CN116555588A - Process method for producing crude tin by utilizing sodium stannate leaching waste residues - Google Patents
Process method for producing crude tin by utilizing sodium stannate leaching waste residues Download PDFInfo
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- CN116555588A CN116555588A CN202310478287.8A CN202310478287A CN116555588A CN 116555588 A CN116555588 A CN 116555588A CN 202310478287 A CN202310478287 A CN 202310478287A CN 116555588 A CN116555588 A CN 116555588A
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- tin
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- waste residues
- sodium stannate
- waste
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- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 title claims abstract description 147
- 239000002699 waste material Substances 0.000 title claims abstract description 99
- TVQLLNFANZSCGY-UHFFFAOYSA-N disodium;dioxido(oxo)tin Chemical compound [Na+].[Na+].[O-][Sn]([O-])=O TVQLLNFANZSCGY-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 229940079864 sodium stannate Drugs 0.000 title claims abstract description 33
- 238000000034 method Methods 0.000 title claims abstract description 31
- 238000002386 leaching Methods 0.000 title claims abstract description 25
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 14
- 239000012535 impurity Substances 0.000 claims abstract description 77
- 239000000126 substance Substances 0.000 claims abstract description 46
- 238000002791 soaking Methods 0.000 claims abstract description 29
- 238000001514 detection method Methods 0.000 claims abstract description 21
- 229910052751 metal Inorganic materials 0.000 claims abstract description 21
- 239000002184 metal Substances 0.000 claims abstract description 21
- 150000003606 tin compounds Chemical class 0.000 claims abstract description 18
- 238000011946 reduction process Methods 0.000 claims abstract description 8
- 150000001875 compounds Chemical class 0.000 claims description 38
- 150000002736 metal compounds Chemical class 0.000 claims description 26
- 239000002585 base Substances 0.000 claims description 20
- 239000007788 liquid Substances 0.000 claims description 20
- 239000007787 solid Substances 0.000 claims description 20
- 239000003638 chemical reducing agent Substances 0.000 claims description 14
- 238000003723 Smelting Methods 0.000 claims description 13
- 239000002253 acid Substances 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 9
- 238000002844 melting Methods 0.000 claims description 9
- 230000008018 melting Effects 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 230000000694 effects Effects 0.000 claims description 6
- 230000000737 periodic effect Effects 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 238000007599 discharging Methods 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 5
- 238000007670 refining Methods 0.000 claims description 5
- 238000001228 spectrum Methods 0.000 claims description 5
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 3
- 239000003513 alkali Substances 0.000 claims description 3
- 230000000903 blocking effect Effects 0.000 claims description 3
- 239000000460 chlorine Substances 0.000 claims description 3
- 229910052801 chlorine Inorganic materials 0.000 claims description 3
- 238000000746 purification Methods 0.000 abstract description 10
- 150000002739 metals Chemical class 0.000 abstract description 4
- 239000000243 solution Substances 0.000 description 66
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 6
- 238000003825 pressing Methods 0.000 description 3
- 229910001128 Sn alloy Inorganic materials 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000009713 electroplating Methods 0.000 description 2
- 238000007747 plating Methods 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 235000011121 sodium hydroxide Nutrition 0.000 description 2
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 2
- 230000001502 supplementing effect Effects 0.000 description 2
- 229910000838 Al alloy Inorganic materials 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 239000003929 acidic solution Substances 0.000 description 1
- 238000005904 alkaline hydrolysis reaction Methods 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000000956 alloy Substances 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
- 239000007864 aqueous solution Substances 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000003181 co-melting Methods 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 238000007772 electroless plating Methods 0.000 description 1
- 239000003063 flame retardant Substances 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000009965 odorless effect Effects 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 235000010344 sodium nitrate Nutrition 0.000 description 1
- 239000004317 sodium nitrate Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- GZCWPZJOEIAXRU-UHFFFAOYSA-N tin zinc Chemical compound [Zn].[Sn] GZCWPZJOEIAXRU-UHFFFAOYSA-N 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
- C22B25/06—Obtaining tin from scrap, especially tin scrap
-
- 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
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/005—Preliminary treatment of scrap
-
- 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
- C22B25/00—Obtaining tin
- C22B25/04—Obtaining tin by wet 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
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid leaching
-
- 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
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Manufacturing & Machinery (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Geochemistry & Mineralogy (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention discloses a process method for producing crude tin by utilizing sodium stannate leaching waste residues, and relates to the technical field of crude tin production. The invention comprises the steps of waste residue treatment: purifying sodium stannate leaching waste residues to remove completely unusable impurities, crushing the purified waste residues, reducing the volume of single waste residues and soaking the waste residues: and (3) putting the obtained waste residues into a soaking solution for soaking and dissolving to obtain a solution containing the tin compound. According to the invention, through setting up purification and crushing treatment on waste residues, completely unavailable impurities can be removed, the volume of single waste residues is reduced, the subsequent processing efficiency is improved, and the solution containing tin compounds can be analyzed by putting the solution containing tin compounds into the detection device to detect the element content of the solution containing tin compounds, so that impurity metals closest to the physical and chemical properties of tin are separated out through an impurity reduction step, and the quality of tin simple substances is prevented from being influenced in the subsequent tin reduction process.
Description
Technical Field
The invention relates to the technical field of crude tin production, in particular to a process method for producing crude tin by utilizing sodium stannate leaching waste residues.
Background
Sodium stannate, colorless hexagonal crystal or white powder, is odorless, is insoluble in organic matters, is easy to dissolve in water, and the aqueous solution is alkaline. The method is mainly applied to alkaline tin plating and copper plating in the electroplating industry, and electroplating and electroless plating of alloys such as tin alloy, zinc-tin alloy, aluminum alloy and the like; used as a fire retardant and weighting agent in the textile industry; used as mordant in printing and dyeing industry, etc. The production method of the sodium stannate mainly comprises the following steps:
(1) Oxidizing agent alkaline hydrolysis method: the tin material is mixed with caustic soda and sodium nitrate to react into coarse sodium stannate, and then nitrate is decomposed by high-temperature calcination, and then sodium stannate products are obtained through leaching, purifying, impurity removing, concentrating, centrifugal separation, drying and crushing.
(2) Direct melting method: and (3) co-melting the tin concentrate and sodium hydroxide at 400-500 ℃ for 2-3 hours, leaching, purifying and removing impurities such as arsenic, antimony, lead, silicon and the like, concentrating, centrifugally separating and drying to obtain a sodium stannate product.
After sodium stannate is produced, a large amount of sodium stannate leaching waste residues can appear, and a large amount of tin elements exist in the waste residues, so that recycling is needed, the existing recycling method is to directly use a reducing agent for reduction operation, but part of elements with similar physical and chemical properties to tin exist in the sodium stannate leaching waste residues, and the part of elements are separated out together with tin in the reduction process of the sodium stannate leaching waste residues, so that the quality of the recycled tin is greatly influenced, and certain defects exist.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a process method for producing crude tin by utilizing sodium stannate leaching waste residues, which solves the problems in the prior art.
In order to achieve the above purpose, the invention is realized by the following technical scheme: a process for preparing coarse tin from the leached dregs of sodium stannate includes
(1) And (3) waste residue treatment: purifying sodium stannate leaching waste residues to remove completely unusable impurities, and crushing the purified waste residues to reduce the volume of single waste residues;
(2) Soaking waste residues: soaking and dissolving the waste residue obtained in the step (1) in a soaking solution to obtain a solution of a tin-containing compound, wherein the soaking solution is concentrated acid;
(3) And (3) component detection: putting the solution of the tin-containing compound obtained in the step (2) into a detection device, detecting the element content of the solution, and obtaining an impurity metal compound a which is contained in the solution of the tin-containing compound and has the closest physical and chemical properties to tin;
(4) Reduction of impurities: adding an impurity reducing agent into the solution of the tin-containing compound obtained in the step (2), reducing the impurity metal compound a in the solution of the tin-containing compound, so that the impurity metal compound a closest to the physicochemical properties of tin is reduced into solid and separated out of the solution, obtaining a solid impurity metal compound a and refining the solution of the tin-containing compound;
(5) Tin reduction: adding a tin reducing agent into the refined tin-containing compound solution obtained in the step (4), reducing the tin compound into a tin simple substance and separating out solid, and filtering the solution containing solid tin to obtain a crude tin simple substance and waste liquid;
(6) Smelting a crude tin simple substance: smelting the crude tin simple substance obtained in the step (5), and naturally cooling after heating and melting the crude tin simple substance to obtain a block-shaped crude tin product;
(7) And (3) treating waste liquid: and (3) adding a water treatment agent and weak base into the waste liquid obtained in the step (5), purifying the waste liquid, balancing the pH value, and naturally discharging after reaching the discharge standard.
The method has the advantages that through setting up purification and crushing treatment on waste residues, completely unavailable impurities can be removed, the volume of single waste residues is reduced, the subsequent processing efficiency is improved, and through putting the solution containing the tin compound into the detection device and detecting the element content of the solution containing the tin compound, the solution containing the tin compound can be analyzed, so that impurity metals closest to the physical and chemical properties of tin are separated out through the subsequent impurity reduction step, and the quality of tin simple substances is prevented from being influenced in the subsequent tin reduction process.
Preferably, when the waste residue is crushed in the step (1), the waste residue is placed at the top of the hard filter plate, a downward impact force is generated on the waste residue at the top of the hard filter plate by using a pressing hammer, the waste residue is crushed by the pressing hammer, and the hard filter plate can filter the filter residue and generate a blocking force on the waste residue, so that the crushing effect of the pressing hammer is improved.
Preferably, the concentrated acid adopted in (2) is hydrochloric acid, and in the process of soaking in the solution, chlorine is continuously introduced into the solution, and meanwhile, heating is carried out to accelerate soaking and dissolution.
Preferably, the detection device in (3) is a spectrum analyzer, and if the detected impurity metal content closest to the physicochemical property of tin is less than 1%, the impurity metal is skipped, and the impurity metal with the next content more than 1% is selected as the impurity metal compound a.
Preferably, in the step (3), one of the reference bases for judging that the physical and chemical properties of tin are the closest to each other is the periodic table, and the element compound closest to tin on the periodic table is selected as the impurity metal compound a.
Preferably, in the reduction processes in (4) and (5), stirring is performed by using a stirring device, so that the reduction speeds of the impurity metal and the tin are accelerated, and heating is performed simultaneously, so that the activities of the impurity metal, the tin and the reducing agent are improved.
Preferably, the smelting temperature in (6) is 240 ℃ and is greater than the melting point of the elemental tin.
Preferably, the weak base used in (7) is sodium bicarbonate, the weak base is used in an amount larger than the concentrated acid used in (2), the weak base is added in a plurality of times, the pH value is detected by a pH meter at the same time when the weak base is added, and when the pH value is between 6.5 and 8.5, the alkali addition is stopped.
The invention provides a process method for producing crude tin by utilizing sodium stannate leaching waste residues. The beneficial effects are as follows:
(1) According to the invention, through setting up purification and crushing treatment on waste residues, completely unavailable impurities can be removed, the volume of single waste residues is reduced, the subsequent processing efficiency is improved, and the solution containing tin compounds can be analyzed by putting the solution containing tin compounds into the detection device to detect the element content of the solution containing tin compounds, so that impurity metals closest to the physical and chemical properties of tin are separated out through the impurity reduction step, and the quality of tin simple substances is prevented from being influenced in the subsequent tin reduction process.
(2) According to the invention, the element detection accuracy can be greatly improved by arranging the spectrum analyzer, the impurity reduction step waste caused by less reduction impurities can be avoided by skipping the impurity metal with the proportion of less than 1%, and the processing efficiency and the processing cost can be improved.
(3) According to the invention, the acidic solution can be prevented from influencing the environment by supplementing sodium bicarbonate, and meanwhile, the pH value is controlled between 6.5 and 8.5, so that the purification requirement can be reduced, the purification efficiency can be improved, and the purification cost can be reduced on the premise of not influencing the environment.
Drawings
FIG. 1 is a block diagram of the overall flow of the present invention.
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.
Example 1:
referring to fig. 1, the present invention provides a technical solution: a process for preparing coarse tin from the leached dregs of sodium stannate includes
(1) And (3) waste residue treatment: purifying sodium stannate leaching waste residues to remove completely unusable impurities, and crushing the purified waste residues to reduce the volume of single waste residues;
(2) Soaking waste residues: soaking and dissolving the waste residue obtained in the step (1) in a soaking solution to obtain a solution of a tin-containing compound, wherein the soaking solution is concentrated acid;
(3) And (3) component detection: putting the solution of the tin-containing compound obtained in the step (2) into a detection device, detecting the element content of the solution, and obtaining an impurity metal compound a which is contained in the solution of the tin-containing compound and has the closest physical and chemical properties to tin;
(4) Reduction of impurities: adding an impurity reducing agent into the solution of the tin-containing compound obtained in the step (2), reducing the impurity metal compound a in the solution of the tin-containing compound, so that the impurity metal compound a closest to the physicochemical properties of tin is reduced into solid and separated out of the solution, obtaining a solid impurity metal compound a and refining the solution of the tin-containing compound;
(5) Tin reduction: adding a tin reducing agent into the refined tin-containing compound solution obtained in the step (4), reducing the tin compound into a tin simple substance and separating out solid, and filtering the solution containing solid tin to obtain a crude tin simple substance and waste liquid;
(6) Smelting a crude tin simple substance: smelting the crude tin simple substance obtained in the step (5), and naturally cooling after heating and melting the crude tin simple substance to obtain a block-shaped crude tin product;
(7) And (3) treating waste liquid: and (3) adding a water treatment agent and weak base into the waste liquid obtained in the step (5), purifying the waste liquid, balancing the pH value, and naturally discharging after reaching the discharge standard.
The method has the advantages that through setting up purification and crushing treatment on waste residues, completely unavailable impurities can be removed, the volume of single waste residues is reduced, the subsequent processing efficiency is improved, and through putting the solution containing the tin compound into the detection device and detecting the element content of the solution containing the tin compound, the solution containing the tin compound can be analyzed, so that impurity metals closest to the physical and chemical properties of tin are separated out through the subsequent impurity reduction step, and the quality of tin simple substances is prevented from being influenced in the subsequent tin reduction process.
Example 2:
referring to fig. 1, the present invention provides a technical solution: a process for preparing coarse tin from the leached dregs of sodium stannate includes
(1) And (3) waste residue treatment: purifying sodium stannate leaching waste residues to remove completely unusable impurities, and crushing the purified waste residues to reduce the volume of single waste residues;
(2) Soaking waste residues: soaking and dissolving the waste residue obtained in the step (1) in a soaking solution to obtain a solution of a tin-containing compound, wherein the soaking solution is concentrated acid;
(3) And (3) component detection: putting the solution of the tin-containing compound obtained in the step (2) into a detection device, detecting the element content of the solution, and obtaining an impurity metal compound a which is contained in the solution of the tin-containing compound and has the closest physical and chemical properties to tin;
(4) Reduction of impurities: adding an impurity reducing agent into the solution of the tin-containing compound obtained in the step (2), reducing the impurity metal compound a in the solution of the tin-containing compound, so that the impurity metal compound a closest to the physicochemical properties of tin is reduced into solid and separated out of the solution, obtaining a solid impurity metal compound a and refining the solution of the tin-containing compound;
(5) Tin reduction: adding a tin reducing agent into the refined tin-containing compound solution obtained in the step (4), reducing the tin compound into a tin simple substance and separating out solid, and filtering the solution containing solid tin to obtain a crude tin simple substance and waste liquid;
(6) Smelting a crude tin simple substance: smelting the crude tin simple substance obtained in the step (5), and naturally cooling after heating and melting the crude tin simple substance to obtain a block-shaped crude tin product;
(7) And (3) treating waste liquid: and (3) adding a water treatment agent and weak base into the waste liquid obtained in the step (5), purifying the waste liquid, balancing the pH value, and naturally discharging after reaching the discharge standard.
(1) When well waste residue is broken, place the waste residue at stereoplasm filter plate top, use to push down the hammer, produce decurrent impact force to the waste residue at stereoplasm filter plate top, push down the hammer and smash the waste residue, the stereoplasm filter plate is when carrying out the filtration to the filter residue, produces the blocking force to the waste residue, improves the crushing effect of pushing down the hammer.
(2) The concentrated acid adopted in the process is hydrochloric acid, and in the process of soaking the solution, chlorine is continuously introduced into the solution, and meanwhile, the solution is heated to accelerate the soaking and dissolving.
(3) The detection device is a spectrum analyzer, and if the detected impurity metal content which is the closest to the physical and chemical properties of tin is less than 1%, the impurity metal is skipped, and the impurity metal with the next content ratio of more than 1% is selected as the impurity metal compound a.
(3) One of the reference bases for judging the closest physical and chemical properties of tin is the periodic table of elements, and the element compound closest to tin on the periodic table of elements is selected as the impurity metal compound a.
The element detection accuracy can be greatly improved by arranging the spectrum analyzer, impurity reduction step waste caused by less reduction impurities can be avoided by skipping impurity metal with the proportion of less than 1%, and the processing efficiency can be improved and the processing cost can be reduced.
Example 3:
referring to fig. 1, the present invention provides a technical solution: a process for preparing coarse tin from the leached dregs of sodium stannate includes
(1) And (3) waste residue treatment: purifying sodium stannate leaching waste residues to remove completely unusable impurities, and crushing the purified waste residues to reduce the volume of single waste residues;
(2) Soaking waste residues: soaking and dissolving the waste residue obtained in the step (1) in a soaking solution to obtain a solution of a tin-containing compound, wherein the soaking solution is concentrated acid;
(3) And (3) component detection: putting the solution of the tin-containing compound obtained in the step (2) into a detection device, detecting the element content of the solution, and obtaining an impurity metal compound a which is contained in the solution of the tin-containing compound and has the closest physical and chemical properties to tin;
(4) Reduction of impurities: adding an impurity reducing agent into the solution of the tin-containing compound obtained in the step (2), reducing the impurity metal compound a in the solution of the tin-containing compound, so that the impurity metal compound a closest to the physicochemical properties of tin is reduced into solid and separated out of the solution, obtaining a solid impurity metal compound a and refining the solution of the tin-containing compound;
(5) Tin reduction: adding a tin reducing agent into the refined tin-containing compound solution obtained in the step (4), reducing the tin compound into a tin simple substance and separating out solid, and filtering the solution containing solid tin to obtain a crude tin simple substance and waste liquid;
(6) Smelting a crude tin simple substance: smelting the crude tin simple substance obtained in the step (5), and naturally cooling after heating and melting the crude tin simple substance to obtain a block-shaped crude tin product;
(7) And (3) treating waste liquid: and (3) adding a water treatment agent and weak base into the waste liquid obtained in the step (5), purifying the waste liquid, balancing the pH value, and naturally discharging after reaching the discharge standard.
(4) And (5) stirring the materials by using a stirring device in the reduction process, accelerating the reduction speed of the impurity metal and tin, and simultaneously heating the materials to improve the activities of the impurity metal, the tin and the reducing agent.
(6) The smelting temperature is 240 ℃ and is higher than the melting point of the simple substance of tin.
(7) The weak base used in (2) is sodium bicarbonate, the weak base is used in an amount larger than the concentrated acid used in (2), the weak base is added for multiple times, a pH meter is used for pH detection at the same time at the interval of adding the weak base each time, and when the pH value is between 6.5 and 8.5, the alkali addition is stopped.
The acid solution can be prevented from influencing the environment by supplementing sodium bicarbonate, and meanwhile, the pH value is controlled between 6.5 and 8.5, so that the purification requirement can be reduced, the purification efficiency can be improved, and the purification cost can be reduced on the premise of not influencing the environment.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
Claims (8)
1. A process method for producing crude tin by utilizing sodium stannate leaching waste residues is characterized by comprising the following steps: comprising
(1) And (3) waste residue treatment: purifying sodium stannate leaching waste residues to remove completely unusable impurities, and crushing the purified waste residues to reduce the volume of single waste residues;
(2) Soaking waste residues: soaking and dissolving the waste residue obtained in the step (1) in a soaking solution to obtain a solution of a tin-containing compound, wherein the soaking solution is concentrated acid;
(3) And (3) component detection: putting the solution of the tin-containing compound obtained in the step (2) into a detection device, detecting the element content of the solution, and obtaining an impurity metal compound a which is contained in the solution of the tin-containing compound and has the closest physical and chemical properties to tin;
(4) Reduction of impurities: adding an impurity reducing agent into the solution of the tin-containing compound obtained in the step (2), reducing the impurity metal compound a in the solution of the tin-containing compound, so that the impurity metal compound a closest to the physicochemical properties of tin is reduced into solid and separated out of the solution, obtaining a solid impurity metal compound a and refining the solution of the tin-containing compound;
(5) Tin reduction: adding a tin reducing agent into the refined tin-containing compound solution obtained in the step (4), reducing the tin compound into a tin simple substance and separating out solid, and filtering the solution containing solid tin to obtain a crude tin simple substance and waste liquid;
(6) Smelting a crude tin simple substance: smelting the crude tin simple substance obtained in the step (5), and naturally cooling after heating and melting the crude tin simple substance to obtain a block-shaped crude tin product;
(7) And (3) treating waste liquid: and (3) adding a water treatment agent and weak base into the waste liquid obtained in the step (5), purifying the waste liquid, balancing the pH value, and naturally discharging after reaching the discharge standard.
2. The process for producing crude tin by utilizing sodium stannate leaching waste residues according to claim 1, wherein the process comprises the following steps: (1) When well waste residue is broken, place the waste residue at stereoplasm filter plate top, use to push down the hammer, produce decurrent impact force to the waste residue at stereoplasm filter plate top, push down the hammer and smash the waste residue, the stereoplasm filter plate is when carrying out the filtration to the filter residue, produces the blocking force to the waste residue, improves the crushing effect of pushing down the hammer.
3. The process for producing crude tin by utilizing sodium stannate leaching waste residues according to claim 1, wherein the process comprises the following steps: (2) The concentrated acid adopted in the process is hydrochloric acid, and in the process of soaking the solution, chlorine is continuously introduced into the solution, and meanwhile, the solution is heated to accelerate the soaking and dissolving.
4. The process for producing crude tin by utilizing sodium stannate leaching waste residues according to claim 1, wherein the process comprises the following steps: (3) The detection device is a spectrum analyzer, and if the detected impurity metal content which is the closest to the physical and chemical properties of tin is less than 1%, the impurity metal is skipped, and the impurity metal with the next content ratio of more than 1% is selected as the impurity metal compound a.
5. The process for producing crude tin by utilizing sodium stannate leaching waste residues, which is characterized in that: (3) One of the reference bases for judging the closest physical and chemical properties of tin is the periodic table of elements, and the element compound closest to tin on the periodic table of elements is selected as the impurity metal compound a.
6. The process for producing crude tin by utilizing sodium stannate leaching waste residues according to claim 1, wherein the process comprises the following steps: (4) And (5) stirring the materials by using a stirring device in the reduction process, accelerating the reduction speed of the impurity metal and tin, and simultaneously heating the materials to improve the activities of the impurity metal, the tin and the reducing agent.
7. The process for producing crude tin by utilizing sodium stannate leaching waste residues according to claim 1, wherein the process comprises the following steps: (6) The smelting temperature is 240 ℃ and is higher than the melting point of the simple substance of tin.
8. The process for producing crude tin by utilizing sodium stannate leaching waste residue according to claim 7, wherein the process comprises the following steps: (7) The weak base used in (2) is sodium bicarbonate, the weak base is used in an amount larger than the concentrated acid used in (2), the weak base is added for multiple times, a pH meter is used for pH detection at the same time at the interval of adding the weak base each time, and when the pH value is between 6.5 and 8.5, the alkali addition is stopped.
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