CN111170360B - Device and process for preparing lead oxide from desulfurization lead - Google Patents
Device and process for preparing lead oxide from desulfurization lead Download PDFInfo
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- CN111170360B CN111170360B CN201811348013.2A CN201811348013A CN111170360B CN 111170360 B CN111170360 B CN 111170360B CN 201811348013 A CN201811348013 A CN 201811348013A CN 111170360 B CN111170360 B CN 111170360B
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- 238000006477 desulfuration reaction Methods 0.000 title claims abstract description 81
- 230000023556 desulfurization Effects 0.000 title claims abstract description 81
- 229910000464 lead oxide Inorganic materials 0.000 title claims abstract description 33
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 21
- YEXPOXQUZXUXJW-UHFFFAOYSA-N oxolead Chemical compound [Pb]=O YEXPOXQUZXUXJW-UHFFFAOYSA-N 0.000 title abstract 2
- 239000007788 liquid Substances 0.000 claims abstract description 151
- 238000003763 carbonization Methods 0.000 claims abstract description 59
- 238000002386 leaching Methods 0.000 claims abstract description 21
- 238000001354 calcination Methods 0.000 claims abstract description 20
- 238000000746 purification Methods 0.000 claims abstract description 18
- 238000004064 recycling Methods 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 15
- 230000003647 oxidation Effects 0.000 claims abstract description 12
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 12
- 230000003009 desulfurizing effect Effects 0.000 claims abstract description 11
- 239000007789 gas Substances 0.000 claims description 70
- 239000000243 solution Substances 0.000 claims description 60
- 239000000706 filtrate Substances 0.000 claims description 54
- 238000003860 storage Methods 0.000 claims description 42
- 239000012065 filter cake Substances 0.000 claims description 41
- 238000006243 chemical reaction Methods 0.000 claims description 38
- 238000000926 separation method Methods 0.000 claims description 33
- 238000003756 stirring Methods 0.000 claims description 32
- HTUMBQDCCIXGCV-UHFFFAOYSA-N lead oxide Chemical compound [O-2].[Pb+2] HTUMBQDCCIXGCV-UHFFFAOYSA-N 0.000 claims description 31
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 27
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 26
- 238000005086 pumping Methods 0.000 claims description 21
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical group [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 claims description 20
- 238000001035 drying Methods 0.000 claims description 20
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 19
- 229910052802 copper Inorganic materials 0.000 claims description 19
- 239000010949 copper Substances 0.000 claims description 19
- 239000012528 membrane Substances 0.000 claims description 17
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 claims description 16
- 238000010438 heat treatment Methods 0.000 claims description 16
- 238000005406 washing Methods 0.000 claims description 15
- 239000002002 slurry Substances 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- MFEVGQHCNVXMER-UHFFFAOYSA-L 1,3,2$l^{2}-dioxaplumbetan-4-one Chemical compound [Pb+2].[O-]C([O-])=O MFEVGQHCNVXMER-UHFFFAOYSA-L 0.000 claims description 10
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 10
- 229910000003 Lead carbonate Inorganic materials 0.000 claims description 10
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 claims description 10
- 239000000126 substance Substances 0.000 claims description 9
- 239000004471 Glycine Substances 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 8
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 claims description 7
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims description 5
- LSNNMFCWUKXFEE-UHFFFAOYSA-N Sulfurous acid Chemical compound OS(O)=O LSNNMFCWUKXFEE-UHFFFAOYSA-N 0.000 claims description 5
- 235000011941 Tilia x europaea Nutrition 0.000 claims description 5
- 230000000536 complexating effect Effects 0.000 claims description 5
- 239000000428 dust Substances 0.000 claims description 5
- 230000005484 gravity Effects 0.000 claims description 5
- 239000004571 lime Substances 0.000 claims description 5
- 235000013336 milk Nutrition 0.000 claims description 5
- 239000008267 milk Substances 0.000 claims description 5
- 210000004080 milk Anatomy 0.000 claims description 5
- 150000003839 salts Chemical class 0.000 claims description 5
- 239000002893 slag Substances 0.000 claims description 5
- 238000009423 ventilation Methods 0.000 claims description 5
- 235000001014 amino acid Nutrition 0.000 claims description 4
- 229940024606 amino acid Drugs 0.000 claims description 4
- 239000011259 mixed solution Substances 0.000 claims description 4
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Substances [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 3
- MTCFGRXMJLQNBG-REOHCLBHSA-N (2S)-2-Amino-3-hydroxypropansäure Chemical compound OC[C@H](N)C(O)=O MTCFGRXMJLQNBG-REOHCLBHSA-N 0.000 claims description 2
- KJCVRFUGPWSIIH-UHFFFAOYSA-N 1-naphthol Chemical compound C1=CC=C2C(O)=CC=CC2=C1 KJCVRFUGPWSIIH-UHFFFAOYSA-N 0.000 claims description 2
- CDAWCLOXVUBKRW-UHFFFAOYSA-N 2-aminophenol Chemical compound NC1=CC=CC=C1O CDAWCLOXVUBKRW-UHFFFAOYSA-N 0.000 claims description 2
- ISPYQTSUDJAMAB-UHFFFAOYSA-N 2-chlorophenol Chemical compound OC1=CC=CC=C1Cl ISPYQTSUDJAMAB-UHFFFAOYSA-N 0.000 claims description 2
- QTWJRLJHJPIABL-UHFFFAOYSA-N 2-methylphenol;3-methylphenol;4-methylphenol Chemical compound CC1=CC=C(O)C=C1.CC1=CC=CC(O)=C1.CC1=CC=CC=C1O QTWJRLJHJPIABL-UHFFFAOYSA-N 0.000 claims description 2
- IQUPABOKLQSFBK-UHFFFAOYSA-N 2-nitrophenol Chemical compound OC1=CC=CC=C1[N+]([O-])=O IQUPABOKLQSFBK-UHFFFAOYSA-N 0.000 claims description 2
- DCXYFEDJOCDNAF-UHFFFAOYSA-N Asparagine Natural products OC(=O)C(N)CC(N)=O DCXYFEDJOCDNAF-UHFFFAOYSA-N 0.000 claims description 2
- XUJNEKJLAYXESH-REOHCLBHSA-N L-Cysteine Chemical compound SC[C@H](N)C(O)=O XUJNEKJLAYXESH-REOHCLBHSA-N 0.000 claims description 2
- DCXYFEDJOCDNAF-REOHCLBHSA-N L-asparagine Chemical compound OC(=O)[C@@H](N)CC(N)=O DCXYFEDJOCDNAF-REOHCLBHSA-N 0.000 claims description 2
- ZDXPYRJPNDTMRX-VKHMYHEASA-N L-glutamine Chemical compound OC(=O)[C@@H](N)CCC(N)=O ZDXPYRJPNDTMRX-VKHMYHEASA-N 0.000 claims description 2
- AYFVYJQAPQTCCC-GBXIJSLDSA-N L-threonine Chemical compound C[C@@H](O)[C@H](N)C(O)=O AYFVYJQAPQTCCC-GBXIJSLDSA-N 0.000 claims description 2
- OUYCCCASQSFEME-QMMMGPOBSA-N L-tyrosine Chemical compound OC(=O)[C@@H](N)CC1=CC=C(O)C=C1 OUYCCCASQSFEME-QMMMGPOBSA-N 0.000 claims description 2
- MTCFGRXMJLQNBG-UHFFFAOYSA-N Serine Natural products OCC(N)C(O)=O MTCFGRXMJLQNBG-UHFFFAOYSA-N 0.000 claims description 2
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 claims description 2
- AYFVYJQAPQTCCC-UHFFFAOYSA-N Threonine Natural products CC(O)C(N)C(O)=O AYFVYJQAPQTCCC-UHFFFAOYSA-N 0.000 claims description 2
- 239000004473 Threonine Substances 0.000 claims description 2
- 150000001413 amino acids Chemical class 0.000 claims description 2
- 235000009582 asparagine Nutrition 0.000 claims description 2
- 229960001230 asparagine Drugs 0.000 claims description 2
- 229930003836 cresol Natural products 0.000 claims description 2
- 235000018417 cysteine Nutrition 0.000 claims description 2
- XUJNEKJLAYXESH-UHFFFAOYSA-N cysteine Natural products SCC(N)C(O)=O XUJNEKJLAYXESH-UHFFFAOYSA-N 0.000 claims description 2
- ZDXPYRJPNDTMRX-UHFFFAOYSA-N glutamine Natural products OC(=O)C(N)CCC(N)=O ZDXPYRJPNDTMRX-UHFFFAOYSA-N 0.000 claims description 2
- 229940056932 lead sulfide Drugs 0.000 claims description 2
- 229910052981 lead sulfide Inorganic materials 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- 239000011736 potassium bicarbonate Substances 0.000 claims description 2
- 229910000028 potassium bicarbonate Inorganic materials 0.000 claims description 2
- 235000015497 potassium bicarbonate Nutrition 0.000 claims description 2
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 2
- 235000011181 potassium carbonates Nutrition 0.000 claims description 2
- TYJJADVDDVDEDZ-UHFFFAOYSA-M potassium hydrogencarbonate Chemical compound [K+].OC([O-])=O TYJJADVDDVDEDZ-UHFFFAOYSA-M 0.000 claims description 2
- 235000011118 potassium hydroxide Nutrition 0.000 claims description 2
- 235000017550 sodium carbonate Nutrition 0.000 claims description 2
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 2
- OUYCCCASQSFEME-UHFFFAOYSA-N tyrosine Natural products OC(=O)C(N)CC1=CC=C(O)C=C1 OUYCCCASQSFEME-UHFFFAOYSA-N 0.000 claims description 2
- -1 bisphenol a Chemical compound 0.000 claims 1
- YCIMNLLNPGFGHC-UHFFFAOYSA-N catechol Chemical compound OC1=CC=CC=C1O YCIMNLLNPGFGHC-UHFFFAOYSA-N 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 17
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 abstract description 4
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 20
- 239000001569 carbon dioxide Substances 0.000 description 10
- 229910002092 carbon dioxide Inorganic materials 0.000 description 10
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 9
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 description 8
- 239000011505 plaster Substances 0.000 description 7
- 239000011593 sulfur Substances 0.000 description 6
- 229910052717 sulfur Inorganic materials 0.000 description 6
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 5
- 230000008929 regeneration Effects 0.000 description 5
- 238000011069 regeneration method Methods 0.000 description 5
- 230000001276 controlling effect Effects 0.000 description 4
- 238000003912 environmental pollution Methods 0.000 description 4
- 238000001914 filtration Methods 0.000 description 4
- 238000011084 recovery Methods 0.000 description 4
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulphite Substances [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 3
- 235000010265 sodium sulphite Nutrition 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 238000003723 Smelting Methods 0.000 description 2
- SSQNAPWMQSPZRM-UHFFFAOYSA-N benzene-1,4-diol;sodium Chemical compound [Na].OC1=CC=C(O)C=C1 SSQNAPWMQSPZRM-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229940046892 lead acetate Drugs 0.000 description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 description 2
- 235000011152 sodium sulphate Nutrition 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 235000004554 glutamine Nutrition 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000009853 pyrometallurgy Methods 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 235000004400 serine Nutrition 0.000 description 1
- NESLWCLHZZISNB-UHFFFAOYSA-M sodium phenolate Chemical compound [Na+].[O-]C1=CC=CC=C1 NESLWCLHZZISNB-UHFFFAOYSA-M 0.000 description 1
- 235000008521 threonine Nutrition 0.000 description 1
- 235000002374 tyrosine Nutrition 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G21/00—Compounds of lead
- C01G21/02—Oxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention provides a device and a process for preparing lead oxide by desulfurizing lead, wherein the device comprises a gas purification unit, an oxidation unit, a solid-liquid separator and a conveying pipe, wherein the gas purification unit comprises a first desulfurization tank, a fan and a second carbonization tank; the oxidation unit comprises a leaching tank, a first carbonization tank, a calciner and a conveying device; the tail gas after calcination in the calciner is conveyed to a first desulfurization tank through a fan; and introducing the tail gas treated by the first desulfurization tank into a second carbonization tank for purifying again, returning the purified tail gas to the first carbonization tank for reutilization, and transferring the solution in the second carbonization tank into the first desulfurization tank for recycling through a conveying pipe. The tail gas after calcination is treated for multiple times, so that sulfur dioxide contained in the tail gas is thoroughly purified, the influence on the previous working procedures is effectively reduced by the purified gas, the pollution of raw materials by the gas is reduced, the raw materials can be better recycled, the consumption of the raw materials is effectively reduced, the production cost is saved, and the production efficiency is improved.
Description
Technical Field
The invention relates to a lead oxide preparation technology, in particular to a device and a process for preparing lead oxide from desulfurization lead.
Background
The lead plaster of the waste lead-acid storage battery is usually prepared by smelting a certain amount of coal, sodium carbonate and scrap iron into a reverberatory furnace or a short kiln at high temperature to produce reduced lead; lead oxide includes red lead and yellow lead, and is prepared through smelting refined lead, slow oxidation with air, conversion at certain temperature and crushing.
It is reported that some Zhejiang company uses an atomic economy method to wet treat lead plaster of waste lead-acid storage batteries to produce lead oxide, and the technological line is that the lead plaster is converted by sodium hydroxide to remove sulfate radical in the lead plaster to produce low-sulfur lead plaster and sodium sulfate solution. Purifying, evaporating, concentrating, cooling and crystallizing the sodium sulfate solution to prepare anhydrous sodium sulfate; leaching the desulfurized lead plaster into a solution by adopting acetic acid, wherein lead in the lead plaster generates lead acetate solution, unleached lead, other metal impurities and organic matters are remained in residues, and the residues are used for producing crude lead by pyrometallurgy of lead; and introducing carbon dioxide gas into the lead acetate solution to generate lead carbonate precipitate, regenerating acetic acid, returning the regenerated acetic acid to the previous working procedure for recycling, and drying and calcining the lead carbonate to generate lead oxide and carbon dioxide gas. The lead oxide is used for the production of lead-acid storage batteries, and the carbon dioxide gas is returned to the previous working procedure for use.
The above-mentioned atomic economic process has the following defects that when the carbon dioxide gas after calcination ranges from the previous process, the incomplete reaction of the previous process is caused by the incomplete sulfur contained in the gas, and the raw materials are replaced after a period of reaction, so that the production cost is increased.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a device and a process for preparing lead oxide by desulfurizing lead, which can reduce raw material pollution, improve regeneration cycle and is beneficial to environmental protection.
The technical scheme of the invention is as follows: the device for preparing the lead oxide from the desulfurized lead comprises a gas purification unit, an oxidation unit, a solid-liquid separator and a conveying pipe, wherein the gas purification unit comprises a first desulfurization tank, a fan and a second carbonization tank, and the first desulfurization tank is connected with the second carbonization tank through the conveying pipe; the oxidation unit comprises a leaching tank, a first carbonization tank, a calciner and a conveying device, wherein the leaching tank is connected with the first carbonization tank through a conveying pipe, the first carbonization tank is connected with a solid-liquid separator, the solution after solid-liquid separation is returned to the leaching tank for recycling, and filter residues after solid-liquid separation are transferred into the calciner through the conveying device; the tail gas after calcination in the calciner is conveyed to a first desulfurization tank through a fan; and introducing the tail gas treated by the first desulfurization tank into a second carbonization tank for purifying again, returning the purified tail gas to the first carbonization tank for reutilization, and transferring the solution in the second carbonization tank into the first desulfurization tank for recycling through a conveying pipe.
Further, the gas purification unit further comprises a second desulfurization tank, a solid-liquid separator and a liquid storage tank, wherein the solid-liquid separator comprises a fourth solid-liquid separator, one end of the fourth solid-liquid separator is connected with the first desulfurization tank, and the other end of the fourth solid-liquid separator is connected with the second desulfurization tank; the second desulfurization tank is connected with the second carbonization tank through a conveying pipe, and a liquid storage tank is arranged on the conveying pipe connected with the first desulfurization tank.
Further, the oxidation unit further comprises a solid-liquid separator, a washing and drying device and a purifying tank, wherein the solid-liquid separator comprises a first solid-liquid separator, a second solid-liquid separator and a third solid-liquid separator; the two ends of the purifying tank are respectively connected with a first solid-liquid separator and a second solid-liquid separator, the first solid-liquid separator is connected with the leaching tank, and the second solid-liquid separator is connected with the first carbonization tank; the third solid-liquid separator is connected with the first carbonization tank, and filter residues separated by the third solid-liquid separator are transferred into a washing and drying device through a conveying device, and the washing and drying device is connected with the calciner through the conveying device.
Further, the upper part of the second desulfurization tank is provided with a stirring reaction chamber, and the lower part of the second desulfurization tank is provided with a filter; pumps are arranged on the conveying pipes; the filtrate separated by the solid-liquid separator is transferred into the liquid storage tank, and one end of the fan is provided with a wind flowmeter.
A process for preparing lead oxide from desulfurized lead comprises the following steps:
(1) Adding crushed desulfurization lead paste and 1-10M amino acid solution into a leaching tank according to a solid-liquid ratio of 1:10-3:1, adding 10-40% hydrogen peroxide with 10-150% of the specific gravity of the desulfurization lead paste, heating to 40-80 ℃, stirring for 2-4 hours, complexing lead, and performing solid-liquid separation to obtain filtrate and a filter cake after the reaction is completed;
(2) Transferring the filtrate in the step (1) into a purifying tank, adding lead powder according to 2-8 times of the weight fraction of copper in the solution to remove copper in the complex lead solution, controlling the temperature at 45-80 ℃, stirring for 15-60 minutes, and performing solid-liquid separation to obtain filtrate and filter cake copper slag after the reaction is completed;
(3) Pumping the filtrate in the step (2) into a first carbonization tank, introducing gas at normal temperature, stopping ventilation when the pH value of the slurry is reduced to 6-7, performing solid-liquid separation to obtain filtrate and a filter cake after the reaction is finished, washing the filter cake, then sending the filter cake to a drying process, and returning the washed water to the filtrate in the step (1) together;
(4) Transferring the dried filter cake in the step (3) to a kiln calciner, calcining and collecting dust at the temperature of 350-500 ℃, and further treating calcined tail gas;
(5) Introducing the tail gas calcined in the step (4) into a first desulfurization tank containing a desulfurizing agent with the concentration of 1-12M and lime milk, reducing the pH value of the solution to 8, reducing the introducing amount or stopping introducing, heating to 40-80 ℃, stirring for 1-3 hours, performing solid-liquid separation after the reaction is finished, wherein the filter pulp is mixed liquid containing the desulfurizing agent and sulfite, and the filter cake is calcium sulfate;
(6) Pumping the filter pulp in the step (5) into a second desulfurization tank, adding organic phenol substances, carrying out desulfurization again on the solution, and carrying out solid-liquid separation after the stirring reaction is completed, wherein filtrate is a solution containing organic salt and filter cake calcium sulfate;
(7) Transferring the filtrate obtained in the step (6) into a second carbonization tank as a solution containing organic salt, introducing the tail gas treated in the step (5), and directly returning the solution to the first desulfurization tank for recycling after the stirring reaction is completed; the purified tail gas is conveyed to a first carbonization tank for reuse.
Further, the amino acid in the step (1) is one or more of glycine, serine, threonine, cysteine, tyrosine, asparagine and glutamine.
Further, 99% of lead powder is added according to the mass fraction of 1-7 times of copper in the solution in the step (2) to remove copper in the complex lead solution, the temperature is controlled at 60 ℃, and the stirring time is 30-100 minutes.
Further, the filter cake in the step (4) is dried at the temperature of 150-200 ℃ until the water content is less than or equal to 1% of lead carbonate powder.
Further, the desulfurizing agent in the step (5) is one or more of sodium carbonate, sodium hydroxide, sodium bicarbonate, potassium hydroxide, potassium carbonate and potassium bicarbonate with strong alkalinity.
Further, the organic phenol substance in the step (6) is one or more of bisphenol A, phenol, cresol, aminophenol, nitrophenol, naphthol and chlorophenol.
Further, the organic phenol substance in the step (6) is bisphenol A, 99.5% of bisphenol A is added according to the mol ratio of 1:5-5:1 of sulfate radical, and the mixture is heated to 50 ℃ and stirred for 1.5 hours.
Further, the introducing amount of the tail gas after the treatment in the step (7) is 1-8L/min, the pH value of the solution is reduced to 7.5, and the introducing amount is reduced or the introducing is stopped.
Further, the solid-liquid separation is carried out by adopting a membrane filter press.
The invention has the following characteristics:
1. the tail gas after calcination is treated for multiple times, so that sulfur dioxide contained in the tail gas is thoroughly purified, the influence on the previous working procedures is effectively reduced by the purified gas, the pollution of raw materials by the tail gas is reduced, the raw materials can be better recycled, the consumption of the raw materials is effectively reduced, the production cost is saved, and the production efficiency is improved.
2. The intermediate raw materials are not consumed in the whole process, the raw materials are recycled, the production cost is effectively reduced, the tail gas is purified, sulfur in the tail gas is further purified by the design of the second carbonization tank, the purifying effect is effectively improved, and the pollution to the environment is reduced.
3. The invention has ingenious design, the regeneration and circulation of raw materials, the waste utilization of tail gas after calcination, the reduction of environmental pollution, the effective improvement of the recovery rate of lead oxide and the improvement of the working efficiency.
The detailed structure of the present invention is further described below with reference to the accompanying drawings and detailed description.
Drawings
FIG. 1-is a process flow diagram of example 1;
FIG. 2-is a process flow diagram of the apparatus for preparing lead oxide from lead sulfide in example 1;
101-leaching tank, 102-pump, 103-first solid-liquid separator, 104-liquid storage tank, 105-purifying tank, 106-second solid-liquid separator, 107-first carbonization tank, 108-third solid-liquid separator, 109-conveying device, 110-washing and drying device, 111-calciner, 201-first desulfurization tank, 202-air flowmeter, 203-fan, 204-fourth solid-liquid separator, 205-second desulfurization tank, 206-second carbonization tank.
Description of the embodiments
Examples
As shown in fig. 1-2: the device for preparing the lead oxide from the desulfurized lead comprises a gas purification unit, an oxidation unit, a solid-liquid separator and a conveying pipe, wherein the gas purification unit comprises a first desulfurization tank 201, a fan 203 and a second carbonization tank 206, and the first desulfurization tank 201 is connected with the second carbonization tank 206 through the conveying pipe; the oxidation unit comprises a leaching tank 101, a first carbonization tank 107, a calciner 111 and a conveying device 109, wherein the leaching tank 101 is connected with the first carbonization tank 107 through a conveying pipe, the first carbonization tank 107 is connected with a solid-liquid separator, the solution after solid-liquid separation is returned to the leaching tank 101 for recycling, and filter residues after solid-liquid separation are transferred into the calciner 111 through the conveying device 109; the tail gas after calcination in the calciner 111 is conveyed to the first desulfurizing tank 201 through a fan 203; the tail gas treated by the first desulfurization tank 201 is led into the second carbonization tank 206 for purification again, and the purified tail gas returns to the first carbonization tank 107 for reuse, and the solution in the second carbonization tank 206 is transferred into the first desulfurization tank 201 for recycling through a conveying pipe.
The gas purification unit further comprises a second desulfurization tank 205, a solid-liquid separator and a liquid storage tank 104, wherein the solid-liquid separator comprises a fourth solid-liquid separator 204, one end of the fourth solid-liquid separator 204 is connected with the first desulfurization tank 201, and the other end of the fourth solid-liquid separator is connected with the second desulfurization tank 205; the second desulfurization tank 205 is connected with the second carbonization tank 206 through a conveying pipe, and a liquid storage tank 104 is arranged on the conveying pipe connecting the second carbonization tank 206 with the first desulfurization tank 201.
The oxidation unit further comprises a solid-liquid separator, a washing and drying device 110 and a purification tank 105, wherein the solid-liquid separator comprises a first solid-liquid separator 103, a second solid-liquid separator 106 and a third solid-liquid separator 108; the two ends of the purifying tank 105 are respectively connected with a first solid-liquid separator 103 and a second solid-liquid separator 106, the first solid-liquid separator 103 is connected with the leaching tank 101, and the second solid-liquid separator 106 is connected with the first carbonization tank 107; the third solid-liquid separator 108 is connected to the first carbonization tank 107, and the filter residue separated by the third solid-liquid separator 108 is transferred to the washing and drying device 110 through the conveyor 109, and the washing and drying device 110 is connected to the calciner 111 through the conveyor 109.
The upper part of the second desulfurization tank 205 is a stirring reaction chamber, and the lower part is provided with a filter; pumps 102 are arranged on the conveying pipes; the filtrate separated by the solid-liquid separator is transferred into the liquid storage tank 104, one end of the fan 203 is provided with a wind flowmeter 202 for detecting wind speed and flow, and the size of the air inlet is regulated according to the reaction requirement.
The first desulfurization tank 201, the second desulfurization tank 205, the second carbonization tank 206, the leaching tank 101, the purification tank 105 and the first carbonization tank 107 are internally provided with stirring devices and heating devices, the top of the tank body is provided with a feed inlet, the lower part of the tank body is provided with a discharge outlet, the side surface of the tank body is provided with a thermometer and a PH value meter, and meanwhile, the tank body is provided with a circulating pump 102 for enabling solution in the tank body to flow up and down, so that solution precipitation is prevented or blockage of the tank body and a conveying pipe caused by scaling in the tank body is prevented; the stirring device is driven by a motor, the heating device is a resistance heater, and heating is provided according to the requirements of reaction conditions.
The device for preparing lead oxide by adopting the desulfurization lead is used for preparing lead oxide, and comprises the following treatment processes:
(1) Adding crushed desulfurization lead paste and 10M glycine solution into a leaching tank 101 according to a solid-liquid ratio of 1:4, adding hydrogen peroxide containing 20% and accounting for 50% of the specific gravity of the desulfurization lead paste, heating to 60 ℃, stirring for 2-4 hours, complexing lead, carrying out solid-liquid separation to obtain filtrate and a filter cake by adopting a membrane filter press of a first solid-liquid separator 103 after the reaction is completed, and transferring the filtrate into a liquid storage tank 104 for later use.
(2) Transferring the filtrate in the liquid storage tank 104 in the step (1) into a purifying tank 105, adding 99% lead powder according to 5 times of the mass fraction of copper in the solution to remove copper in the complex lead solution, controlling the temperature at 60 ℃, stirring for 30 minutes, performing solid-liquid separation into filtrate and filter cake copper slag by adopting a second solid-liquid separator 106 membrane filter press after the reaction is completed, and transferring the filtrate into the liquid storage tank 104 for standby.
(3) Pumping the filtrate in the liquid storage tank 104 in the step (2) into a first carbonization tank 107, introducing gas at normal temperature, stopping ventilation when the pH value of the slurry is reduced to 6-7, performing solid-liquid separation to obtain filtrate and a filter cake by adopting a membrane filter press of a third solid-liquid separator 108 after the reaction is finished, washing the filter cake, then sending the filter cake to a drying process, transferring the washed water and the filtrate in the step into the liquid storage tank 104, and returning the water and the filtrate in the step to the step (1) for recycling.
(4) Drying the filter cake obtained in the step (3) at the temperature of 150-200 ℃ until the water content is less than or equal to 1% of lead carbonate powder, transferring the lead carbonate powder into a kiln calciner 111, calcining and dust collecting the lead carbonate powder at the temperature of 350-500 ℃, and further treating the calcined tail gas.
(5) Introducing the tail gas containing carbon dioxide after calcination in the step (4) into a first desulfurization tank 201 containing 6M sodium hydroxide and lime milk, reducing the pH value of the solution to 8, reducing the introducing amount or stopping introducing, heating to 60 ℃, stirring for 2 hours, performing solid-liquid separation by using a fourth solid-liquid separator 204 membrane filter press after the reaction is completed, pumping the slurry which is mixed solution containing sodium hydroxide and sulfite into a liquid storage tank 104 for standby by a pump 102, and filtering cake which is calcium sulfate.
(6) Pumping the filter slurry in the liquid storage tank 104 in the step (5) into a second desulfurization tank 205, adding hydroquinone of an organic phenol substance, adding hydroquinone of 99.5% according to the molar ratio of 1:2 of sulfate radical, heating to 50 ℃ and stirring for 1.5 hours, carrying out solid-liquid separation by adopting a membrane filter press after the reaction is finished, filtering the filtrate into a solution containing sodium hydroquinone and filter cake calcium sulfate, and pumping the filtrate into the liquid storage tank 104 for standby.
(7) Pumping the filtrate in the liquid storage tank 104 in the step (6) into a second carbonization tank 206 by using a solution containing organic salt, then introducing the tail gas treated in the step (5), wherein the introducing amount of the tail gas is 2L/min, the pH value of the solution is reduced to 7.5, the introducing amount is reduced or the introducing is stopped, after the stirring reaction is completed, conveying the purified tail gas into the first carbonization tank 107 by using a fan 203 for recycling, and directly transferring the solution into the liquid storage tank 104 to be returned to the first desulfurization tank 201 for recycling.
Analysis shows that the content of carbon dioxide after the tail gas desulfurization is 12 percent and the content of sulfur is 12ppm; the purity of the lead oxide is 99.94%, the recovery rate is 98%, and the glycine regeneration rate after tail gas purification is improved by 50%; the result shows that the tail gas after calcination is purified and changed into valuable, so that the environmental pollution is effectively reduced, the raw material replacement frequency is reduced, the raw material consumption is reduced, and the production cost is saved.
Examples
The lead oxide preparation device for preparing lead oxide by using the desulfurization lead in the embodiment 1 comprises the following treatment processes:
(1) Adding crushed desulfurization lead paste and 9M glycine solution into a leaching tank 101 according to a solid-liquid ratio of 1:3, adding hydrogen peroxide containing 20% and accounting for 50% of the specific gravity of the desulfurization lead paste, heating to 60 ℃, stirring for 2-4 hours, complexing lead, performing solid-liquid separation to obtain filtrate and filter cake by adopting a first solid-liquid separator 103 membrane filter press after the reaction is completed, and pumping the filtrate into a liquid storage tank 104 for standby by a pump 102.
(2) Transferring the filtrate in the liquid storage tank 104 in the step (1) into a purifying tank 105, adding 99% lead powder according to 5 times of the mass fraction of copper in the solution to remove copper in the complex lead solution, controlling the temperature at 60 ℃, stirring for 30 minutes, performing solid-liquid separation into filtrate and filter cake copper slag by adopting a second solid-liquid separator 106 membrane filter press after the reaction is completed, and pumping the filtrate into the liquid storage tank 104 for standby by a pump 102.
(3) Pumping the filtrate in the liquid storage tank 104 in the step (2) into a first carbonization tank 107, introducing gas at normal temperature, stopping ventilation when the pH value of the slurry is reduced to 6.5, performing solid-liquid separation into filtrate and filter cake by adopting a membrane filter press after the reaction is finished, washing the filter cake, then sending the filter cake to a drying process, and pumping the washed water and the filtrate in the step into the liquid storage tank 104 together for recycling in the step (1).
(4) Drying the filter cake obtained in the step (3) at the temperature of 150 ℃ until the water content is less than or equal to 1% of lead carbonate powder, transferring the lead carbonate powder into a kiln calciner 111, calcining and dust collecting the lead carbonate powder at the temperature of 400 ℃, and further treating the calcined tail gas.
(5) Introducing the tail gas containing carbon dioxide after calcination in the step (4) into a first desulfurization tank 201 containing 7M sodium hydroxide and lime milk, reducing the pH value of the solution to 8, reducing the introducing amount or stopping introducing, heating to 60 ℃, stirring for 2 hours, performing solid-liquid separation by using a third solid-liquid separator 108 membrane filter press after the reaction is completed, transferring the slurry into a liquid storage tank 104 for later use, wherein the slurry is mixed solution containing sodium hydroxide and sulfite, and the filter cake is calcium sulfate.
(6) Pumping the filter pulp in the step (5) into a second desulfurization tank 205, adding hydroquinone of an organic phenol substance, adding hydroquinone of 99.5% according to the molar ratio of 1:1 of sulfate radical, heating to 50 ℃, stirring for 1.5 hours, desulfurizing the solution again, performing solid-liquid separation by adopting a membrane filter press after the reaction is finished, pumping the separated filtrate into a liquid storage tank 104 for standby by a pump 102, wherein the filtrate is a solution containing sodium hydroquinone and filter cake calcium sulfate.
(7) Transferring the filtrate in the liquid storage tank 104 in the step (6) into a second carbonization tank, introducing the tail gas treated in the step (5), wherein the introducing amount of the tail gas is 3L/min, the pH value of the solution is reduced to 7, the introducing amount is reduced or the introducing is stopped, after the stirring reaction is completed, conveying the purified tail gas into the first carbonization tank 107 through a fan 203 for reuse, and directly transferring the solution into the liquid storage tank 104 to be returned to the first desulfurization tank 201 for recycling.
Analysis shows that the content of carbon dioxide after the tail gas desulfurization is 13 percent and the content of sulfur is 14ppm; the purity of the lead oxide is 99.95%, the recovery rate is 98.4%, and the glycine regeneration rate after tail gas purification is improved by 52%; the result shows that the tail gas after calcination is purified and changed into valuable, so that the environmental pollution is effectively reduced, the raw material replacement frequency is reduced, the raw material consumption is reduced, and the production cost is saved.
Examples
The lead oxide preparation device for preparing lead oxide by using the desulfurization lead in the embodiment 1 comprises the following treatment processes:
(1) Adding crushed desulfurization lead paste and 8M glycine solution into a leaching tank 101 according to a solid-liquid ratio of 1:2, adding 25% hydrogen peroxide with 40% of the specific gravity of the desulfurization lead paste, heating to 65 ℃, stirring for 3 hours, complexing lead, performing solid-liquid separation to obtain filtrate and filter cake by adopting a first solid-liquid separator 103 membrane filter press after the reaction is completed, and pumping the filtrate into a liquid storage tank 104 for standby by a pump 102.
(2) Transferring the filtrate in the liquid storage tank 104 in the step (1) into a purifying tank 105, adding 99% lead powder according to 5 times of the mass fraction of copper in the solution to remove copper in the complex lead solution, controlling the temperature at 60 ℃, stirring for 30 minutes, performing solid-liquid separation into filtrate and filter cake copper slag by adopting a second solid-liquid separator 106 membrane filter press after the reaction is completed, and pumping the filtrate into the liquid storage tank 104 for standby by a pump 102.
(3) Pumping the filtrate in the liquid storage tank 104 in the step (2) into a first carbonization tank 107, introducing gas at normal temperature, stopping ventilation when the pH value of the slurry is reduced to 6.5, performing solid-liquid separation to obtain filtrate and a filter cake by adopting a membrane filter press of a third solid-liquid separator 108 after the reaction is finished, washing the filter cake, then sending the filter cake to a drying process, and transferring the washed water and the filtrate in the step into the liquid storage tank 104 for recycling after returning to the step (1).
(4) Drying the filter cake obtained in the step (3) at 160 ℃, transferring the filter cake to kiln calciner 111 until the water content is less than or equal to 1%, calcining and dust collecting at 400 ℃, and further treating the calcined tail gas.
(5) Introducing the tail gas containing carbon dioxide after calcination in the step (4) into a first desulfurization tank 201 containing 8M sodium hydroxide and lime milk, reducing the pH value of the solution to 8, reducing the introducing amount or stopping introducing, heating to 60 ℃, stirring for 2 hours, performing solid-liquid separation by using a fourth solid-liquid separator 204 membrane filter press after the reaction is completed, filtering slurry into mixed solution containing sodium hydroxide and sulfite, pumping filtrate into a liquid storage tank 104 for standby by a pump 102, and filtering cake is calcium sulfate.
(6) Pumping the filter slurry in the liquid storage tank 104 in the step (5) into a second desulfurization tank 205, adding phenol which is an organic phenol substance, adding 99.5% of phenol according to the proportion of the molar quantity of sulfate radical of 2:1, heating to 70 ℃ and stirring for 1.5 hours, carrying out solid-liquid separation on the solution after the reaction is completed by adopting a membrane filter press, pumping the filtrate into the liquid storage tank 104 for standby by adopting a pump 102, wherein the filtrate is a solution containing sodium phenolate and filter cake calcium sulfate.
(7) Transferring the filtrate in the liquid storage tank 104 in the step (6) into a second carbonization tank 206, introducing the tail gas treated in the step (5), wherein the introducing amount of the tail gas is 4L/min, the pH value of the solution is reduced to 7, the introducing amount is reduced or the introducing is stopped, after the stirring reaction is completed, introducing the purified tail gas into the first carbonization tank for reuse, and directly transferring the reacted solution into the liquid storage tank 104 to be returned to the first desulfurization tank 201 for recycling.
Analysis shows that the content of carbon dioxide after the tail gas desulfurization is 12.6 percent and the content of sulfur is 14ppm; the purity of the lead oxide is 99.94%, the recovery rate is 97.9%, and the glycine regeneration rate after tail gas purification is improved by 53%; the result shows that the tail gas after calcination is purified and changed into valuable, so that the environmental pollution is effectively reduced, the raw material replacement frequency is reduced, the raw material consumption is reduced, and the production cost is saved.
The preferred embodiments of the present invention have been described in detail above, but it is apparent that the present invention is not limited to the above-described embodiments. Within the scope of the technical idea of the invention, various equivalent modifications can be made to the technical solution of the invention, which all belong to the protection scope of the invention. In addition, the technical features described in the above-described specific embodiments may be combined separately and independently as long as they are within the technical concept of the present invention.
Claims (10)
1. The device for preparing the lead oxide from the desulfurized lead is characterized by comprising a gas purification unit, an oxidation unit, a solid-liquid separator and a conveying pipe, wherein the gas purification unit comprises a first desulfurization tank, a fan and a second carbonization tank, and the first desulfurization tank is connected with the second carbonization tank through the conveying pipe; the oxidation unit comprises a leaching tank, a first carbonization tank, a calciner and a conveying device, wherein the leaching tank is connected with the first carbonization tank through a conveying pipe, the first carbonization tank is connected with a solid-liquid separator, the solution after solid-liquid separation is returned to the leaching tank for recycling, and filter residues after solid-liquid separation are transferred into the calciner through the conveying device; the tail gas after calcination in the calciner is conveyed to a first desulfurization tank through a fan; and introducing the tail gas treated by the first desulfurization tank into a second carbonization tank for purifying again, returning the purified tail gas to the first carbonization tank for reutilization, and transferring the solution in the second carbonization tank into the first desulfurization tank for recycling through a conveying pipe.
2. The apparatus for preparing lead oxide from desulfurization lead according to claim 1, wherein the gas purification unit further comprises a second desulfurization tank, a solid-liquid separator and a liquid storage tank, the solid-liquid separator comprises a fourth solid-liquid separator, one end of the fourth solid-liquid separator is connected with the first desulfurization tank, and the other end of the fourth solid-liquid separator is connected with the second desulfurization tank; the second desulfurization tank is connected with the second carbonization tank through a conveying pipe, and a liquid storage tank is arranged on the conveying pipe connected with the first desulfurization tank.
3. The apparatus for preparing lead oxide from desulfurization lead according to claim 2, wherein the oxidation unit further comprises a solid-liquid separator, a washing and drying apparatus and a purification tank, the solid-liquid separator comprising a first solid-liquid separator, a second solid-liquid separator and a third solid-liquid separator; the two ends of the purifying tank are respectively connected with a first solid-liquid separator and a second solid-liquid separator, the first solid-liquid separator is connected with the leaching tank, and the second solid-liquid separator is connected with the first carbonization tank; the third solid-liquid separator is connected with the first carbonization tank, and filter residues separated by the third solid-liquid separator are transferred into a washing and drying device through a conveying device, and the washing and drying device is connected with the calciner through the conveying device.
4. The apparatus for preparing lead oxide from desulfurization lead according to claim 2 or 3, wherein the second desulfurization tank has a stirring reaction chamber at the upper part and a filter at the lower part; pumps are arranged on the conveying pipes; the filtrate separated by the solid-liquid separator is transferred into the liquid storage tank, and one end of the fan is provided with a wind flowmeter.
5. The process for preparing the lead oxide by desulfurizing the lead is characterized by comprising the following steps of:
(1) Adding crushed desulfurization lead paste and 1-10M amino acid solution into a leaching tank according to a solid-liquid ratio of 1:10-3:1, adding 10-40% hydrogen peroxide with the specific gravity of 10-150% of the desulfurization lead paste, heating to 40-80 ℃, stirring for 2-4 hours, complexing lead, and performing solid-liquid separation to obtain filtrate and a filter cake after the reaction is completed;
(2) Transferring the filtrate in the step (1) into a purifying tank, adding lead powder according to 2-8 times of the mass fraction of copper in the solution to remove copper in the complex lead solution, controlling the temperature at 45-80 ℃, stirring for 15-60 minutes, and performing solid-liquid separation to obtain filtrate and filter cake copper slag after the reaction is completed;
(3) Pumping the filtrate in the step (2) into a first carbonization tank, introducing gas at normal temperature, stopping ventilation when the pH value of the slurry is reduced to 6-7, performing solid-liquid separation to obtain filtrate and a filter cake after the reaction is finished, washing the filter cake, then sending the filter cake to a drying process, and returning the washed water to the filtrate in the step (1) together;
(4) Transferring the dried filter cake in the step (3) to a kiln calciner, calcining and dust collecting at the temperature of 350-500 ℃, and further treating calcined tail gas;
(5) Introducing the tail gas calcined in the step (4) into a first desulfurization tank containing a desulfurizing agent with the concentration of 1-12M and lime milk, reducing the pH value of the solution to 8, reducing the introducing amount or stopping introducing, heating to 40-80 ℃, stirring for 1-3 hours, carrying out solid-liquid separation after the reaction is finished, wherein the filter pulp is mixed solution containing the desulfurizing agent and sulfite, and the filter cake is calcium sulfate;
(6) Pumping the filter pulp in the step (5) into a second desulfurization tank, adding organic phenol substances, carrying out desulfurization again on the solution, and carrying out solid-liquid separation after the stirring reaction is completed, wherein filtrate is a solution containing organic salt and filter cake calcium sulfate;
(7) Transferring the filtrate obtained in the step (6) into a second carbonization tank as a solution containing organic salt, introducing the tail gas treated in the step (5), and directly returning the solution to the first desulfurization tank for recycling after the stirring reaction is completed; the purified tail gas is conveyed to a first carbonization tank for reuse.
6. The process for preparing lead oxide from lead sulfide according to claim 5, wherein the amino acid in the step (1) is one or more of glycine, serine, threonine, cysteine, tyrosine, asparagine, and glutamine.
7. The process for preparing lead oxide from the desulfurized lead according to claim 5, wherein 99% of lead powder is added according to 1-7 times of the mass fraction of copper in the solution in the step (2) to remove copper in the complex lead solution, the temperature is controlled at 60 ℃, and the stirring time is 30-100 minutes; drying the filter cake in the step (4) at the temperature of 150-200 ℃ until the water content is less than or equal to 1% of lead carbonate powder; the desulfurizing agent in the step (5) is one or more of sodium carbonate, sodium hydroxide, sodium bicarbonate, potassium hydroxide, potassium carbonate and potassium bicarbonate with strong alkalinity.
8. The process for preparing lead oxide from desulfurized lead according to claim 5, wherein the organic phenol substance in the step (6) is one or more of benzenediol, bisphenol a, phenol, cresol, aminophenol, nitrophenol, naphthol and chlorophenol; the organic phenol substance in the step (6) is bisphenol A, 99.5% of bisphenol A is added according to the mol ratio of 1:5-5:1 of sulfate radical, and the mixture is heated to 50 ℃ and stirred for 1.5 hours.
9. The process for preparing lead oxide from the desulfurized lead according to claim 5, wherein the introducing amount of the tail gas treated in the step (7) is 1-8L/min, and the pH value of the solution is reduced to 7.5 to reduce the introducing amount or the introducing is stopped.
10. The tail gas desulfurization process according to any one of claims 5 to 9, wherein the solid-liquid separation is carried out by a membrane filter press.
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