CN106884093B - A kind of thick aurin smelting method - Google Patents
A kind of thick aurin smelting method Download PDFInfo
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- CN106884093B CN106884093B CN201710188566.5A CN201710188566A CN106884093B CN 106884093 B CN106884093 B CN 106884093B CN 201710188566 A CN201710188566 A CN 201710188566A CN 106884093 B CN106884093 B CN 106884093B
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- filter residue
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- aurin
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- nitric acid
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- 238000000034 method Methods 0.000 title claims abstract description 65
- 238000003723 Smelting Methods 0.000 title claims abstract description 25
- FYEHYMARPSSOBO-UHFFFAOYSA-N Aurin Chemical compound C1=CC(O)=CC=C1C(C=1C=CC(O)=CC=1)=C1C=CC(=O)C=C1 FYEHYMARPSSOBO-UHFFFAOYSA-N 0.000 title claims abstract description 15
- 241001060848 Carapidae Species 0.000 title claims abstract description 15
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims abstract description 42
- 229910017604 nitric acid Inorganic materials 0.000 claims abstract description 42
- 238000001914 filtration Methods 0.000 claims abstract description 33
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 32
- 229910000906 Bronze Inorganic materials 0.000 claims abstract description 26
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000010974 bronze Substances 0.000 claims abstract description 26
- KUNSUQLRTQLHQQ-UHFFFAOYSA-N copper tin Chemical compound [Cu].[Sn] KUNSUQLRTQLHQQ-UHFFFAOYSA-N 0.000 claims abstract description 26
- 230000029087 digestion Effects 0.000 claims abstract description 24
- FGIUAXJPYTZDNR-UHFFFAOYSA-N potassium nitrate Chemical compound [K+].[O-][N+]([O-])=O FGIUAXJPYTZDNR-UHFFFAOYSA-N 0.000 claims abstract description 24
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 20
- 239000000706 filtrate Substances 0.000 claims abstract description 19
- 239000002893 slag Substances 0.000 claims abstract description 16
- 235000010333 potassium nitrate Nutrition 0.000 claims abstract description 12
- 239000004323 potassium nitrate Substances 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- 238000000184 acid digestion Methods 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 3
- 229910052737 gold Inorganic materials 0.000 claims description 66
- 239000010931 gold Substances 0.000 claims description 66
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 claims description 65
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 24
- 239000012535 impurity Substances 0.000 claims description 21
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 20
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 14
- 229910052787 antimony Inorganic materials 0.000 claims description 14
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims description 14
- 229910052709 silver Inorganic materials 0.000 claims description 14
- 239000004332 silver Substances 0.000 claims description 14
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 10
- 229910052802 copper Inorganic materials 0.000 claims description 10
- 239000010949 copper Substances 0.000 claims description 10
- 229910052742 iron Inorganic materials 0.000 claims description 10
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 9
- 229910052710 silicon Inorganic materials 0.000 claims description 9
- 239000010703 silicon Substances 0.000 claims description 9
- 235000006408 oxalic acid Nutrition 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 4
- IRPDISVJRAYFBI-UHFFFAOYSA-N nitric acid;potassium Chemical compound [K].O[N+]([O-])=O IRPDISVJRAYFBI-UHFFFAOYSA-N 0.000 claims description 2
- 230000008569 process Effects 0.000 abstract description 31
- 230000001698 pyrogenic effect Effects 0.000 abstract description 6
- NTVYFDOMBHOLGP-UHFFFAOYSA-N gold nitric acid Chemical compound [Au].O[N+]([O-])=O NTVYFDOMBHOLGP-UHFFFAOYSA-N 0.000 abstract description 2
- 239000013066 combination product Substances 0.000 abstract 1
- 229940127555 combination product Drugs 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 40
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 21
- 238000013019 agitation Methods 0.000 description 20
- 238000005406 washing Methods 0.000 description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 17
- 239000008367 deionised water Substances 0.000 description 15
- 229910021641 deionized water Inorganic materials 0.000 description 15
- 239000006260 foam Substances 0.000 description 15
- 229910052751 metal Inorganic materials 0.000 description 14
- 239000002184 metal Substances 0.000 description 14
- 238000000605 extraction Methods 0.000 description 8
- 238000007670 refining Methods 0.000 description 8
- 238000005868 electrolysis reaction Methods 0.000 description 7
- 238000002844 melting Methods 0.000 description 7
- 230000008018 melting Effects 0.000 description 7
- 238000011084 recovery Methods 0.000 description 7
- 239000002253 acid Substances 0.000 description 6
- 238000005266 casting Methods 0.000 description 6
- 239000004615 ingredient Substances 0.000 description 6
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 5
- 239000002585 base Substances 0.000 description 5
- 230000000052 comparative effect Effects 0.000 description 5
- 238000001816 cooling Methods 0.000 description 5
- 238000010790 dilution Methods 0.000 description 5
- 239000012895 dilution Substances 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 239000011591 potassium Substances 0.000 description 5
- 229910052700 potassium Inorganic materials 0.000 description 5
- 239000000047 product Substances 0.000 description 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 229910045601 alloy Inorganic materials 0.000 description 4
- 239000000956 alloy Substances 0.000 description 4
- 238000004090 dissolution Methods 0.000 description 4
- 239000003513 alkali Substances 0.000 description 3
- QZPSXPBJTPJTSZ-UHFFFAOYSA-N aqua regia Chemical compound Cl.O[N+]([O-])=O QZPSXPBJTPJTSZ-UHFFFAOYSA-N 0.000 description 3
- 229910044991 metal oxide Inorganic materials 0.000 description 3
- 150000004706 metal oxides Chemical class 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 230000004044 response Effects 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- RAHZWNYVWXNFOC-UHFFFAOYSA-N Sulphur dioxide Chemical compound O=S=O RAHZWNYVWXNFOC-UHFFFAOYSA-N 0.000 description 2
- UCXOJWUKTTTYFB-UHFFFAOYSA-N antimony;heptahydrate Chemical compound O.O.O.O.O.O.O.[Sb].[Sb] UCXOJWUKTTTYFB-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000005496 eutectics Effects 0.000 description 2
- 238000010304 firing Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- BZSXEZOLBIJVQK-UHFFFAOYSA-N 2-methylsulfonylbenzoic acid Chemical compound CS(=O)(=O)C1=CC=CC=C1C(O)=O BZSXEZOLBIJVQK-UHFFFAOYSA-N 0.000 description 1
- 229910001020 Au alloy Inorganic materials 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 241000416536 Euproctis pseudoconspersa Species 0.000 description 1
- 239000005708 Sodium hypochlorite Substances 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- 239000011324 bead Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 238000005660 chlorination reaction Methods 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000007499 fusion processing Methods 0.000 description 1
- -1 gold ion Chemical class 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- HWSZZLVAJGOAAY-UHFFFAOYSA-L lead(II) chloride Chemical compound Cl[Pb]Cl HWSZZLVAJGOAAY-UHFFFAOYSA-L 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- NICDRCVJGXLKSF-UHFFFAOYSA-N nitric acid;trihydrochloride Chemical compound Cl.Cl.Cl.O[N+]([O-])=O NICDRCVJGXLKSF-UHFFFAOYSA-N 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- VKJKEPKFPUWCAS-UHFFFAOYSA-M potassium chlorate Chemical compound [K+].[O-]Cl(=O)=O VKJKEPKFPUWCAS-UHFFFAOYSA-M 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 description 1
- 230000007928 solubilization Effects 0.000 description 1
- 238000005063 solubilization Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-L sulfite Chemical compound [O-]S([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-L 0.000 description 1
- 230000007306 turnover Effects 0.000 description 1
- 238000000108 ultra-filtration Methods 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B11/00—Obtaining noble metals
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B9/00—General processes of refining or remelting of metals; Apparatus for electroslag or arc remelting of metals
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The present invention relates to a kind of thick aurin smelting methods, and specific step is as follows：(1) thick gold nitric acid solution digestion, is obtained by filtration filter residue I；(2) potassium nitrate is added in filter residue I, is roasted after mixing, obtains fired slags；(3) potassium hydroxide solution digestion is added in fired slags, filter residue II is obtained by filtration；(4) by the nitric acid digestion of filter residue II, filter residue III is obtained by filtration；(5) hydrochloric acid is added in filter residue III and filtrate is obtained by filtration in hydrogen peroxide reaction, handle, obtain bronze.For bronze purity after being refined using this method 99.99% or more, which overcomes the general wet process-disadvantage that pyrogenic process combination product purity is not high, smelting temperature is high, process flow is complicated, the period is long.
Description
Technical field
The invention belongs to metallurgical technology fields, are related to a kind of thick gold refining technology.
Background technique
Gold is the metal that the mankind more early have found and utilize, and due to rare, special and precious, is considered as hardware since ancient times
First of, there is the title of the king of metal.It has high erosion-resisting stability, good electric conductivity and thermal conductivity, golden original
Daughter nucleus catches the effective cross-section for grabbing neutron with larger, has various catalyst properties in the alloy of gold.
The main method refined at present has electrolysis method, extraction, all-wet refining, wet process-pyrogenic process combination refining.
The basic principle of electro deposition is：Anode is done with thick gold, it is golden golden with other more electronegativity under direct current electro ultrafiltration
Belong to and enter electrolyte in the form of an ion, because gold ion concentration is big, current potential is high, and gold takes the lead in obtaining electronics precipitation in cathode, makes thick gold
It is purified.Fineness of gold obtained by electrolysis method is 99.99% or more, and quality is more stable, but electrolysis process has following lack
Point：It is high (generally requiring thick gold grade 90% or more) to ingredient requirement；Technical conditions are more demanding；Production cycle is long；Process
In overstock a large amount of gold, make troubles capital turnover and safeguarding work.
It is high, easy to operate excellent that extraction with respect to electrolysis process there is with short production cycle, process not overstock gold, direct yield
Gesture, but the deficiency of extraction is also quite obvious：The selectivity of the extractant of extraction process is little, and extraction reagent disappears
Consumption is big, and production pollution on the environment is larger, and work situation is poor, and waste gas pollution control and treatment is difficult, and extraction generally requires the gold of raw material
Content reaches 80-90%.
General Whote-wet method technique is：Thick bronze sulfuric acid treatment, dissolves away iron, zinc, if silver-colored grade is high then molten with nitric acid
Xie Yin and copper, finally with aqua regia dissolution gold (or make oxidant with one of chlorine, sodium chlorate, potassium chlorate, sodium hypochlorite,
Gold is dissolved in hydrochloric acid solution), insoluble matter (chloride containing silver, lead chloride and silica etc.) is isolated from gold-containing solution
Come, adjust pH value, golden chloro-complex is reduced into bronze with reducing agent oxalic acid (salt) or sulfur dioxide (sulphite), bronze is used
Nitric acid boils, and dissolves away the impurity wherein carried secretly, and bronze is repeatedly washed, and removes soluble impurity, dries, casts gold
Ingot.It is easy to operate using general wet processing, it is easy to accomplish mechanization, but the purity of obtained gold can only achieve
99.9% or so.
Wet process and pyrogenic process combination smelting process are generally divided into nitric acid point silver, the molten gold of chloroazotic acid, aqua regia residue pyrometallurgical smelting, electrolysis
Silver, gold, the techniques such as ingot casting.The technique there are the shortcomings that：First is that containing Jin Heyin in aqua regia residue, it is difficult to melting, in order to guarantee back
Yield reduces clinker taste, and during melting, temperature has reached 1000-1100 DEG C or so, smelting time reach 10h with
On, cause gold and silver to volatilize；Second is that process flow is complicated, equipment is various, and operating condition is poor；Third is that if the content of gold will reach
99.99%, it is necessary to which carrying out further refining using electrolysis method, extraction or chemical method again can be only achieved requirement.
The patent of Patent No. 011000597 discloses Amminochloride process of purifying gold, mainly includes following
Step：Nitric acid removal of impurities, filtration washing, chlorination leaching gold, filtration washing, golden reduction, filtration washing, golden melting, this method solve
The disadvantage of process flow complexity in general wet process and pyrogenic process combination smelting process, but this method smelting temperature reaches 1250 DEG C,
It is not fully solved the disadvantage that temperature is high in fusion process.
Application No. is 2014106516324 patents to disclose a kind of method of Enrichment purification gold, what this method used
Technical solution is：Alloy, sulfuric acid oxidation dissolution, Alkaline solubilization, nitric acid oxidation dissolution are configured, wherein configuration alloy is by gold head
Jewelry alloy waste material and tough cathode sprinkle pearl after melting at 1100-1250 DEG C, and then water quenching obtains alloy bead in the hot water, lead to
Cross efficiently concentrating and purification that the principle being constantly enriched with realizes gold.For smelting temperature at 1100-1250 DEG C, there is no complete in this method
Complete solution determine wet process-pyrogenic process combination smelting process the problem of.
Summary of the invention
In view of this, this method uses general wet process and pyrogenic process the object of the present invention is to provide a kind of thick aurin smelting method
It combines, as long as the gold content in thick gold is 70% or more, so that it may the product for being refined, and being obtained using this method
In, gold content reaches 99.99% or more.Overcome general wet process-pyrogenic process not high enough, pyrometallurgical smelting that combines method product purity
Temperature is high, the disadvantage of process flow complexity.This method raw material grade requirement is low, product grade is high, with short production cycle, operation letter
It is single, mechanization easy to accomplish.
The present invention provides a kind of thick aurin smelting methods, and specific step is as follows：
(1) thick gold nitric acid solution digestion, filtering obtain filter residue I；
(2) potassium nitrate is added in filter residue I, is roasted after mixing, obtains fired slags；
(3) by fired slags and potassium hydroxide solution digestion, filter residue II is obtained by filtration；
(4) by the nitric acid digestion of filter residue II, filtering obtains filter residue III；
(5) hydrochloric acid and hydrogen peroxide reaction is added in filter residue III, filtrate is obtained by filtration；Processing, obtains bronze.
Preferably, in step (1), the mass percent of the nitric acid is 15-30%, the weighing body of thick gold and nitric acid solution
Product is than being 1:1-3.
Preferably, in step (2), the temperature of the roasting is 450-600 DEG C.
Preferably, in step (2), the nitric acid potassium application rate is the 10%-40% of I weight of filter residue.
Preferably, in step (3), the mass percent of the potassium hydroxide solution is 10-40%, fired slags and hydrogen-oxygen
The w/v for changing potassium solution is 1:1-3.
Preferably, in step (4), the mass percent of the nitric acid is 10-20%, and the weight of filter residue II and nitric acid is 1:
1-3。
Preferably, in step (5), the volumetric concentration of hydrochloric acid is 15-36%.
Preferably, in step (5), the volume of the hydrogen peroxide is 0.2-0.4 times of hydrochloric acid volume.
Preferably, obtained in step (5) filtrate the specific steps are：Hydrochloric acid is added in filter residue III, heats and stirs, then
Hydrogen peroxide is added, reacts, filtering obtains filtrate.
It preferably, is that filtrate is adjusted into pH value in 1.5-3, heats and stirs, add the step of processing in step (5)
Oxalic acid reacts, and filters, and drying obtains bronze.
Beneficial effects of the present invention：Potassium nitrate is added in firing stage in the present invention, can allow the metal congruent melting for being insoluble in soda acid
Body, antimony metal, metal impurities are in roasting and nitric acid nak response generates the metal oxide for being soluble in acid and the burnt antimony for being dissolved in alkali
Sour potassium, to lay the foundation for subsequent further removing impurity.
The temperature of roasting is only needed at 450-600 DEG C, compared to 1000-1200 DEG C of general gold pyrometallurgical smelting, temperature
It is relatively very low, and the time of melting is very short, it being capable of the effectively save energy.
The impurity of thick gold is mainly silver, antimony, iron, copper, silicon, and gold content first uses nitric acid digestion can in 70-90%, thick bronze
To remove most silver, iron, copper, there are also a small amount of metal (such as antimony), with metal impurities existing for eutectic or metal inclusion
It is difficult to be dissolved with soda acid and remove, potassium nitrate is added in filter residue I and is roasted, indissoluble impurity antimony can generate molten with nitric acid nak response
In the potassium pyroantimonate of alkali, other metal impurities can generate the metal oxide for being soluble in acid with nitric acid nak response, and fired slags pass through
Foreign metal antimony and impurity silicon can be dissolved in alkaline solution and be removed by potassium hydroxide digestion, and potassium hydroxide digestion slag is through pernitric acid
Digestion can further remove impurity silver, iron, copper, and by above step, the impurity in thick gold eliminates substantially, it is subsequent will be golden
Be dissolved in the solution of hydrochloric acid and hydrogen peroxide, filtering can remove impurity silicon and remaining argentalium, Jinliu in the solution, by also
Former and cleaning obtains the bronze that purity reaches 99.99% or more, and the rate of recovery of gold reaches 98% or more.
Using step of the invention, first most energy dissolved impurity is removed, is then directed to indissoluble impurity antimony, metal
Eutectic, metal inclusion are added potassium nitrate in leached mud I and carry out calcination process, antimony is converted to the pyroantimonic acid for being soluble in alkali
Potassium, other converting metal impurities are the metal oxide for being soluble in acid, and fired slags digestion in potassium hydroxide is molten by potassium pyroantimonate
Solution removes, and further removes other metal impurities by nitric acid digestion again, thus eliminates the impurity in thick gold substantially
, using golden dissolution and separate out the impurity further removed in slightly gold, so that impurity substantially completely eliminates, and obtains
The gold that gold content is 99.99%.
The present invention requires to reduce compared to electrolysis method and extraction to the gold content of raw material, and overcomes general wet process
The disadvantage that the method for refining product purity combined with pyrogenic process is inadequate, gold and silver is difficult to melting, process flow complexity, life of the invention
It is fewer to produce step, with short production cycle, method and easy to operate, it is easy to accomplish mechanization, small pollution of the environment.
Specific embodiment
Embodiment 1
Slightly the percentage composition of each ingredient of gold is：Gold 70.35%, silver 20.05%, copper 3.32%, iron 3.19%, antimony
1.64%, silicon 1.35%.Implementation steps are as follows：
(1) the thick bronze of 50.4879g is weighed, addition mass fraction is 20% nitric acid solution 100mL, is placed in digestion on electric furnace
2h, filtering, filter residue I are washed with deionized 3 times, and filter residue weight in wet base is 39.3214g.
(2) 16g potassium nitrate is added in the filter residue I that step (1) obtains, and mixes, send Muffle kiln roasting 1.5h, maturing temperature is
600℃。
(3) it is 25% potassium hydroxide solution 80mL digestion 1h that mass fraction, which is added, in the fired slags that step (2) obtains, and is filtered,
Filter residue II is washed with deionized 3 times.
(4) it is 15% nitric acid solution 80mL digestion 1h, filtering, filter residue that mass fraction, which is added, in the filter residue II that step (3) obtains
III is washed 3 times with 5% nitric acid solution.
(5) it is that 20% hydrochloric acid solution 80mL is placed in magnetic agitation water-bath that mass fraction, which is added, in the filter residue III that step (4) obtains
In pot, bath temperature is 85 DEG C, under conditions of magnetic agitation, is slowly added to 20mL hydrogen peroxide with constant flow pump, reacts 2h, reaction
After be added 80mL deionized water dilution, cooling and standings 0.5h, filtering, obtain filtrate, the deionized water foam washing 3 of filter residue IV
It is secondary.
(6) filtrate obtained by step (5) adjusts pH value in 1.5-3 with saturation sodium hydroxide solution, is placed in magnetic agitation water-bath
In pot, bath temperature is 85 DEG C, under conditions of magnetic agitation, 37g oxalic acid is added and reacts 1h, filters while hot, bronze quality
Score is nitric acid solution foam washing 2 times of 10%, then with deionized water foam washing 3 times, drying, ingot casting, gold content 99.992%,
Weight is 34.8075g, and the golden rate of recovery is 98%.
Embodiment 2
Slightly bronze ingredient is：Gold 70.35%, silver 20.05%, copper 3.32%, iron 3.19%, antimony 1.64%, silicon 1.35%.
Implementation steps are as follows：
(1) the thick bronze of 50.3245g is weighed, addition mass fraction is 20% nitric acid solution 100mL, is placed in digestion on electric furnace
1h, filtering, filter residue I are washed with deionized 3 times, and filter residue weight in wet base is 38.3214g.
(2) 16g potassium nitrate is added in the filter residue I that step (1) obtains, and mixes, send Muffle kiln roasting 2h, maturing temperature is
500℃。
(3) it is 5% that mass fraction, which is added, in the fired slags that step (2) obtains
Potassium hydroxide solution 200mL digestion 1h, filtering, filter residue II are washed with deionized 3 times.
(4) it is 15% nitric acid solution 110mL digestion 1h, filtering, filter residue that mass fraction, which is added, in the filter residue II that step (3) obtains
It is washed 3 times with 5% nitric acid solution.
(5) it is that 15% hydrochloric acid solution 110mL is placed in magnetic agitation water-bath that mass fraction, which is added, in the filter residue III that step (4) obtains
In pot, bath temperature is 85 DEG C, under conditions of magnetic agitation, is slowly added to 40mL hydrogen peroxide with constant flow pump, reacts 2h, reaction
After be added 170mL deionized water dilution, cooling and standings 0.5h, filtering, obtain filtrate, the deionized water foam washing of filter residue IV
3 times.
(6) filtrate obtained by step (5) adjusts pH value in 1.5-3 with saturation sodium hydroxide solution, is placed in magnetic agitation water-bath
In pot, bath temperature is 85 DEG C, under conditions of magnetic agitation, 37g oxalic acid is added and reacts 1h, filters while hot, bronze quality
Score is nitric acid solution foam washing 2 times of 10%, then with deionized water foam washing 3 times, drying, ingot casting, gold content 99.991%,
Weight is 34.6952g, and the golden rate of recovery is 98%.
Embodiment 3
Slightly bronze ingredient is：Gold 81.15%, silver 11.27%, copper 2.37%, iron 2.08%, antimony 1.70%, silicon 1.43%.
Implementation steps are as follows：
(1) the thick bronze of 50.5064g is weighed, addition mass fraction is 30% nitric acid solution 45mL, is placed in digestion on electric furnace
1h, filtering, filter residue I are washed with deionized 3 times, and filter residue weight in wet base is 39.5324g.
(2) 8g potassium nitrate is added in the filter residue I that step (1) obtains, and mixes, send Muffle kiln roasting 1.5h, maturing temperature is
500℃。
(3) it is 30% potassium hydroxide solution 45mL digestion 1h that mass fraction, which is added, in the fired slags that step (2) obtains, and is filtered,
Filter residue II is washed with deionized 3 times.
(4) it is 30% nitric acid solution 45mL digestion 1h, filtering, filter residue that mass fraction, which is added, in the filter residue II that step (3) obtains
It is washed 3 times with 5% nitric acid solution.
(5) it is that 35% hydrochloric acid solution 55mL is placed in magnetic agitation water-bath that mass fraction, which is added, in the filter residue III that step (4) obtains
In pot, bath temperature is 80 DEG C, under conditions of magnetic agitation, is slowly added to 22mL hydrogen peroxide with constant flow pump, reacts 2h, reaction
After be added 110mL deionized water dilution, cooling and standings 1h, filtering, obtain filtrate, the deionized water foam washing 3 of filter residue IV
It is secondary.
(6) filtrate obtained by step (5) adjusts pH value in 1.5-3 with saturation sodium hydroxide solution, is placed in magnetic agitation water-bath
In pot, bath temperature is 80 DEG C, under conditions of magnetic agitation, 44g oxalic acid is added and reacts 1h, filters while hot, bronze quality
Score is nitric acid solution foam washing 2 times of 10%, then with deionized water foam washing 3 times, drying, ingot casting, gold content 99.992%,
Weight is 40.2483g, and the golden rate of recovery is 98.2%.
Embodiment 4
Slightly bronze ingredient is：Gold 90.64%, silver 6.47%, copper 1.25%, iron 0.78%, antimony 0.53%, silicon 0.33%.
Implementation steps are as follows：
(1) the thick bronze of 50.5647g is weighed, addition mass fraction is 15% nitric acid solution 100mL, is placed in digestion on electric furnace
1h, filtering, filter residue I are washed with deionized 3 times, and filter residue weight in wet base is 46.9677g.
(2) 4.6g potassium nitrate is added in the filter residue I that step (1) obtains, and mixes, send Muffle kiln roasting 2h, maturing temperature is
600℃。
(3) it is 10% potassium hydroxide solution 100mL digestion 1h that mass fraction, which is added, in the fired slags that step (2) obtains, and is filtered,
Filter residue II is washed with deionized 3 times.
(4) it is 30% nitric acid solution 45mL digestion 1h, filtering, filter residue that mass fraction, which is added, in the filter residue II that step (3) obtains
It is washed 3 times with 5% nitric acid solution.
(5) it is that 35% hydrochloric acid solution 70mL is placed in magnetic agitation water-bath that mass fraction, which is added, in the filter residue III that step (4) obtains
In pot, bath temperature is 90 DEG C, under conditions of magnetic agitation, is slowly added to 25mL hydrogen peroxide with constant flow pump, reacts 2h, reaction
After be added 110mL deionized water dilution, cooling and standings 1h, filtering, obtain filtrate, the deionized water foam washing 3 of filter residue IV
It is secondary.
(6) filtrate obtained by step (5) adjusts pH value in 1.5-3 with saturation sodium hydroxide solution, is placed in magnetic agitation water-bath
In pot, bath temperature is 90 DEG C, under conditions of magnetic agitation, 46g oxalic acid is added and reacts 1h, filters while hot, bronze quality
Score is nitric acid solution foam washing 2 times of 10%, then with deionized water foam washing 3 times, drying, ingot casting, gold content 99.993%,
Weight is 45.0561g, and the golden rate of recovery is 98.3%.
Comparative example
Slightly bronze ingredient is：Gold 70.35%, silver 20.05%, copper 3.32%, iron 3.19%, antimony 1.64%, silicon 1.35%.
Implementation steps are as follows：
(1) the thick bronze of 50.3245g is weighed, addition mass fraction is 20% nitric acid solution 100mL, is placed in digestion on electric furnace
1h, filtering, filter residue I are washed with deionized 3 times, and filter residue weight in wet base is 38.3214g.
(2) filter residue I that step (1) obtains is added 16g sodium hydroxide and send Muffle kiln roasting 2h, and maturing temperature is 500 DEG C.
(3) it is 5% potassium hydroxide solution 200mL digestion 1h that mass fraction, which is added, in the fired slags that step (2) obtains, and is filtered,
Filter residue II is washed with deionized 3 times.
(4) it is 15% nitric acid solution 110mL digestion 1h, filtering, filter residue that mass fraction, which is added, in the filter residue II that step (3) obtains
It is washed 3 times with 5% nitric acid solution.
(5) it is that 15% hydrochloric acid solution 110mL is placed in magnetic agitation water-bath that mass fraction, which is added, in the filter residue III that step (4) obtains
In pot, bath temperature is 85 DEG C, under conditions of magnetic agitation, is slowly added to 40mL hydrogen peroxide with constant flow pump, reacts 2h, reaction
After be added 170mL deionized water dilution, cooling and standings 0.5h, filtering, obtain filtrate, the deionized water foam washing of filter residue IV
3 times.
(6) filtrate obtained by step (5) adjusts pH value in 1.5-3 with saturation sodium hydroxide solution, is placed in magnetic agitation water-bath
In pot, bath temperature is 85 DEG C, under conditions of magnetic agitation, 37g oxalic acid is added and reacts 1h, filters while hot, bronze quality
Score is nitric acid solution foam washing 2 times of 10%, then with deionized water foam washing 3 times, drying, ingot casting, gold content 98.02%,
Weight is 36.9124g, and the golden rate of recovery is 90%.
Comparative example is compared with embodiment 2, and the main distinction is embodiment 2 in the roasting process of step (2)
In joined the potassium nitrate of 60g, and what is be added in comparative example is sodium hydroxide, the gold content for the gold that embodiment 2 obtains
It is 99.991%, the rate of recovery of gold is 98%, and the gold content that comparative example obtains gold is 98.02%, the recycling of gold
Rate is 90%, and embodiment 2 and comparative example are added potassium nitrate in firing stage as the result is shown and have effect outstanding, significantly
Improve the gold content of gold after refining.General wet refining process, gold content can only achieve 99.9%, and it is special to generally require
Processing the gold content of gold could be made to reach 99.99%, compared to general wet refining process, the gold of this patent gold
Content reaches 99.99% or more, has effect outstanding, and compared to refinery practice associated with general wet process and pyrogenic process, this is specially
The step of benefit is simple, easy to accomplish, and the temperature roasted only has 450-600 DEG C, and temperature is lower, can the effectively save energy.
Claims (10)
1. a kind of thick aurin smelting method, which is characterized in that include the following steps：
(1) slightly golden nitric acid solution digestion will be used, the impurity of the thick gold is mainly silver, antimony, iron, copper, silicon, and gold content is in 70-
90%, it then filters, obtains filter residue I；
(2) potassium nitrate is added in filter residue I, is roasted after mixing, obtains fired slags；
(3) potassium hydroxide solution digestion is added in fired slags, filter residue II is obtained by filtration；
(4) by the nitric acid digestion of filter residue II, filtering obtains filter residue III；
(5) hydrochloric acid and hydrogen peroxide reaction is added in filter residue III, filtrate is obtained by filtration；Processing, obtains bronze.
2. thick aurin smelting method according to claim 1, which is characterized in that in step (1), the quality percentage of the nitric acid
Number is 15-30%, and the w/v of thick gold and nitric acid solution is 1:1-3.
3. thick aurin smelting method according to claim 1, which is characterized in that in step (2), the temperature of the roasting is
450-600℃。
4. thick aurin smelting method according to claim 1, which is characterized in that in step (2), nitric acid potassium application rate is filter residue I
The 10%-40% of weight.
5. thick aurin smelting method according to claim 1, which is characterized in that in step (3), the potassium hydroxide solution
Mass percent be 5-30%, the w/v of fired slags and potassium hydroxide solution is 1:1-3.
6. thick aurin smelting method according to claim 1, which is characterized in that in step (4), the quality percentage of the nitric acid
Counting is 10-20%, and the w/v of filter residue II and nitric acid is 1:1-3.
7. thick aurin smelting method according to claim 1, which is characterized in that in step (5), the volumetric concentration of hydrochloric acid is
15-36%.
8. thick aurin smelting method according to claim 1, which is characterized in that in step (5), the volume of the hydrogen peroxide is
0.2-0.4 times of hydrochloric acid volume.
9. thick aurin smelting method according to claim 1-8, which is characterized in that step obtains filtrate in (5)
The specific steps are：Hydrochloric acid is added in filter residue III, heats and stirs, hydrogen peroxide is then added, react, filtering obtains filtrate.
10. thick aurin smelting method according to claim 1-8, which is characterized in that in step (5) the step of processing
For filtrate is adjusted pH value in 1.5-3, heats and stirs, add oxalic acid, react, filter, drying obtains bronze.
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| AU2021329906A1 (en) | 2020-08-18 | 2023-04-27 | Enviro Metals, LLC | Metal refinement |
| CN114453589B (en) * | 2022-02-18 | 2022-11-29 | 贵研铂业股份有限公司 | Preparation method of high-purity gold |
| CN114577977B (en) * | 2022-03-30 | 2023-04-21 | 山东省地质矿产勘查开发局第六地质大队(山东省第六地质矿产勘查院) | Method for analyzing gold ore containing graphite and sample roasting effect analysis equipment thereof |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101024864A (en) * | 2007-02-14 | 2007-08-29 | 苏州天地环境科技有限公司 | Method for recovering gold and copper from gold-plated printed circuit board waste material |
| CN101122032A (en) * | 2007-05-21 | 2008-02-13 | 江西铜业集团公司 | One-step producing technique for high-purity gold |
| CN103233132A (en) * | 2013-04-22 | 2013-08-07 | 金川集团股份有限公司 | Method for removing impurities from gold powder |
| CN103667706A (en) * | 2013-11-29 | 2014-03-26 | 重庆材料研究院有限公司 | Separation and purification method of gold in gold platinum alloy waste |
| CN103882240A (en) * | 2014-04-16 | 2014-06-25 | 芒市海华开发有限公司 | Method and equipment for extracting gold and silver from smelting slag |
| CN104017994A (en) * | 2014-06-17 | 2014-09-03 | 昆明贵金属研究所 | Method for recovering gold and tin from gold-tin alloy scrap |
| CN104328284A (en) * | 2014-11-17 | 2015-02-04 | 中南大学 | Method for enriching and purifying gold |
-
2017
- 2017-03-27 CN CN201710188566.5A patent/CN106884093B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101024864A (en) * | 2007-02-14 | 2007-08-29 | 苏州天地环境科技有限公司 | Method for recovering gold and copper from gold-plated printed circuit board waste material |
| CN101122032A (en) * | 2007-05-21 | 2008-02-13 | 江西铜业集团公司 | One-step producing technique for high-purity gold |
| CN103233132A (en) * | 2013-04-22 | 2013-08-07 | 金川集团股份有限公司 | Method for removing impurities from gold powder |
| CN103667706A (en) * | 2013-11-29 | 2014-03-26 | 重庆材料研究院有限公司 | Separation and purification method of gold in gold platinum alloy waste |
| CN103882240A (en) * | 2014-04-16 | 2014-06-25 | 芒市海华开发有限公司 | Method and equipment for extracting gold and silver from smelting slag |
| CN104017994A (en) * | 2014-06-17 | 2014-09-03 | 昆明贵金属研究所 | Method for recovering gold and tin from gold-tin alloy scrap |
| CN104328284A (en) * | 2014-11-17 | 2015-02-04 | 中南大学 | Method for enriching and purifying gold |
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