CN111747442A - Method for producing active zinc oxide by wet process - Google Patents
Method for producing active zinc oxide by wet process Download PDFInfo
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- CN111747442A CN111747442A CN202010775929.7A CN202010775929A CN111747442A CN 111747442 A CN111747442 A CN 111747442A CN 202010775929 A CN202010775929 A CN 202010775929A CN 111747442 A CN111747442 A CN 111747442A
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 84
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 41
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 20
- 230000008569 process Effects 0.000 title description 16
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims abstract description 41
- 238000002386 leaching Methods 0.000 claims abstract description 38
- 239000011701 zinc Substances 0.000 claims abstract description 38
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 38
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 24
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- 239000007788 liquid Substances 0.000 claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 12
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims abstract description 9
- 239000000843 powder Substances 0.000 claims abstract description 8
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 7
- 238000003825 pressing Methods 0.000 claims abstract description 7
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000005977 Ethylene Substances 0.000 claims abstract description 6
- 239000002253 acid Substances 0.000 claims abstract description 6
- 238000001704 evaporation Methods 0.000 claims abstract description 6
- 235000010482 polyoxyethylene sorbitan monooleate Nutrition 0.000 claims abstract description 6
- 229920000053 polysorbate 80 Polymers 0.000 claims abstract description 6
- 238000000227 grinding Methods 0.000 claims abstract description 4
- 238000012216 screening Methods 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 53
- 239000012535 impurity Substances 0.000 claims description 19
- 238000001354 calcination Methods 0.000 claims description 18
- 238000001035 drying Methods 0.000 claims description 14
- 239000012065 filter cake Substances 0.000 claims description 9
- UOURRHZRLGCVDA-UHFFFAOYSA-D pentazinc;dicarbonate;hexahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Zn+2].[Zn+2].[Zn+2].[Zn+2].[Zn+2].[O-]C([O-])=O.[O-]C([O-])=O UOURRHZRLGCVDA-UHFFFAOYSA-D 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 9
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 8
- 229910052785 arsenic Inorganic materials 0.000 claims description 8
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 claims description 8
- 239000013078 crystal Substances 0.000 claims description 8
- ORUIBWPALBXDOA-UHFFFAOYSA-L magnesium fluoride Chemical compound [F-].[F-].[Mg+2] ORUIBWPALBXDOA-UHFFFAOYSA-L 0.000 claims description 8
- 229910001635 magnesium fluoride Inorganic materials 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 238000011084 recovery Methods 0.000 claims description 6
- 238000004064 recycling Methods 0.000 claims description 5
- 230000009286 beneficial effect Effects 0.000 claims description 4
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 3
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 claims description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 235000012538 ammonium bicarbonate Nutrition 0.000 claims description 3
- 239000001099 ammonium carbonate Substances 0.000 claims description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- IWLXWEWGQZEKGZ-UHFFFAOYSA-N azane;zinc Chemical compound N.[Zn] IWLXWEWGQZEKGZ-UHFFFAOYSA-N 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 229910052742 iron Inorganic materials 0.000 claims description 3
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 claims description 3
- 239000011259 mixed solution Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 229910000069 nitrogen hydride Inorganic materials 0.000 claims description 3
- 239000007800 oxidant agent Substances 0.000 claims description 3
- 230000001590 oxidative effect Effects 0.000 claims description 3
- 239000012286 potassium permanganate Substances 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- 229910052979 sodium sulfide Inorganic materials 0.000 claims description 3
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims description 3
- 239000011343 solid material Substances 0.000 claims description 3
- RNWHGQJWIACOKP-UHFFFAOYSA-N zinc;oxygen(2-) Chemical class [O-2].[Zn+2] RNWHGQJWIACOKP-UHFFFAOYSA-N 0.000 claims 1
- 239000002245 particle Substances 0.000 abstract description 5
- 230000008020 evaporation Effects 0.000 abstract description 3
- 239000012295 chemical reaction liquid Substances 0.000 abstract 1
- 239000006193 liquid solution Substances 0.000 abstract 1
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 9
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 8
- 230000000694 effects Effects 0.000 description 5
- 230000000536 complexating effect Effects 0.000 description 4
- 230000009471 action Effects 0.000 description 3
- FMRLDPWIRHBCCC-UHFFFAOYSA-L Zinc carbonate Chemical compound [Zn+2].[O-]C([O-])=O FMRLDPWIRHBCCC-UHFFFAOYSA-L 0.000 description 2
- 239000000084 colloidal system Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 2
- 239000011667 zinc carbonate Substances 0.000 description 2
- 229910000010 zinc carbonate Inorganic materials 0.000 description 2
- 235000004416 zinc carbonate Nutrition 0.000 description 2
- UGZADUVQMDAIAO-UHFFFAOYSA-L zinc hydroxide Chemical compound [OH-].[OH-].[Zn+2] UGZADUVQMDAIAO-UHFFFAOYSA-L 0.000 description 2
- 229940007718 zinc hydroxide Drugs 0.000 description 2
- 229910021511 zinc hydroxide Inorganic materials 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006477 desulfuration reaction Methods 0.000 description 1
- 230000023556 desulfurization Effects 0.000 description 1
- FWABRVJYGBOLEM-UHFFFAOYSA-N diazanium;azane;carbonate Chemical compound N.[NH4+].[NH4+].[O-]C([O-])=O FWABRVJYGBOLEM-UHFFFAOYSA-N 0.000 description 1
- 238000010981 drying operation Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000012452 mother liquor Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G9/00—Compounds of zinc
- C01G9/02—Oxides; Hydroxides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- 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
- C01P2006/12—Surface area
-
- 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)
- Manufacture And Refinement Of Metals (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a method for producing active zinc oxide by a wet method, which comprises the following steps: (1) crushing: adding zinc calcine into a grinder for grinding, and screening by a 100-mesh filter screen to obtain zinc calcine powder, (2) leaching: putting zinc calcine powder into a leaching tank, adding a prepared leaching agent, heating to 50-60 ℃, carrying out combined leaching to prepare zinc ammine complex liquid, (3) putting the zinc ammine complex liquid prepared in the step (2) into a reaction kettle, heating to 85-88 ℃, adding 0.4-0.6 kg of ammonium persulfate into each cubic meter of the solution, stirring, and carrying out filter pressing to obtain the pure reaction liquid. When refined zinc liquid is evaporated, 1kg of ethylene acid and 1kg of Tween 80 are added into the refined liquid solution before ammonia evaporation per cubic meter, and the average particle size of the dried and calcined nano zinc oxide reaches 20-50um, and the specific surface area reaches 80m2/g, so that the wet-process produced active zinc oxide has stable quality, higher purity and large specific surface area.
Description
Technical Field
The invention relates to the technical field of preparation of zinc oxide, in particular to a method for producing active zinc oxide by a wet method.
Background
At present, zinc oxide on the market is mainly classified into indirect method, direct method and wet method zinc oxide. The indirect method is zinc oxide obtained by a one-step oxidation method using zinc ingots as raw materials, the zinc oxide has large consumption and wide application, but the cost is higher because the zinc ingots are used as the raw materials, and the direct method is zinc oxide obtained by the one-step oxidation method after the zinc-containing waste materials are subjected to impurity removal through processes such as desulfurization and the like. The zinc oxide obtained by the method has low cost, but the application range has certain limitation because the impurity content does not reach the standard. Therefore, in the last decade, China has appeared a large amount of zinc oxide produced by wet process, also called active zinc oxide, or also called nano zinc oxide, the wet process active zinc oxide process is divided into sulfuric acid process active zinc oxide and ammonia process active zinc oxide, the sulfuric acid process active zinc oxide has fast reaction speed, raw material adaptation area and product quality can be selected as the best, because of the use of sulfuric acid in the production process and the higher cost of water treatment, and the price of soda is greatly increased in recent years, and the examination and approval of sulfuric acid process active zinc oxide has been stopped in part of provinces and markets.
The active zinc oxide produced by the traditional ammonia-ammonium carbonate method has the advantages of low cost, complete recovery of mother liquor and small influence on the surrounding environment, and has the fatal defects of insufficient activity, unstable color, low content and the like of the product quality, so that in recent years, small-sized factories of the process stop production or transfer production in a break.
Disclosure of Invention
The present invention aims to provide a method for producing active zinc oxide by a wet process to solve the problems of the background art.
In order to achieve the purpose, the invention provides the following technical scheme: a method for producing active zinc oxide by a wet process, comprising the following steps:
(1) crushing: adding the zinc calcine into a grinder for grinding, and screening by a 100-mesh filter screen to obtain zinc calcine powder;
(2) leaching: putting zinc calcine powder into a leaching tank, adding a prepared leaching agent, heating to 50-60 ℃, and performing combined leaching to prepare a zinc ammine complex solution;
(3) and (3) putting the zinc-ammonia complex solution prepared in the step (2) into a reaction kettle, heating to 85-88 ℃, adding 0.4-0.6 kg of ammonium persulfate into each cubic meter of solution, stirring, and performing filter pressing to obtain a pure reaction solution.
(4) Removing impurities: (41) removing impurities such as iron, manganese, arsenic and the like in the leaching solution from the net reaction solution obtained in the step (3) by using a potassium permanganate or ammonium persulfate oxidant;
(42) adding zinc powder, heating to 40-60 ℃, keeping the temperature and reacting for 30 minutes-1 hour, adding sodium sulfide, heating to 60-80 ℃, keeping the temperature and reacting for 30 minutes-1 hour; finally, refined zinc liquid is obtained through filter pressing;
(43) adding 1kg of ethylene acid and 1kg of Tween 80 into each cubic meter of refined zinc liquid, mixing, adding the mixed refined zinc liquid into a steamer, continuously introducing steam under the pressure of 0.35mpa, controlling the temperature to be 68-72 ℃, evaporating for two hours, and crystallizing.
(5) And (3) dehydrating: cooling the crystal obtained in the step (33), and rinsing the crystal with deionized water to obtain a basic zinc carbonate filter cake;
(5) and (3) calcining: and (3) adding the basic zinc carbonate filter cake obtained in the step (4) into a drying furnace, drying at 100-160 ℃ for 1-2 hours, and adding the dried basic zinc carbonate filter cake into a calcining furnace for calcining to obtain the high-purity active zinc oxide.
Preferably, the leaching agent solution in the step (2) is a mixed solution of ammonia water and ammonium bicarbonate, the molar concentration of NH3 in the solution is controlled to be 5.7-6.3 mol/L, and the molar concentration of CO32 in the solution is controlled to be 0.8-1.2 mol/L.
Preferably, the concentration of the benzene solution in the step (1) is 0.5%, and the benzene solution is a liquid of benzene solution and solvent.
Preferably, magnesium fluoride is added into the leaching agent in the step (2), namely, 0.2-0.4 kg of magnesium fluoride is added into each cubic meter of solution, so that the recovery rate of the secondary zinc oxide can be properly improved, and the method is beneficial to removing the arsenic impurity content in the solution.
Preferably, the drying oven in the step (5) is a mechanical device for reducing moisture of the material by using heat energy, and is used for performing a drying operation on the object, and the drying oven heats the moisture in the material, generally referred to as moisture or other volatile liquid components, to evaporate and escape so as to obtain a solid material with a specified moisture content.
Preferably, the calcining furnace in the step (5) refers to a thermal equipment for heat-treating the carbon raw material at high temperature to improve the performance of the raw material.
Preferably, the calcination temperature in the step (5) is 500-550 ℃, and the calcination time in the step (5) is 6-8 hours.
Preferably, the leaching reaction time in the step (2) is 60-120 minutes, and the temperature of the leaching reaction is 60-70 ℃.
Preferably, the ammonia gas decomposed in the step (43) is absorbed by water and then is led into the leaching tank in the step (2) for recycling through an ammonia recycling system.
Compared with the prior art, the invention has the beneficial effects that: before impurity removal, the prepared zinc ammine complexing solution is put into a reaction kettle, the solution is heated to 85-88 ℃, 0.4-0.6 kg of ammonium persulfate is added into the solution per cubic meter, the mixture is stirred and is filter-pressed to obtain a clean reaction solution, Fe (OH)2 and sulfate series colloid small particles which are difficult to remove in the zinc ammine complexing solution can be removed and purified, then impurity removal is carried out, the impurity removal effect is improved, the concentration of a leaching agent is strictly controlled, magnesium fluoride is added into the leaching solution, the recovery rate of zinc hypoxide can be properly improved, the content of arsenic impurities in the solution can be removed, when refined zinc solution is evaporated, 1kg of ethylene acid and 1kg of Tween 80 are added into the refined solution per cubic meter before ammonia evaporation, zinc hydroxide and zinc carbonate crystals are coated, the average particle size of the dried and calcined nano zinc oxide reaches 20-50um, and the specific surface area reaches 80m2/g, therefore, the wet method for producing the active zinc oxide has stable quality, higher purity, large specific surface area and good activity.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention provides a technical scheme that: a method for producing active zinc oxide by a wet process, comprising the following steps:
(1) crushing: adding the zinc calcine into a grinder for grinding, and screening by a 100-mesh filter screen to obtain zinc calcine powder;
(2) leaching: putting zinc calcine powder into a leaching tank, adding a prepared leaching agent, heating to 50-60 ℃, and performing combined leaching to prepare a zinc ammine complex solution;
(3) and (3) putting the zinc-ammonia complex solution prepared in the step (2) into a reaction kettle, heating to 85-88 ℃, adding 0.4-0.6 kg of ammonium persulfate into each cubic meter of solution, stirring, and performing filter pressing to obtain a pure reaction solution.
(4) Removing impurities: (41) removing impurities such as iron, manganese, arsenic and the like in the leaching solution from the net reaction solution obtained in the step (3) by using a potassium permanganate or ammonium persulfate oxidant;
(42) adding zinc powder, heating to 40-60 ℃, keeping the temperature and reacting for 30 minutes-1 hour, adding sodium sulfide, heating to 60-80 ℃, keeping the temperature and reacting for 30 minutes-1 hour; finally, refined zinc liquid is obtained through filter pressing;
(43) adding 1kg of ethylene acid and 1kg of Tween 80 into each cubic meter of refined zinc liquid, mixing, adding the mixed refined zinc liquid into a steamer, continuously introducing steam under the pressure of 0.35mpa, controlling the temperature to be 68-72 ℃, evaporating for two hours, and crystallizing.
(5) And (3) dehydrating: cooling the crystal obtained in the step (33), and rinsing the crystal with deionized water to obtain a basic zinc carbonate filter cake;
(5) and (3) calcining: and (3) adding the basic zinc carbonate filter cake obtained in the step (4) into a drying furnace, drying at 100-160 ℃ for 1-2 hours, and adding the dried basic zinc carbonate filter cake into a calcining furnace for calcining to obtain the high-purity active zinc oxide.
In the step (2), the leaching agent solution is a mixed solution of ammonia water and ammonium bicarbonate, the molar concentration of NH3 in the solution is controlled to be 5.7-6.3 mol/L, and the molar concentration of CO32 is controlled to be 0.8-1.2 mol/L.
Magnesium fluoride is also added into the leaching agent in the step (2), namely, 0.2-0.4 kg of magnesium fluoride is added into each cubic meter of solution, so that the recovery rate of the secondary zinc oxide can be properly improved, and the method is beneficial to removing the arsenic impurity content in the solution.
The drying furnace in the step (5) is a mechanical device for reducing moisture of the material by using heat energy, and is used for drying the object, and the drying machine heats the material to enable moisture in the material, generally moisture or other volatile liquid components, to be vaporized and escaped so as to obtain the solid material with the specified moisture content.
The calcining furnace in the step (5) is a thermal device for carrying out heat treatment on the carbon raw material at a high temperature so as to improve the performance of the raw material.
The calcination temperature in the step (5) is 500-550 ℃, and the calcination time in the step (5) is 6-8 hours.
In the step (2), the leaching reaction time is 60-120 minutes, and the temperature of the leaching reaction is 60-70 ℃.
And (3) absorbing the ammonia gas decomposed in the step (43) by using water, and guiding the ammonia gas to the leaching tank in the step (2) through an ammonia circulating system for recycling.
Before impurity removal, the prepared zinc ammine complexing solution is put into a reaction kettle, the solution is heated to 85-88 ℃, 0.4-0.6 kg of ammonium persulfate is added into the solution per cubic meter, the mixture is stirred and is filter-pressed to obtain a clean reaction solution, Fe (OH)2 and sulfate series colloid small particles which are difficult to remove in the zinc ammine complexing solution can be removed and purified, then impurity removal is carried out, the impurity removal effect is improved, the concentration of a leaching agent is strictly controlled, magnesium fluoride is added into the leaching solution, the recovery rate of zinc hypoxide can be properly improved, the content of arsenic impurities in the solution can be removed, when refined zinc solution is evaporated, 1kg of ethylene acid and 1kg of Tween 80 are added into the refined solution per cubic meter before ammonia evaporation, zinc hydroxide and zinc carbonate crystals are coated, the average particle size of the dried and calcined nano zinc oxide reaches 20-50um, and the specific surface area reaches 80m2/g, therefore, the wet method for producing the active zinc oxide has stable quality, higher purity, large specific surface area and good activity.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus. Without further limitation.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (8)
1. A method for producing active zinc oxide by a wet method is characterized by comprising the following steps:
(1) crushing: adding the zinc calcine into a grinder for grinding, and screening by a 100-mesh filter screen to obtain zinc calcine powder;
(2) leaching: putting zinc calcine powder into a leaching tank, adding a prepared leaching agent, heating to 50-60 ℃, and performing combined leaching to prepare a zinc ammine complex solution;
(3) and (3) putting the zinc-ammonia complex solution prepared in the step (2) into a reaction kettle, heating to 85-88 ℃, adding 0.4-0.6 kg of ammonium persulfate into each cubic meter of solution, stirring, and performing filter pressing to obtain a pure reaction solution.
(4) Removing impurities: (41) removing impurities such as iron, manganese, arsenic and the like in the leaching solution from the net reaction solution obtained in the step (3) by using a potassium permanganate or ammonium persulfate oxidant;
(42) adding zinc powder, heating to 40-60 ℃, keeping the temperature and reacting for 30 minutes-1 hour, adding sodium sulfide, heating to 60-80 ℃, keeping the temperature and reacting for 30 minutes-1 hour; finally, refined zinc liquid is obtained through filter pressing;
(43) adding 1kg of ethylene acid and 1kg of Tween 80 into each cubic meter of refined zinc liquid, mixing, adding the mixed refined zinc liquid into a steamer, continuously introducing steam under the pressure of 0.35mpa, controlling the temperature to be 68-72 ℃, evaporating for two hours, and crystallizing.
(5) And (3) dehydrating: cooling the crystal obtained in the step (33), and rinsing the crystal with deionized water to obtain a basic zinc carbonate filter cake;
(5) and (3) calcining: and (3) adding the basic zinc carbonate filter cake obtained in the step (4) into a drying furnace, drying at 100-160 ℃ for 1-2 hours, and adding the dried basic zinc carbonate filter cake into a calcining furnace for calcining to obtain the high-purity active zinc oxide.
2. The method for producing active zinc oxide by a wet method according to claim 1, wherein the leaching agent solution in the step (2) is a mixed solution of ammonia water and ammonium bicarbonate, the molar concentration of NH3 in the solution is controlled to be 5.7 mol/L-6.3 mol/L, and the molar concentration of C032 is controlled to be 0.8 mol/L-1.2 mol/L.
3. The method for producing the active zinc oxide by the wet method according to claim 1, wherein magnesium fluoride is added into the leaching agent in the step (2), namely, 0.2-0.4 kg of magnesium fluoride is added into each cubic meter of solution, so that the recovery rate of the secondary zinc oxide can be improved properly, and the method is beneficial to removing the arsenic impurity content in the solution.
4. The method for producing active zinc oxide by wet method according to claim 1, wherein the drying oven in step (5) is a mechanical device for reducing moisture of the material by using heat energy, and is used for drying the object, and the drying oven heats the material to evaporate moisture in the material, generally moisture or other volatile liquid components, so as to obtain solid material with specified moisture content.
5. The method for producing activated zinc oxide by a wet method according to claim 1, wherein the calcining furnace in the step (5) is a thermal equipment for heat-treating carbon raw materials at high temperature to improve the properties of the raw materials.
6. The method for producing the active zinc oxide by the wet method according to claim 1, wherein the calcining temperature in the step (5) is 500-550 ℃, and the calcining time in the step (5) is 6-8 hours.
7. The method for producing the active zinc oxide by the wet method according to the claim 1, wherein the leaching reaction time in the step (2) is 60-120 minutes, and the temperature of the leaching reaction is 60-70 ℃.
8. The method for producing the active zinc oxide by the wet method according to the claim 1, wherein the ammonia gas decomposed in the step (43) is absorbed by water and then is led into the leaching tank in the step (2) for recycling through an ammonia recycling system.
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| CN202010775929.7A CN111747442A (en) | 2020-08-05 | 2020-08-05 | Method for producing active zinc oxide by wet process |
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| CN202010775929.7A CN111747442A (en) | 2020-08-05 | 2020-08-05 | Method for producing active zinc oxide by wet process |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112323097A (en) * | 2020-10-16 | 2021-02-05 | 昆明理工大学 | A method and system for removing sulfur dioxide in flue gas by zinc-ammonia complex coupled persulfate advanced oxidation technology |
| CN112892176A (en) * | 2021-01-15 | 2021-06-04 | 北京单原子催化科技有限公司 | Recovery processing method of zinc in zinc oxide desulfurization waste agent |
| CN113264549A (en) * | 2021-06-04 | 2021-08-17 | 江永县潇湘化工有限公司 | New preparation process of active zinc oxide |
| CN114150163A (en) * | 2021-12-17 | 2022-03-08 | 扬州新达再生资源科技有限公司 | Zinc dross regeneration process |
| CN114540638A (en) * | 2022-01-11 | 2022-05-27 | 云南云铜锌业股份有限公司 | Zinc leachate purification method |
| CN118908267A (en) * | 2024-08-01 | 2024-11-08 | 株洲安特新材料科技有限公司 | Method for producing active zinc oxide by wet process |
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| CN114540638B (en) * | 2022-01-11 | 2024-02-27 | 云南云铜锌业股份有限公司 | Zinc leaching solution purifying method |
| CN118908267A (en) * | 2024-08-01 | 2024-11-08 | 株洲安特新材料科技有限公司 | Method for producing active zinc oxide by wet process |
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