CN105197982A - Method for producing electronic-grade zinc oxide from high-chloride zinc hypoxide - Google Patents
Method for producing electronic-grade zinc oxide from high-chloride zinc hypoxide Download PDFInfo
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- CN105197982A CN105197982A CN201510627821.2A CN201510627821A CN105197982A CN 105197982 A CN105197982 A CN 105197982A CN 201510627821 A CN201510627821 A CN 201510627821A CN 105197982 A CN105197982 A CN 105197982A
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- zinc oxide
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 132
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 66
- 239000011701 zinc Substances 0.000 title claims abstract description 29
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 229910052725 zinc Inorganic materials 0.000 title claims abstract description 13
- 238000004519 manufacturing process Methods 0.000 title claims description 28
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 19
- UGZADUVQMDAIAO-UHFFFAOYSA-L zinc hydroxide Chemical compound [OH-].[OH-].[Zn+2] UGZADUVQMDAIAO-UHFFFAOYSA-L 0.000 claims abstract description 14
- UYJXRRSPUVSSMN-UHFFFAOYSA-P ammonium sulfide Chemical compound [NH4+].[NH4+].[S-2] UYJXRRSPUVSSMN-UHFFFAOYSA-P 0.000 claims abstract description 13
- 238000002386 leaching Methods 0.000 claims abstract description 10
- 229940007718 zinc hydroxide Drugs 0.000 claims abstract description 10
- 229910021511 zinc hydroxide Inorganic materials 0.000 claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000003837 high-temperature calcination Methods 0.000 claims abstract description 7
- 238000001354 calcination Methods 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 6
- 229910052742 iron Inorganic materials 0.000 claims abstract description 6
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 5
- 239000002994 raw material Substances 0.000 claims description 22
- 238000001556 precipitation Methods 0.000 claims description 21
- 239000000460 chlorine Substances 0.000 claims description 19
- 238000000034 method Methods 0.000 claims description 19
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 18
- 229910052801 chlorine Inorganic materials 0.000 claims description 18
- 238000006243 chemical reaction Methods 0.000 claims description 17
- 239000007788 liquid Substances 0.000 claims description 17
- 239000011572 manganese Substances 0.000 claims description 15
- 239000010949 copper Substances 0.000 claims description 14
- 229910052793 cadmium Inorganic materials 0.000 claims description 11
- 229910052802 copper Inorganic materials 0.000 claims description 11
- 239000012535 impurity Substances 0.000 claims description 11
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 10
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 10
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims description 10
- 230000002000 scavenging effect Effects 0.000 claims description 10
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 claims description 9
- 238000001914 filtration Methods 0.000 claims description 7
- 150000002500 ions Chemical class 0.000 claims description 7
- 239000000047 product Substances 0.000 claims description 7
- 150000003839 salts Chemical class 0.000 claims description 7
- 239000000706 filtrate Substances 0.000 claims description 6
- 238000006386 neutralization reaction Methods 0.000 claims description 6
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 5
- 229910021529 ammonia Inorganic materials 0.000 claims description 5
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 5
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 5
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 5
- 235000011149 sulphuric acid Nutrition 0.000 claims description 5
- 239000001117 sulphuric acid Substances 0.000 claims description 5
- PSIOOHPZLJTGJH-UHFFFAOYSA-M S(=O)(=O)([O-])[O-].[NH4+].[Zn+] Chemical compound S(=O)(=O)([O-])[O-].[NH4+].[Zn+] PSIOOHPZLJTGJH-UHFFFAOYSA-M 0.000 claims description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 4
- 239000012286 potassium permanganate Substances 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 3
- 239000012065 filter cake Substances 0.000 claims description 3
- 229910052748 manganese Inorganic materials 0.000 claims description 3
- 238000005649 metathesis reaction Methods 0.000 claims description 3
- 230000003647 oxidation Effects 0.000 claims description 3
- 230000001590 oxidative effect Effects 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- IWLXWEWGQZEKGZ-UHFFFAOYSA-N azane;zinc Chemical compound N.[Zn] IWLXWEWGQZEKGZ-UHFFFAOYSA-N 0.000 claims description 2
- 229910021645 metal ion Inorganic materials 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims 1
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 claims 1
- 238000013019 agitation Methods 0.000 claims 1
- 238000000605 extraction Methods 0.000 claims 1
- 239000011593 sulfur Substances 0.000 claims 1
- 229910052717 sulfur Inorganic materials 0.000 claims 1
- 238000005516 engineering process Methods 0.000 abstract description 5
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 abstract description 2
- 239000012847 fine chemical Substances 0.000 abstract description 2
- 238000005272 metallurgy Methods 0.000 abstract 2
- 230000003472 neutralizing effect Effects 0.000 abstract 1
- 235000014692 zinc oxide Nutrition 0.000 description 48
- 239000000243 solution Substances 0.000 description 24
- 239000000203 mixture Substances 0.000 description 8
- 238000000746 purification Methods 0.000 description 8
- 238000005352 clarification Methods 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- 229910001385 heavy metal Inorganic materials 0.000 description 4
- 239000005083 Zinc sulfide Substances 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 239000002243 precursor Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- RNWHGQJWIACOKP-UHFFFAOYSA-N zinc;oxygen(2-) Chemical class [O-2].[Zn+2] RNWHGQJWIACOKP-UHFFFAOYSA-N 0.000 description 3
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 2
- 230000029087 digestion Effects 0.000 description 2
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- RWSOTUBLDIXVET-UHFFFAOYSA-O sulfonium Chemical compound [SH3+] RWSOTUBLDIXVET-UHFFFAOYSA-O 0.000 description 2
- 241000370738 Chlorion Species 0.000 description 1
- 206010024769 Local reaction Diseases 0.000 description 1
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 238000003483 aging Methods 0.000 description 1
- 235000012538 ammonium bicarbonate Nutrition 0.000 description 1
- BIGPRXCJEDHCLP-UHFFFAOYSA-N ammonium bisulfate Chemical compound [NH4+].OS([O-])(=O)=O BIGPRXCJEDHCLP-UHFFFAOYSA-N 0.000 description 1
- 239000003637 basic solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000000536 complexating effect Effects 0.000 description 1
- 238000005202 decontamination Methods 0.000 description 1
- 230000003588 decontaminative effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 238000009854 hydrometallurgy Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 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 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000011403 purification operation Methods 0.000 description 1
- 230000003252 repetitive effect Effects 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 235000010265 sodium sulphite Nutrition 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention relates to the technical field of wet metallurgy and fine chemicals, in particular to a technology for producing electronic-grade zinc oxide from high-chloride zinc hypoxide. The technology is characterized in that with the high-chloride zinc hypoxide being not dechlorinated in advance, the electronic-grade zinc oxide 99.95% in purity is prepared by preparing the zinc hydroxide directly according to the wet metallurgy including ammonium salt-ammonia water leaching, iron removal by oxidization, edulcoration by zinc powder and ammonium sulfide and neutralizing, and then subjecting the zinc hydroxide to high-temperature calcination at the temperature of 1,000-1,100 DEG C in a drying calcining furnace.
Description
Technical field
The present invention relates to hydrometallurgy and technology of fine chemicals, particularly relate to a kind of production technique being raw material production electronic-grade zinc oxide with high chlorine secondary zinc oxide.
Background technology
Along with the progress of science and technology, more and more higher to the purity requirement of zinc oxide.Electronic industry is produced zinc oxide chemical purity used and is required to reach 99.95%.A zinc oxide manufacturing enterprise if go out electronic-grade zinc oxide with impure high secondary zinc oxide for raw material production, then indicates that its production technique is quite perfect, has higher state of the art.
Mostly the existing method preparing electronic-grade zinc oxide is that based on the zinc oxide higher by purity be raw material, by being dissolved in acidity or basic solution, then deep purifying is carried out to solution, the last precursor being settled out high-purity zinc oxide from scavenging solution, then high-temperature calcination acquisition electronic-grade zinc oxide is carried out to precursor.The present invention is directly to be not suitable for the impure high high chlorine secondary zinc oxide of production electrolytic zinc for raw material, leached and meticulous solution purification operation by ammonium ammonia complexing, directly obtain the refined liquid of deep purifying, from refined liquid, be settled out the precursor of zinc hydroxide form again, obtain electronic-grade zinc oxide through high-temperature calcination.
Summary of the invention
For realizing above object, the present invention by the following technical solutions:
With high chlorine secondary zinc oxide for a technique for raw material production electronic-grade zinc oxide, comprise the following steps:
(1) leach: make leaching agent with ammoniacal liquor, volatile salt or ammonium sulfate, the zinc in high chlorine secondary zinc oxide is leached and makes zinc ammonia complex solution; This step principal reaction formula is as follows:
ZnO+2NH
4 ++2NH
3=Zn（NH
3）
4 2++H
2O
(2) iron removal by oxidation, manganese: add potassium permanganate and carry out oxidizing reaction in the leach liquor that above-mentioned operation obtains, make the Fe in leach liquor
2+, Mn
2+be oxidized to the Fe of indissoluble
3+, Mn
4+compound precipitation out, and filters excessively, obtains filtrate; This step principal reaction formula is as follows:
3Fe
2++Mn
7+=3Fe
3+↓+Mn
4+↓3Mn
2++2Mn
7+=5Mn
4+↓
(3) zinc dust precipitation copper removal, cadmium, lead: add zinc powder and carry out replacement(metathesis)reaction in the filtrate that above-mentioned operation obtains, makes copper, cadmium, plumbous Precipitation, and excessively filters, and is purified liquid; This step principal reaction formula is as follows:
Pb
2++Zn=Zn
2++Pb↓Cu
2++Zn=Zn
2++Cu↓Cd
2++Zn=Zn
2++Cd↓
This operation can make the copper content in solution be down to 0.0002g/L, and lead content is down to 0.002-0.005g/L, and cadmium content is down to 0.0001g/L.
(4) scavenging solution is refined: because the sulfide solubility product of the impurity such as Pb, Cu, Cd is very little. and the solubility product of ZnS is relatively large, therefore can (NH be selected
4)
2s does precipitation agent removal of impurities.
In order to carry out deep impurity-removing purification, in the scavenging solution that above-mentioned operation obtains, add ammonium sulfide solution, control temperature 30-40 DEG C, clarification time 30-120min; Metal ion remaining in scavenging solution is made to generate the coarse grained metallic sulfide being easy to sedimentation and filtration; Again through clarification and ageing, clarification and digestion time 60-600min, cross the sulfide filtering precipitation, obtain refined liquid.This step principal reaction formula is as follows:
Cd
2++S
2-=CdS↓Cu
2++S
2-=CuS↓Pb
2++S
2-=PbS↓Zn
2++S
2-=ZnS
Getting the solution through above-mentioned purification is placed on watch-glass, drips a rare ammonium sulfide solution, if the sulfide precipitation band black generated or grey, then illustrates that removal of impurities is incomplete, needs repetitive decontamination operation; If the sulfide precipitation generated is pure white, explanation generates pure zinc sulphide, and removal of impurities completes.
(5) neutralization precipitation zinc hydroxide: the refined liquid to the deep purifying containing network ammonia zine ion adds dilute sulphuric acid or special zinc sulfate ammonium double salt, and zinc is separated out from solution with zinc hydroxide form; This step principal reaction formula is as follows:
Zn（NH
3）
4 2++2H
2SO
4+2H
20=Z（OH）
2↓+2（NH
4）
2SO
4+2H
+
Zn（NH
3）
4 2++2ZnSO
4·（NH
4）
2SO
4·6H
20=3Zn（OH）
2↓+3（NH
4）
2SO
4+2H
+
(6) calcine: zinc hydroxide above-mentioned steps obtained increases pure water, through pressure filter press filtration, filter cake is sent into drying and calcining kiln and is obtained electronic-grade zinc oxide product through 1000-1100 DEG C of high-temperature calcination.This step principal reaction formula is as follows:
Zn（OH）
2=ZnO+H
20
The quality of scavenging solution purification of the present invention is the key ensureing product purity zinc oxide.In order to ensure that the heavy metal in solution obtains deep removal, when adding ammonium sulfide purification of heavy metal, take following measure: 1) accurate control has been carried out to purification temperature, the grain size of the sulfide that purification is generated is controlled, improve its settling velocity: the clarification time 2) increasing ammonium sulfide purification, make the reaction of removal of impurities more abundant; 3) ammonium sulfide adds in the form of a solution, avoids local reaction to make sulfonium ion fully contact with beavy metal impurity and to react; First the sulfonium ion added in fact is form zinc sulphide with a large amount of zine ion existed in solution to precipitate, then is changed into the sulfide of heavy metal by solid-liquid reaction by the beavy metal impurity ion in solid-state zinc sulphide and solution; Because this solid-liquid reaction is a slow process, so certain reaction times must be ensured; 4) extend the clarification of liquid and digestion time after purification, make precipitation and solution separating complete.
Compared with prior art, the beneficial effect that the present invention has is:
(1) a kind of technique that is raw material production electronic-grade zinc oxide with high chlorine secondary zinc oxide inferior provided by the invention, contrast routine is raw material production electronic-grade zinc oxide with high-grade zinc oxide is a kind of no small innovation.
(2) a kind of technique that is raw material production electronic-grade zinc oxide with high chlorine secondary zinc oxide provided by the invention, stable process conditions, operates simple and easy, is not only applicable to produce electronic-grade zinc oxide, and can be used for other high-grade zinc oxides of large-scale industrial production.
(3) produce electronic-grade zinc oxide with the high chlorine secondary zinc oxide being unsuitable for producing electrolytic zinc, eliminate the operation of medium temperature roast defluorinate, chlorine, make high chlorine secondary zinc oxide inferior obtain value added applications.
(4) extensive sodium sulphite is replaced except auxiliary work with the ammonium sulfide impurity removal process become more meticulous, both the deep purifying of heavy metal ion had been reached, turn avoid the pollution of sodium ion to solution, after making heavy zinc oxide, liquid can be recycled and reused for the leaching of raw material secondary zinc oxide, has saved reagent consumption.
Accompanying drawing illustrates:
Fig. 1 is of the present invention a kind of with the block diagram of high chlorine secondary zinc oxide for the technical process of raw material production electronic-grade zinc oxide.
Embodiment
Below in conjunction with the drawings and the specific embodiments, the present invention is described in detail.
Embodiment 1
With high chlorine secondary zinc oxide for raw material, its chemical composition is as shown in table 1.
The chemical composition of table 1 raw material secondary zinc oxide
| Element term | Zn | Fe | Pb | Cd | Cu | Mn | Cl |
| Content, % | 44.24 | 3.78 | 4.75 | 0.038 | 0.026 | 0.051 | 11.5 |
As can be seen from the composition of table 1, this secondary zinc oxide is the raw material that a kind of metal impurities and chlorion are high.
With the technique of above-mentioned secondary zinc oxide for raw material production electronic-grade zinc oxide, comprise the following steps:
(1) leach: make leaching solvent with ammoniacal liquor, industrial sulphuric acid ammonium, be dissolved under liquid-solid ratio is 4:1 by 50 grams of secondary zinc oxides in 80 grams of ammonium sulfate and 45 milliliters of ammoniacal liquor, thin up is 200 milliliters to liquid, and induction stirring leaches 3 hours.Filter, obtain leach liquor and wash water totally 240 milliliters, leached mud weighs 16.56 grams.The composition of leach liquor and wash water mixed solution and the composition of leached mud are respectively as shown in table 2 and table 3.By slag, the leaching yield of zinc is 82.56%; By liquid, the leaching yield of zinc is 79.36%.Leached mud is sent rotary kiln back to and is reclaimed zinc oxide.
The composition of table 2 leach liquor and wash water mixed solution
| Element term | Zn | Fe | Pb | Cd | Cu | Mn |
| Content, g/L | 73.14 | 0.0087 | 0.00086 | 0.050 | 0.00027 | 0.044 |
The composition of table 3 leached mud
| Element term | Zn | Fe | Pb | Cd | Cu | Mn |
| Content, % | 23.30 | 9.97 | 2.94 | 0.036 | 0.076 | 0.080 |
(2) iron removal by oxidation, manganese: add potassium permanganate in the leach liquor obtained in above-mentioned steps and wash water mixed solution and carry out oxidizing reaction, by the Fe in leach liquor
2+, Mn
2+be oxidized to the Fe of indissoluble
3+, Mn
4+compound precipitation out.
(3) zinc dust precipitation copper removal, cadmium, lead: add 2 grams of zinc powders and carry out replacement(metathesis)reaction in the filtrate that above-mentioned steps obtains, make copper, cadmium, plumbous Precipitation, and excessively filter, be purified liquid.
(4) add a small amount of ammonium sulfide solution in the scavenging solution obtained to above-mentioned steps, when the sulfide precipitation that filtrate added drop-wise ammonium sulfide solution generates is pure white, illustrate that removal of impurities is complete.
(5) neutralization precipitation zinc hydroxide: add dilute sulphuric acid or special zinc sulfate ammonium double salt to the deep purifying liquid containing network ammonia zine ion, zinc is separated out with zinc hydroxide form from solution.
(6) drying and calcining: zinc hydroxide above-mentioned steps obtained increases pure water, through pressure filter press filtration, filter cake is sent into drying and calcining kiln and is obtained electronic-grade zinc oxide product through 1000-1100 DEG C of high-temperature calcination.The composition of this zinc oxide product shows, ratio >=99.95% of Zn content and total metal content (calculating cadmium, copper, iron, manganese, plumbous five kinds of foreign metals), quality meets the requirement to electronic-grade zinc oxide.
Embodiment 2
Replace except 80 grams of ammonium sulfate except 50 grams of secondary zinc oxides being dissolved under liquid-solid ratio is 4:1 96 grams of bicarbonate of ammonia, other operations and embodiment 1 duplicate.Obtain the effect identical with embodiment 1.
Claims (7)
1. with high chlorine secondary zinc oxide for a production technique for raw material production electronic-grade zinc oxide, it is characterized in that: comprise the following steps:
(1) leach: make leaching solvent with ammoniacal liquor, volatile salt or ammonium sulfate, the zinc in high cl content secondary zinc oxide is leached and makes zinc ammonia complex solution;
(2) iron removal by oxidation, manganese: add potassium permanganate and carry out oxidizing reaction, by the Fe in leach liquor in the leach liquor that above-mentioned steps obtains
2+, Mn
2+be oxidized to the Fe of indissoluble
3+, Mn
4+compound precipitation out, and cross filter, obtain filtrate;
(3) zinc dust precipitation copper removal, cadmium, lead: add zinc powder and carry out replacement(metathesis)reaction in the filtrate that above-mentioned steps obtains, makes copper, cadmium, lead be precipitated out, and excessively filters, and is purified liquid;
(4) scavenging solution is refined: in the scavenging solution that above-mentioned steps obtains, add ammonium sulfide, makes metal ion remaining in scavenging solution generate the metallic sulfide of indissoluble, crosses and filter precipitation, obtain refined liquid;
(5) neutralization precipitation zinc hydroxide: add dilute sulphuric acid or special zinc sulfate ammonium double salt to the refined liquid containing network ammonia zine ion, zinc is separated out with zinc hydroxide form from solution;
(6) calcine: zinc hydroxide above-mentioned steps obtained adds water washing, through pressure filter press filtration, filter cake is sent into drying and calcining kiln and is obtained electronic-grade zinc oxide product through 1100 DEG C of high-temperature calcinations.
2. according to claim 1 a kind of with high chlorine secondary zinc oxide for the production technique of raw material production electronic-grade zinc oxide, it is characterized in that: during leaching, in leaching solvent, ammonia density is 75-90g/L, and volatile salt or ammonium sulfate concentrations are 80-150g/L; By total mol ratio NH during described leaching
4 +: Zn=4:1-1.2 drops into secondary zinc oxide, and extraction time is 2-4 hour.
3. according to the production technique that a kind of described in claim 1-2 is raw material production electronic-grade zinc oxide with high chlorine secondary zinc oxide, it is characterized in that: in step (2), described iron removal by oxidation reaction conditions is 40-70 DEG C, stirs, and the amount dropping into potassium permanganate is Fe in leach liquor
2++ Mn
2+the 2-10 of total mass doubly; Reaction times is 1-1.5 hour.
4. the production technique that a kind of according to claim 1-3 is raw material production electronic-grade zinc oxide with high chlorine secondary zinc oxide, it is characterized in that: in step (3), conditions of replacement reaction is doubly add zinc powder by the 2-4 of copper, cadmium, plumbous total mass in solution, and stirring reaction 30-60 minute.
5. the production technique that a kind of according to any one of claim 1-4 is raw material production electronic-grade zinc oxide with high chlorine secondary zinc oxide, it is characterized in that: in step (4), ammonium sulfide used is the ammonium sulfide of effective sulfur content 7-9%, dilute with water 8-10 doubly, under agitation slowly add in scavenging solution, react press filtration after 1-1.5 hour; The add-on of described ammonium sulfide is 1-1.15 times of the molar weight sum of the impurity such as copper, cadmium, lead.
6. be the production technique of raw material production electronic-grade zinc oxide with secondary zinc oxide according to a kind of described in claim 1-5, it is characterized in that: neutralization precipitation zinc hydroxide described in step (5) adopts the zinc sulfate ammonium double salt adding dilute sulphuric acid or obtain in advance by the refined liquid that dilute sulphuric acid acidifying contains network ammonia zine ion; Neutralization precipitation carries out under fully stirring, and when in solution, zinc ion concentration drops to below 1g/L, neutralization precipitation can stop.
7. according to the production technique that a kind of described in claim 1-6 is raw material production electronic-grade zinc oxide with high chlorine secondary zinc oxide, it is characterized in that: in step (5), gained zinc hydroxide drops in drying and calcining kiln after washing, press filtration, through 1000-1100 DEG C of high-temperature calcination, fully divide and solve electronic-grade zinc oxide.
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|---|---|---|---|
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109055764A (en) * | 2018-09-30 | 2018-12-21 | 贵州省兴安环保科技有限公司 | A kind of comprehensive recovering process of the low zinc material of high chlorine |
| CN109467118A (en) * | 2019-01-17 | 2019-03-15 | 柳三春 | Dechlorination containing chlorine zinc oxide complex and the method for distilling hydrochloric acid |
| CN110040763A (en) * | 2019-05-10 | 2019-07-23 | 河北远大中正生物科技有限公司 | It is a kind of using high chlorine secondary zinc oxide as the technique of raw material coproduction low sulfuric chlorohydrin zinc and common salt |
| CN112408461A (en) * | 2020-12-10 | 2021-02-26 | 平江县吉成科技有限责任公司 | Preparation method of feed-grade active zinc oxide |
| 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 |
| WO2021190025A1 (en) * | 2020-03-24 | 2021-09-30 | 鑫联环保科技股份有限公司 | Ammonium complex system-based method for separating and purifying lead, zinc, cadmium, and copper |
| CN115161492A (en) * | 2022-07-07 | 2022-10-11 | 桂林理工大学 | Method for preparing high-grade zinc oxide by treating secondary zinc oxide in rotary kiln |
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2015
- 2015-09-29 CN CN201510627821.2A patent/CN105197982A/en active Pending
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| CN109055764A (en) * | 2018-09-30 | 2018-12-21 | 贵州省兴安环保科技有限公司 | A kind of comprehensive recovering process of the low zinc material of high chlorine |
| CN109467118A (en) * | 2019-01-17 | 2019-03-15 | 柳三春 | Dechlorination containing chlorine zinc oxide complex and the method for distilling hydrochloric acid |
| CN110040763A (en) * | 2019-05-10 | 2019-07-23 | 河北远大中正生物科技有限公司 | It is a kind of using high chlorine secondary zinc oxide as the technique of raw material coproduction low sulfuric chlorohydrin zinc and common salt |
| WO2021190025A1 (en) * | 2020-03-24 | 2021-09-30 | 鑫联环保科技股份有限公司 | Ammonium complex system-based method for separating and purifying lead, zinc, cadmium, and copper |
| CN112408461A (en) * | 2020-12-10 | 2021-02-26 | 平江县吉成科技有限责任公司 | Preparation method of feed-grade active zinc oxide |
| CN112408461B (en) * | 2020-12-10 | 2022-08-16 | 平江县吉成科技有限责任公司 | Preparation method of feed-grade active zinc oxide |
| 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 |
| CN115161492A (en) * | 2022-07-07 | 2022-10-11 | 桂林理工大学 | Method for preparing high-grade zinc oxide by treating secondary zinc oxide in rotary kiln |
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