788 liquid Substances 0.000 abstract description 87
- 239000000779 smoke Substances 0.000 abstract description 5
- 239000000428 dust Substances 0.000 abstract description 3
- 238000002156 mixing Methods 0.000 abstract description 3
- 238000002485 combustion reaction Methods 0.000 abstract description 2
- 238000002955 isolation Methods 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 239000010949 copper Substances 0.000 description 34
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 29
- 229910052802 copper Inorganic materials 0.000 description 29
- 239000002893 slag Substances 0.000 description 25
- 238000006243 chemical reaction Methods 0.000 description 22
- 238000000034 method Methods 0.000 description 14
- 230000008569 process Effects 0.000 description 12
- 101100298225 Caenorhabditis elegans pot-2 gene Proteins 0.000 description 11
- 101100298222 Caenorhabditis elegans pot-1 gene Proteins 0.000 description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 9
- 238000010586 diagram Methods 0.000 description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 8
- 238000007670 refining Methods 0.000 description 7
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 6
- 238000007599 discharging Methods 0.000 description 6
- 229910052760 oxygen Inorganic materials 0.000 description 6
- 239000001301 oxygen Substances 0.000 description 6
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 238000004090 dissolution Methods 0.000 description 4
- 229910052742 iron Inorganic materials 0.000 description 4
- 229910052757 nitrogen Inorganic materials 0.000 description 4
- 239000007789 gas Substances 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- 230000008018 melting Effects 0.000 description 3
- 238000005272 metallurgy Methods 0.000 description 3
- 229910052785 arsenic Inorganic materials 0.000 description 2
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- AQMRBJNRFUQADD-UHFFFAOYSA-N copper(I) sulfide Chemical compound [S-2].[Cu+].[Cu+] AQMRBJNRFUQADD-UHFFFAOYSA-N 0.000 description 2
- OMZSGWSJDCOLKM-UHFFFAOYSA-N copper(II) sulfide Chemical compound [S-2].[Cu+2] OMZSGWSJDCOLKM-UHFFFAOYSA-N 0.000 description 2
- 238000007667 floating Methods 0.000 description 2
- 238000011010 flushing procedure Methods 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000010079 rubber tapping Methods 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000005987 sulfurization reaction Methods 0.000 description 2
- 238000012546 transfer Methods 0.000 description 2
- WHBHBVVOGNECLV-OBQKJFGGSA-N 11-deoxycortisol Chemical compound O=C1CC[C@]2(C)[C@H]3CC[C@](C)([C@@](CC4)(O)C(=O)CO)[C@@H]4[C@@H]3CCC2=C1 WHBHBVVOGNECLV-OBQKJFGGSA-N 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 239000011133 lead Substances 0.000 description 1
- -1 meanwhile Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005192 partition Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B25/00—Obtaining tin
- C22B25/08—Refining
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B25/00—Obtaining tin
- C22B25/02—Obtaining tin by dry processes
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/006—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals with use of an inert protective material including the use of an inert gas
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
- C22B9/10—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals with refining or fluxing agents; Use of materials therefor, e.g. slagging or scorifying agents
- C22B9/103—Methods of introduction of solid or liquid refining or fluxing agents
-
- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a crude tin double-pot sulphuration impurity removal reactor, which comprises: the device comprises a first pot body, a second pot body and a communication device, wherein the first pot body is of a closed structure, a closed feeding device and a first stirrer are arranged on the first pot body, the closed feeding device is used for adding sulfur, and the first stirrer is used for stirring materials in the first pot body; the second pot body is communicated with the first pot body through the communication device, and a second stirrer is arranged on the second pot body and is identical to the first stirrer in structure and used for stirring materials in the second pot body. The crude tin double-pot sulfur-adding impurity-removing reactor adopts a double-pot structure, and can realize the isolation, mixing and unified collection of scum of liquid in two pot bodies through controlling the rotating speed and the steering of two stirrers. Solves the problems of contact combustion of sulfur and air due to overhigh temperature when the traditional metal impurity removing pot is used for adding sulfur and removing impurities, reduces sulfur loss, avoids SO 2 smoke generation, reduces smoke dust to interfere operation and pollutes the environment.
Description
Technical Field
The invention relates to the technical field of vacuum metallurgy, in particular to a crude tin double-pot sulfur-adding and impurity-removing reactor which is used for adding sulfur and removing copper to crude tin.
Background
With the increasing reduction of tin ore resources, low-grade tin ore is increased, crude tin obtained by smelting low-grade tin concentrate contains more impurities, and the requirements on the purity of refined tin for industrial application are increasingly strict, so that a tin fire refining process consisting of various operations is formed. The fire refining of tin refers to the process of removing impurities in crude tin at a temperature higher than the melting point of tin to produce refined tin, and is an important component of the tin metallurgy process, and the fire refining mainly removes impurities such as iron, copper, lead, bismuth, arsenic, antimony and the like in the crude tin.
The removal of copper by sulphuration is a necessary stage of the fire refining of crude tin and is now well established. The basic principle of the sulfur-adding and copper-removing is that sulfur is added into liquid crude tin and is strongly stirred based on the fact that the affinity of sulfur and copper is larger than that of sulfur and tin, most of the added sulfur is firstly dissolved in the tin liquid due to the large concentration of the tin liquid, meanwhile, copper in the tin liquid and sulfur are combined to generate stable cuprous sulfide sulfur and copper to generate cuprous sulfide (Cu 2 S), the melting point is high (1130 ℃), the density is small (5.6 g/cm 3), and the copper-adding and copper-removing agent is insoluble in tin and floats on the surface of the tin liquid to generate sulfur slag. The sulfur addition can remove iron, and generally, the iron is removed by condensation firstly and then the copper is removed by sulfur addition, but if the copper content of the crude tin is more than 0.5%, the copper is removed by sulfur addition firstly and then the iron and the arsenic are removed by condensation.
In chinese patent CN102492861a, a method for fire refining of crude tin is disclosed, which uses conventional methods for sulphidation and copper removal. The traditional method uses a single pot to remove copper, all operations are completed in one open container, the problem that sulfur element is easy to directly burn exists, redundant smoke dust can be generated, efficiency is reduced, and observation and sampling are not easy.
Disclosure of Invention
The invention provides a double-pot crude tin sulphuration and impurity removal reactor for realizing sulphuration and copper removal technology in crude tin fire refining, which aims to solve the problems of low efficiency, poor operation environment, large environmental pollution, large labor intensity of workers and the like of the traditional crude tin sulphuration and copper removal equipment.
Specifically, the invention is realized as follows:
A crude tin double pot sulfur impurity removal reactor comprising:
The first pot body is of a closed structure, a closed feeding device and a first stirrer are arranged on the first pot body, the closed feeding device is used for adding materials, and the first stirrer is used for stirring the materials in the first pot body;
The second pot body is communicated with the first pot body through a communication device, and is provided with a second stirrer, and the second stirrer has the same structure as the first stirrer and is used for stirring materials in the second pot body;
two ends of the communication device are respectively overlapped with the tangential directions outside the first pot body and the second pot body;
the communication device is used for:
1) Isolating materials in the first pot body and the second pot body when the first stirrer and the second stirrer rotate reversely and at the same speed;
2) When the first stirrer and the second stirrer rotate in the same direction and at the same speed, the materials in the first pot body and the second pot body are communicated, so that the materials in the first pot body and the second pot body are mixed;
3) When the first stirrer and the second stirrer rotate in the same direction and at different speeds and the rotating speed of the first stirrer is larger than that of the second stirrer, materials in the first pot body and the second pot body are communicated, so that scum in the first pot body enters the second pot body.
Further, the communication device includes:
the two ends of the communication shell are respectively connected with the first pot body and the second pot body, and the inside of the communication shell is communicated with the first pot body and the second pot body;
The dredging piece is arranged in the middle of the communication shell, and a first channel and a second channel are formed between the dredging piece and two sides of the communication shell.
Further, one end of the dredging piece, which is close to the first pot body, and one end of the dredging piece, which is close to the second pot body, are arc parts concentric with the pot bodies on two sides and with the same radius; the side of the dredging piece, which is close to the first channel, is a straight part. The connecting channel is isolated into two small channels positioned at two sides of the channel, and the cross section of the channel is about 3-8% in proportion to the cross section of the cylindrical pot body, so that the liquids in the two pots can be uniformly mixed within 1-3 minutes. The structure is characterized in that when the liquid in the two pot bodies rotates at high speed, a part of the liquid in the lower part is thrown out along the tangential direction, and reaches the other pot body through the small channel along the tangential direction, so that the liquid in the two pot bodies can be circularly mixed.
Further, the two pot bodies are combined into a pot body with a long waist structure, and the communication shell is tangent with the shells of the two pot bodies.
Further, the second pot body is provided with a slag dragging device, and the slag dragging device is used for dragging scum in the second pot body.
Further, the slag scooping device is a vertically arranged screw conveyor, one end of the slag scooping device, which extends into the second pot body, is provided with a semi-open type conduit mechanism, the scum is discharged from the semi-open type conduit to enter the screw conveyor, the screw conveyor is used for realizing slag-liquid separation in the second pot body, and the scum is conveyed to a designated position.
Further, the airtight feeding device is a screw feeder, and a motor drives a screw blade to convey the material in the storage bin into the feeding port.
Further, the first/second stirrer drives the first/second stirring paddles by the variable frequency motor and the speed reducer, so that the stirring functions of forward and reverse directions and different speeds can be realized.
The working principle of the invention is as follows:
The working state is as follows: sulfur addition and sulfur dissolution state
At the moment, the first stirrer rotates at a forward high speed, the second stirrer rotates at a reverse high speed, and the rotating speed of the first stirrer and the second stirrer is more than 380r/min; the feeding device slowly adds the sulfur in the feed bin into the first pot body, controls the temperature of tin liquid (240-260 ℃) to enable the tin liquid to be completely dissolved in the liquid in the first pot body, and slowly reacts (Sn+S- & gtSnS). Because the first stirrer and the second stirrer are opposite in steering and same in rotating speed, the liquids in the two pot bodies are also reversely rotated at the same speed, so that the first channel and the second channel are opposite in opposite impact, the liquid in the channel cannot form a passage, the isolated liquids circulate in the two pot bodies respectively, the dissolution of sulfur is ensured to be carried out in the first pot body only, and unreacted elemental sulfur is prevented from being discharged from the second pot body. Or the rotating speed of the first stirrer can be selected to be smaller than that of the second stirrer according to the size of the pot and the reaction temperature, and the turning directions are the same, so that the purpose of dissolving sulfur can be achieved.
And the working state is as follows: mixed reaction state
At this time, the first agitator rotates at a forward high speed, and the second agitator rotates at a forward high speed. The first stirrer and the second stirrer turn to the same direction and rotate at the same speed, so that the liquids in the two pots are rotated in the same direction and at the same speed, a passage can be formed by the liquids in the first passage and the second passage, the liquids can circulate in the two pots, and the liquids in the two pots are fully fused. Because the concentration of tin in the tin liquid is far greater than that of copper, most of added sulfur is firstly dissolved in the tin liquid and reacts with tin to generate SnS, and then reacts with copper (Cu+SnS- & gtCu 2 S).
As the reaction proceeds, the temperature in the pot increases, thereby accelerating the reaction, and when the reaction is too high, the reaction temperature is appropriately controlled.
And the working state is three: slag tapping state
At this time, the first stirrer rotates at a positive high speed, the second stirrer rotates at a positive low speed (the rotating speed is less than 200 r/min), and the slag dragging device starts to work after a period of operation. The first stirrer and the second stirrer rotate in the same direction but at different rotation speeds, so that the liquid in the two pots can rotate in the same direction and at different speeds, a passage can be formed between the liquid in the first channel and the liquid in the second channel, the liquid can circulate in the two pots, the liquid in the first pot body rotates at a high speed to form a larger vortex, scum in the liquid can be quickly lowered to the bottom, the scum is thrown out into the channel in the tangential direction due to centrifugal force, the scum is transferred into the second pot body through the first channel or the second channel at the bottom, tin liquid in the second pot body flows back into the first pot body, and small vortex is formed due to the low rotation speed in the second pot body, the scum can float on the wall of the second pot body, and the scum is fished out through the scum scooping device.
Before the reaction, the first stirrer and the second stirrer rotate in the same direction and at the same speed, the first pot body is communicated with the second pot body, and the air pressure of the two pot bodies is balanced;
After the air pressure is balanced, the first stirrer and the second stirrer reversely rotate at the same speed, the first pot body and the second pot body are isolated, and enter a vulcanizing and reacting state to dissolve sulfur into crude tin liquid;
After sulfur is completely dissolved into crude tin liquid, the first stirrer and the second stirrer rotate in the same direction and at the same speed, the first pot body and the second pot body are communicated, and enter a mixing state, so that the liquids in the two pot bodies are fully fused;
After the liquid in the two pot bodies is fully fused to generate scum, the first stirrer and the second stirrer rotate in the same direction and at different speeds, the rotation speed of the second stirrer is lower than that of the first stirrer, the scum enters a slag discharging state, and the scum is fished out through a slag scooping device.
The specific working process is as follows:
Firstly, nitrogen is introduced into the first pot body (1), and air in the pot is displaced and discharged. Then the first stirrer (11) and the second stirrer (21) are started, the two stirrers rotate at a medium speed in the forward direction, copper-containing crude tin melt is added at the feeding port (23), and at the moment, the air release valve (13) of the first pot body (1) is opened to balance air pressure.
After the material addition is completed and the copper-containing crude tin melt in the two pot bodies is uniformly mixed, the air release valve (13) is closed, the first stirrer (11) is changed into forward high-speed rotation, and the second stirrer (21) reversely rotates at the same speed. Because the rotation speeds of the first stirrer (11) and the second stirrer (21) are the same, the rotation directions are opposite, the liquids in the two pots are also rotated reversely at the same speed, vortex is formed in the pots, the phenomenon of liquid opposite flushing in the two pots occurs in the first channel (35) and the second channel (36), the liquids are blocked from entering the other pot, the liquid in the channels cannot form a passage, and the isolated liquids circulate in the two pots respectively. At the moment, sulfur powder is added into the first pot body (1) through the closed feeding device (12), after the sulfur powder with a proper proportion is added, the closed feeding device (12) is closed, and because the liquid in the two pot bodies circulates independently at the moment, the complete dissolution of sulfur in the first pot body (1) is ensured, and the oxygen in the first pot body (1) is discharged and is filled with nitrogen, so that the sulfur and the oxygen react to generate sulfur dioxide polluted air is avoided. Or the rotating speed of the first stirrer (11) can be selected to be smaller than that of the second stirrer (21) according to the size of the pot and the reaction temperature, and the purposes of dissolving sulfur can be achieved by turning the same direction.
After the added sulfur is completely dissolved into the crude tin liquid, the first stirrer (11) keeps rotating at a positive high speed, the second stirrer (21) also changes into rotating at a positive high speed, the liquid in the first channel (35) and the second channel (36) can form a passage, the liquid can circulate in the two pots, the copper-containing crude tin melt dissolved with the sulfur is uniformly mixed in the two pots, meanwhile, the dissolved sulfur can also continuously react with copper in the melt, and finally black powdery slag is formed on the surface of the tin liquid.
At this time, the stirring speed of the second stirrer (21) is reduced, the rotation speed of the first pot body (1) is the same as that of the second pot body (2), but the rotation speeds of the first pot body and the second pot body are different, so that the liquid in the first channel (35) and the second channel (36) can form a passage, the liquid can slowly circulate in the two pots, the tin liquid in the first pot body (1) rotates at a high speed, copper sulfide slag in the tin liquid can quickly decline, the tin liquid reaches the bottom, and the tin liquid can circulate to the second pot body (2) through the first channel (35) or the second channel (36), and the copper sulfide slag can float upwards in the second pot body (2) along the wall due to the low rotation speed of the second pot body (2), and the slag is fished out through the slag scooping device (22), so that the purpose of adding sulfur and removing copper and refining tin is achieved.
Compared with the prior art, the invention has the beneficial effects that:
(1) The crude tin double-pot sulfur adding and impurity removing reactor adopts a closed structure, and is sealed for sulfur adding, so that the problem that sulfur is directly combusted due to overhigh temperature during sulfur adding can be solved, the loss of sulfur is reduced, the problem of smoke generation during sulfur combustion during single-pot sulfur adding is avoided, and the smoke and dust are prevented from interfering with operation and polluting the environment.
(2) Under the state of adding sulfur and reacting, the gas generated by the reaction in the first pot body is isolated in the first pot body by adopting a liquid blocking mode, so that the gas generated by the reaction is prevented from being discharged from the second pot body.
(3) This two pot sulfur edulcoration reactors of thick tin adopt two pot structures, and the first pot body second pot body is connected through the intercommunication device, is provided with the agitator of independent control in every pot:
(4) The gas isolation in the double-pot is realized through the control of the liquid level in the two-pot, so that the atmosphere in the single-pot is ensured;
(5) The control of the steering of the stirrer in the two pots realizes the valve effect of the liquid in the channel and controls whether the liquid in the two pots performs mass transfer exchange or not;
(6) The controllable transfer of the scum is realized by controlling the rotation speed difference of the stirrers in the two pots.
Drawings
FIG. 1 is a schematic diagram of a crude tin double pot sulfur impurity removal reactor in example 1;
FIG. 2 is a longitudinal sectional view of the crude tin double pot sulfur impurity removal reactor of example 1;
FIG. 3 is a transverse cross-sectional view of the crude tin double pot sulfur impurity removal reactor of example 1;
FIG. 4 is a schematic diagram showing the trajectory of dross in example 1;
FIG. 5 is a schematic diagram of the flow direction and flow velocity of the liquid in the crude tin double pot sulfur and impurity removal reactor of example 1 rotating at the same speed and in the same direction;
FIG. 6 is a schematic diagram of the flow direction and flow rate of the crude tin double pot sulfur impurity removal reactor of example 1 when rotated in the same speed and reverse direction;
FIG. 7 is a schematic diagram showing the replacement of internal oxygen by nitrogen gas introduced into the first pot during the process of adding sulfur and removing copper, wherein (a) is a longitudinal sectional view and (b) is a transverse sectional view;
FIG. 8 is a schematic diagram of adding a crude tin melt into a second pot during the process of adding sulfur and removing copper, wherein (a) is a longitudinal sectional view, and (b) is a transverse sectional view;
FIG. 9 is a schematic diagram of adding solid sulfur to a first pot after stirring two pots at the same speed and in the same direction in the process of adding sulfur and removing copper, wherein (a) is a longitudinal sectional view and (b) is a transverse sectional view;
FIG. 10 is a schematic diagram showing the two pans stirring at the same speed and in the same direction in the process of adding sulfur and removing copper, and uniformly mixing the liquids in the two pans, wherein (a) is a longitudinal sectional view, and (b) is a transverse sectional view;
FIG. 11 is a schematic view showing the floating of dross and the removal of slag from the second pot during the high speed, low speed, co-rotating movement of the first pot during the removal of copper by adding sulfur, wherein (a) is a longitudinal sectional view and (b) is a transverse sectional view;
Fig. 12 is a schematic diagram of discharging the standard tin liquor from the second pot during the sulfur-adding and copper-removing process, wherein (a) is a longitudinal sectional view, and (b) is a transverse sectional view.
Reference numerals:
1-a first pot body; 11-a first stirrer; 12-a closed feeding device; 13-a bleed valve; 2-a second pot body; 21-a second stirrer; 22-a slag dragging device; 23-a charging port; 24-a discharge hole; 3-communication means; 31-a communication housing; 32-a dredger; 33-arc part; 34-a straight portion; 35-a first channel; 36-a second channel; 4-a dross collection container.
Detailed Description
The invention will be described in further detail below with reference to the drawings by means of specific embodiments.
Example 1
As shown in fig. 1-4, this embodiment provides a crude tin double pot sulfur impurity removal reactor, comprising: the first pot body 1, the second pot body 2 and the communication device 3, the first pot body 1 is seal structure, be equipped with airtight feeding device 12, first agitator 11 and bleed valve 13 on it, and first agitator 11 is used for stirring the material in the first pot body 1, airtight feeding device 12 is connected with the vulcanizing agent feed bin, wholly is closed spiral feeder for in adding the vulcanizing agent in the feed bin in the first pot body 1, with the metal liquid reaction in the first pot body 1.
The second pot body 2 is the same as the first pot body 1 in size, and is provided with a second stirrer 12, a slag scooping device 22 and a charging hole 23, wherein the second stirrer 12 is used for stirring liquid in the second pot body 2, and the outlet end of the slag scooping device 22 is connected with a scum collecting container 4 for fishing out the scum after reaction from the second pot body 2.
The slag scooping device 22 is a vertically arranged screw conveyor, one end of the slag scooping device extending into the second pot body 2 is a semi-open conduit mechanism, and the scum is discharged from the semi-open conduit into the screw conveyor, is discharged from the second pot body 2 by the screw conveyor, and is collected by the scum collecting container 4.
The communication device 3 comprises a communication shell 31 and a dredging member 32, wherein two ends of the connection shell 31 are respectively connected with the first pot body 1 and the second pot body 2, a hollow structure is arranged in the connection shell to communicate the first pot body 1 and the second pot body 2, the dredging member 32 is positioned in the middle of the connection shell 31, two ends of the dredging member are arc portions 33, the circle center of the arc portion 33 close to one end of the first pot body 1 is positioned on the axis of the first pot body 1 (namely concentric with the first pot body 1 and with the same radius), the circle center of the arc portion 33 close to one end of the second pot body 2 is positioned on the axis of the second pot body 2 (namely concentric with the second pot body 2 and with the same radius), and the arc portions 33 at two ends can enable vortex in the two pots to be concentric circles so that vortex formation is easier.
The two circular arc portions 33 are connected by the straight portion 34 such that a first passage 35 and a second passage 36 are formed between the straight portion 34 and the connection housing 31.
When the crude tin double-pot sulfur adding and impurity removing reactor is used, the following states exist:
The working state is as follows: charging and sulfur dissolution state
At this time, the first stirrer 11 rotates at a forward direction and the second stirrer 21 rotates at a reverse direction, and the closed charging device 12 slowly charges the vulcanizing agent in the bin into the first pan body 1 to completely dissolve sulfur in the liquid in the first pan body 1. As shown in fig. 6 and 9, since the first stirrer 11 and the second stirrer 21 are opposite in rotation direction and same in rotation speed, the liquids in the two pot bodies are also rotated reversely at the same speed, vortex is formed in the pot bodies, and meanwhile, the phenomenon of liquid opposite flushing in the two pot bodies occurs in the first channel 35 and the second channel 36, the liquids in the channels are blocked from entering the other pot body, so that the liquids in the channels cannot form a passage, the isolated liquids circulate in the two pot bodies respectively, the reaction is ensured to be carried out only in the first pot body 1, oxygen in the first pot body 1 is exhausted, nitrogen is filled, and the pollution of sulfur dioxide generated by the reaction of sulfur and oxygen is avoided.
And the working state is as follows: mixed reaction state
After the added sulfur is completely dissolved into the crude tin liquid, the first stirrer 11 is kept rotating at a forward high speed, and the second stirrer 21 is changed to rotate at a forward high speed. As shown in fig. 5 and 10, the first stirrer 11 and the second stirrer 21 turn in the same direction and rotate at the same speed, so that the liquids in the two pot bodies rotate in the same direction and at the same speed, and thus the liquids in the first channel 35 and the second channel 36 can form a passage, the liquids circulate in the two pot bodies, the liquids in the two pot bodies are fully fused, and sulfur dissolved in the crude tin liquid continuously reacts with copper until the reaction is finished.
And the working state is three: slag tapping state
When the reaction is completed, the first agitator 11 is kept rotating at a positive high speed, the second agitator 21 is changed to rotate at a positive low speed, and the slag-removing device 22 is started. As shown in fig. 4 and 6, the rotation speed of the first stirrer 11 is the same as that of the second stirrer 21, but the rotation speeds of the first stirrer and the second stirrer are different, so that the liquid in the first channel 35 and the second channel 36 can form a passage, the liquid can slowly circulate in the two pots, the liquid in the first pot 1 rotates at a high speed, the scum suspended in the first pot 1 can quickly descend to the bottom, then enters the second pot 2 through the first channel 35 or the second channel 36 at the bottom, and the scum can slowly float in the second pot 2 due to the low rotation speed of the second pot 2, and the scum is fished out by the half-open scum scooping device 22 after floating.
The sulfuration and copper removal process of the sulfuration reactor is as follows (crude tin is taken as an example):
The first step: as shown in fig. 7, nitrogen is introduced into the pot from the air release opening above the first pot body 1 to replace oxygen in the pot, so that the subsequent reaction is in an anaerobic state.
And a second step of: as shown in fig. 8, raw material crude tin a is added from a feed port 23 of the second pot 2, and simultaneously a vent port of the first pot 1 is opened to balance the air pressure in the pot. After the liquid level is reached, the first stirrer 11 and the second stirrer 12 rotate at the same direction and low speed, the rotating speed is less than 200r/min, 150r/min is adopted in the embodiment, and the liquids in the two pots can be uniformly mixed in the state, so that the problem that the impurity concentrations in the two pots are different due to uneven raw material components in the process of feeding for multiple times is solved.
And a third step of: as shown in fig. 9, the closed charging device 12 of the first pot 1 is provided with a structure as follows: solid sulfur (sulfur powder and sulfur blocks can be added) is added in the molar ratio of Cu=1:1, the temperature of tin liquid in the pot is controlled to be 240-260 ℃, the stirring directions of the first stirrer 11 and the second stirrer 12 are opposite (for example, the first pot body 1 is stirred clockwise, the second pot body 2 is stirred anticlockwise) and the rotating speed is the same, the rotating speed is 240-420r/min and lasts for 10-20min, the embodiment is 15min, the liquid level in the first pot body 1 is made to be vortex, the added sulfur is involved in the tin liquid to be dissolved under the anaerobic condition, the liquid level in the second pot body 2 forms a vortex rotating reversely, the liquid in the two pots forms a liquid partition at the position of the communicating device 3, and undissolved sulfur is prevented from circulating into the second pot body 2.
Fourth step: as shown in fig. 10, after the third step is completed, the stirring direction of the second pot 2 is adjusted to be consistent with that of the first pot 1, the rotation speed is the same, the temperature of the tin liquor is controlled to be 280-320 ℃ (the melting point of the simple substance S is 112.8 ℃, the boiling point is 444.6 ℃, and the best reaction condition at 280 ℃ is referred to tin metallurgy, the sulphidation copper removal reaction is carried out in this embodiment, the temperature is 290 ℃, the reaction is carried out for 15-30min, the temperature is 25min in this embodiment, the tin liquor in the two pots is uniformly mixed, copper is removed in the reaction, and black powdery slag is formed on the surface of the tin liquor.
Fifth step: as shown in fig. 11, the stirring rotation speed of the second pot 2 is slowly reduced, the liquid level vortex is reduced, meanwhile, the liquid in the first channel 35 and the second channel 36 can form a passage, the liquid can circulate in the two pots, the liquid in the first pot 1 rotates at a high speed, the scum suspended in the first pot 1 rapidly descends to the bottom, and then is transferred to the second pot 2 through the first channel 35 or the second channel 36 at the bottom, because the density of the sulfur slag is smaller, the rotation speed of the second pot 2 is lower, the sulfur slag gradually rises along the pot wall in the process and floats on the surface of the crude tin liquid, the tin liquid in the second pot 2 flows back to the first pot 1 through the first channel 35 or the second channel 36 at the bottom, and after the time is kept for 15min, the scum skimming device 22 is started to scoop up the scum.
Sixth step: if the Cu content in the tin liquor does not reach the 3N refined tin standard, new sulfur is added from the closed feeding device 12, and the steps three to five are repeated, and slag is fished.
Seventh step: as shown in fig. 12, when the Cu content of tin in the first pot 1 and the second pot 2 reaches the 3N refined tin standard, discharging is performed through the discharging port 24, and during discharging, air circulation in the first pot 1 and the second pot 2 is blocked, and discharging is stopped until the Cu content is tangent to the upper part of the communication channel.
The composition of each stage is shown in Table 1:
TABLE 1
The foregoing description of the invention has been presented for purposes of illustration and description, and is not intended to be limiting. Several simple deductions, modifications or substitutions may also be made by a person skilled in the art to which the invention pertains, based on the idea of the invention.
Claims (4)
1. A crude tin double pot sulfur impurity removal reactor, comprising:
The first pot body (1) is of a closed structure, a closed feeding device (12) and a first stirrer (11) are arranged on the first pot body, the closed feeding device (12) is used for adding materials, and the first stirrer (11) is used for stirring the materials in the first pot body;
The second pot body (2) is communicated with the first pot body (1) through a communication device (3), and a second stirrer (21) is arranged on the second pot body and is used for stirring materials in the second pot body (2);
Two ends of the communication device (3) are respectively overlapped with the external cutting direction of the first pot body (1) and the second pot body (2);
The communication device (3) is used for:
1) When the first stirrer (11) and the second stirrer (21) rotate reversely and at the same speed, materials in the first pot body (1) and the second pot body (2) are isolated;
2) When the first stirrer (11) and the second stirrer (21) rotate in the same direction and at the same speed, materials in the first pot body (1) and the second pot body (2) are communicated, so that the materials in the first pot body (1) and the second pot body (2) are mixed;
3) When the first stirrer (11) and the second stirrer (21) rotate in the same direction and at different speeds, and the rotating speed of the first stirrer (11) is higher than that of the second stirrer (21), materials in the first pot body (1) and the second pot body (2) are communicated, so that scum in the first pot body (1) enters the second pot body (2);
The communication device (3) comprises:
the two ends of the communication shell (31) are respectively connected with the first pot body (1) and the second pot body (2), and the inside of the communication shell is communicated with the first pot body (1) and the second pot body (2);
The dredging piece (32) is arranged in the middle of the communication shell (31), and a first channel (35) and a second channel (36) are formed between the dredging piece and two sides of the communication shell (31);
One end of the dredging piece (32) close to the first pot body (1) and one end close to the second pot body (2) are as follows: an arc part (33) with the same radius and the same center with the two sides of the pot body; the side of the dredging piece (32) close to the first channel (35) and the side of the dredging piece close to the second channel (36) are straight parts (34), the communicating shell (31) is tangent to the shells of the two pot bodies, and the two pot bodies are combined into the reactor with the long waist structure.
2. The crude tin double-pot sulfur-adding impurity-removing reactor according to claim 1, wherein the second pot body (2) is provided with a slag-fishing device (22), and the slag-fishing device (22) is used for fishing scum in the second pot body (2).
3. The crude tin double-pot sulfur-adding and impurity-removing reactor according to claim 2, wherein the slag-fishing device (22) is a vertically arranged screw conveyor, one end of the slag-fishing device extending into the second pot body (2) is a semi-open conduit mechanism, and the scum enters the screw conveyor from the semi-open conduit and is sent out of the second pot body (2) by the screw conveyor.
4. The crude tin double pot sulfur and impurity removal reactor of claim 1, wherein said closed feed means (12) is a screw feeder.
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