CN106119567B - A method of gold of purifying metals - Google Patents
A method of gold of purifying metals Download PDFInfo
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- CN106119567B CN106119567B CN201610808559.6A CN201610808559A CN106119567B CN 106119567 B CN106119567 B CN 106119567B CN 201610808559 A CN201610808559 A CN 201610808559A CN 106119567 B CN106119567 B CN 106119567B
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- gold
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- hydrogen peroxide
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- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 title claims abstract description 105
- 229910052737 gold Inorganic materials 0.000 title claims abstract description 105
- 239000010931 gold Substances 0.000 title claims abstract description 105
- 238000000034 method Methods 0.000 title claims abstract description 31
- 229910052751 metal Inorganic materials 0.000 title claims abstract description 12
- 239000002184 metal Substances 0.000 title claims abstract description 12
- 150000002739 metals Chemical class 0.000 title claims abstract description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- WQYVRQLZKVEZGA-UHFFFAOYSA-N hypochlorite Chemical compound Cl[O-] WQYVRQLZKVEZGA-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000002253 acid Substances 0.000 claims abstract description 8
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 7
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 58
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 50
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 42
- OAKJQQAXSVQMHS-UHFFFAOYSA-N Hydrazine Chemical compound NN OAKJQQAXSVQMHS-UHFFFAOYSA-N 0.000 claims description 36
- 239000011780 sodium chloride Substances 0.000 claims description 29
- 239000000126 substance Substances 0.000 claims description 25
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 24
- 229910000906 Bronze Inorganic materials 0.000 claims description 20
- 239000010974 bronze Substances 0.000 claims description 20
- KUNSUQLRTQLHQQ-UHFFFAOYSA-N copper tin Chemical compound [Cu].[Sn] KUNSUQLRTQLHQQ-UHFFFAOYSA-N 0.000 claims description 20
- 239000000706 filtrate Substances 0.000 claims description 14
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims description 14
- JAJIPIAHCFBEPI-UHFFFAOYSA-N 9,10-dioxoanthracene-1-sulfonic acid Chemical compound O=C1C2=CC=CC=C2C(=O)C2=C1C=CC=C2S(=O)(=O)O JAJIPIAHCFBEPI-UHFFFAOYSA-N 0.000 claims description 13
- 238000007254 oxidation reaction Methods 0.000 claims description 13
- 238000006722 reduction reaction Methods 0.000 claims description 13
- 239000012266 salt solution Substances 0.000 claims description 13
- 238000005868 electrolysis reaction Methods 0.000 claims description 10
- 239000005708 Sodium hypochlorite Substances 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 6
- 230000008929 regeneration Effects 0.000 claims description 6
- 238000011069 regeneration method Methods 0.000 claims description 6
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 claims description 2
- 239000000460 chlorine Substances 0.000 claims description 2
- 229910052801 chlorine Inorganic materials 0.000 claims description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 abstract description 12
- 238000004090 dissolution Methods 0.000 abstract description 8
- 239000000243 solution Substances 0.000 description 14
- 238000006243 chemical reaction Methods 0.000 description 13
- 230000001376 precipitating effect Effects 0.000 description 11
- 239000012535 impurity Substances 0.000 description 10
- 239000003513 alkali Substances 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 7
- -1 alkaline earth metal hypochlorite Chemical class 0.000 description 6
- 239000000843 powder Substances 0.000 description 6
- 239000000376 reactant Substances 0.000 description 6
- 238000003556 assay Methods 0.000 description 5
- 238000001914 filtration Methods 0.000 description 5
- 230000007935 neutral effect Effects 0.000 description 5
- SDLBJIZEEMKQKY-UHFFFAOYSA-M silver chlorate Chemical compound [Ag+].[O-]Cl(=O)=O SDLBJIZEEMKQKY-UHFFFAOYSA-M 0.000 description 5
- NICDRCVJGXLKSF-UHFFFAOYSA-N nitric acid;trihydrochloride Chemical compound Cl.Cl.Cl.O[N+]([O-])=O NICDRCVJGXLKSF-UHFFFAOYSA-N 0.000 description 4
- 238000000746 purification Methods 0.000 description 4
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 238000000605 extraction Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 description 2
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 description 2
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- QWPPOHNGKGFGJK-UHFFFAOYSA-N hypochlorous acid Chemical compound ClO QWPPOHNGKGFGJK-UHFFFAOYSA-N 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 229910021645 metal ion Inorganic materials 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 239000011669 selenium Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- FFRBMBIXVSCUFS-UHFFFAOYSA-N 2,4-dinitro-1-naphthol Chemical compound C1=CC=C2C(O)=C([N+]([O-])=O)C=C([N+]([O-])=O)C2=C1 FFRBMBIXVSCUFS-UHFFFAOYSA-N 0.000 description 1
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 description 1
- ZKQDCIXGCQPQNV-UHFFFAOYSA-N Calcium hypochlorite Chemical compound [Ca+2].Cl[O-].Cl[O-] ZKQDCIXGCQPQNV-UHFFFAOYSA-N 0.000 description 1
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 description 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- REDXJYDRNCIFBQ-UHFFFAOYSA-N aluminium(3+) Chemical compound [Al+3] REDXJYDRNCIFBQ-UHFFFAOYSA-N 0.000 description 1
- 229910052787 antimony Inorganic materials 0.000 description 1
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229910052785 arsenic Inorganic materials 0.000 description 1
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 239000001110 calcium chloride Substances 0.000 description 1
- 229910001628 calcium chloride Inorganic materials 0.000 description 1
- 239000013626 chemical specie Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910001629 magnesium chloride Inorganic materials 0.000 description 1
- YZQBYALVHAANGI-UHFFFAOYSA-N magnesium;dihypochlorite Chemical compound [Mg+2].Cl[O-].Cl[O-] YZQBYALVHAANGI-UHFFFAOYSA-N 0.000 description 1
- 239000011572 manganese Substances 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
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000010907 mechanical stirring Methods 0.000 description 1
- 238000005555 metalworking Methods 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001103 potassium chloride Substances 0.000 description 1
- 235000011164 potassium chloride Nutrition 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-L sulfite Chemical compound [O-]S([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-L 0.000 description 1
- 239000002351 wastewater 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
- C22B11/04—Obtaining noble metals by wet processes
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Electrolytic Production Of Metals (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Treatment Of Water By Oxidation Or Reduction (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
Abstract
The invention discloses a kind of methods of gold of purifying metals.The present invention purify metals gold method, thick gold is dissolved in the mixed liquor containing chloride ion and hypochlorite ion in acid condition first, then lysigenous solubilised state gold is restored with reducing agent.The product of the dissolution is generated in addition to solubilised state gold and water, no other any exhaust gas.In addition, the purity of purified metallic gold of the invention is not less than 99.99%.
Description
Technical field
The present invention relates to the technical fields of metalworking, in particular to a kind of method of gold of purifying metals.
Background technique
The chemical elemental symbol of gold is Au, is a kind of soft, golden yellow, erosion-resisting noble metal.Gold is jewellery industry, electricity
Sub- industry, modern communication, space flight and aviation Ye Deng department important materials.
Currently, mainly having chloroazotic acid method, Boliden technique (chloridising), extraction, electrolysis method to the method for purification of metallic gold
Four kinds.Chloroazotic acid method refer to thick gold be dissolved in chloroazotic acid (by amount of substance than for 4:1 hydrochloric acid and nitric acid mix), wait drive away
After nitric acid, restore.Boliden technique, which refers to, is dissolved in thick gold in hydrochloric acid and chlorine, restores.Extraction is that thick gold is molten
Solution is in chloroazotic acid, then extracts back extraction, finally restores.Electrolysis method, which refers to, is dissolved in thick gold in hydrochloric acid, then electroreduction.
Above in the prior art, the golden generally existing exhaust gas wastewater flow rate of method of purifying metals is big, larger to the pollution of environment.
In addition, the purity of purification is limited.
Summary of the invention
In view of this, one aspect of the present invention is to provide a kind of method of gold of purifying metals, this method is more environmentally friendly, purification
Purity it is higher.
A method of gold of purifying metals, comprising the following steps:
(1) make thick gold that oxidation reaction, shape occur with the mixed liquor containing chloride ion and hypochlorite ion in acid condition
At the gold salt solution containing solubilised state gold；
(2) make the solubilised state gold that reduction reaction occur with reducing agent, obtain purifying gold.
Further, pH acid described in step (1) is 4~7.
Further, the temperature of oxidation reaction described in step (1) is 40~60 DEG C, time of oxidation reaction is 90~
120min。
Further, in step (1), the amount of substance by thick gold is in terms of 1, and the dosage of chloride ion is 2.5~4, hypochlorous acid from
The dosage of son is 2~3.
Further, reduction reaction described in step (2) includes being restored by hydrogen peroxide and being restored by hydrazine later.
Further, the dosage for restoring used hydrogen peroxide by hydrogen peroxide is 2~2.5, with the solubilised state gold
Amount of substance be 1 meter.
Further, the temperature restored by hydrogen peroxide is 55~65 DEG C.
Further, the temperature restored by hydrazine is 50~60 DEG C.
Further, the step (1) further includes before the step for making the gold salt solution alkalinity later and in step (2)
Suddenly, the pH of the alkalinity is 9.5~10.0.
Further, it is 100 mesh bronze below that the thick gold, which is granularity,.
The present invention purify metals gold method, thick gold is dissolved in acid condition containing chloride ion and hypochlorous acid first
The mixed liquor of ion, then lysigenous solubilised state gold is restored with reducing agent.The product of the dissolution in addition to solubilised state gold and water,
No other any exhaust gas generate.In addition, the purity of purified metallic gold of the invention is not less than 99.99%.
Specific embodiment
To facilitate the understanding of the present invention, embodiment to further illustrate the technical scheme of the present invention is closed below.
As used herein, term:
" mass parts " refer to the basic measurement unit for indicating the mass ratio relationship of multiple components, and 1 part can indicate arbitrary list
Position quality, can such as be expressed as 1g, may also indicate that 2.689g etc..If we say that the mass parts of component A are a parts, the matter of B component
Measuring part is b parts, then it represents that the quality of component A and the mass ratio a:b of B component.Or ground, indicate that the quality of component A is aK, B
The quality of component is bK (K is arbitrary number, indicates multiplying factor).It can not misread, unlike mass fraction, all groups
The sum of the mass parts divided are not limited to 100 parts of limitation.
"one", "an" and " described " be used interchangeably and refer to one or more.
"and/or" is used to indicate that one of illustrated situation or both may to occur, for example, A and/or B includes (A
And B) and (A or B)；
In addition, herein by endpoint state range include included within the scope of this all numerical value (for example, 1 to 10 packet
Include 1.4,1.9,2.33,5.75,9.98 etc.).
In addition, the statement of "at least one" herein is including one or more all number (for example, at least two, at least
4, at least six, at least eight, at least ten, at least 25, at least 50, at least 100 etc.).
The method of gold of purifying metals of the invention, comprising the following steps:
(1) make thick gold that oxidation reaction, shape occur with the mixed liquor containing chloride ion and hypochlorite ion in acid condition
At the gold salt solution containing solubilised state gold；
(2) make the solubilised state gold that reduction reaction occur with reducing agent, obtain purifying gold.
In above-mentioned steps (1), the equation of oxidation reaction is 5Cl-+3ClO-+8H++ 2Au=2HAuCl4+3H2O。
Above-mentioned term " solubilised state gold " refers to gold element in water and is in the chemical species of dissolution, such as may include simple metal
Ion, hydrated metal ion, hydroxo complex, complex ions.Based on the equation of above-mentioned oxidation reaction, solubilised state here
Gold is mainly [AuCl4]-。
Above-mentioned thick gold can be not less than the gold of 90wt% for gold content, and contain silver, aluminium, arsenic, bismuth, sodium, manganese, sodium, selenium, antimony
Etc. one or more impurity.The shape of thick gold can be blocky gold, can also be with bronze.For the rate for obtaining higher oxidation reaction,
It is 100 mesh bronze below that thick gold, which is granularity,.Here, to reach 100 mesh granularity below, high pressurewater cleaning can be used
Mode crushed.It, can be first by blocky gold fusing, then high-pressure water jet powder in the embodiment with blocky gold for thick gold
It is broken to be crushed.
Mixed liquor can use the form of aqueous solution.It can be selected according to actual needs as the dosage of water.
It is envisaged that the reactant that can provide chloride ion can be water soluble chloride, such as alkali metal or alkaline earth gold
Belong to chloride, such as potassium chloride, sodium chloride, magnesium chloride, calcium chloride, can also be hydrochloric acid.
Can provide the reactant of chloride ion source can for alkali or alkaline earth metal hypochlorite, as postassium hypochlorite,
Sodium hypochlorite, magnesium hypochlorite, calcium hypochlorite etc..
The source of above-mentioned acid is only limitted to hydrochloric acid, and the additional amount as acid is to make the dosage of pH 4~7.Such as pH can be
4,4.2,4.5,5,5.5,6,6.5,6.8 or 7 etc..
Oxidation reaction can carry out under stirring conditions, so that reaction is more uniform.It can be used as the mode of stirring
Mechanical stirring, the revolving speed of stirring, which can be used, to be stirred at low speed, such as 100~300rpm.
The temperature of oxidation reaction is advisable with 40~60 DEG C, for example, 40 DEG C, 41 DEG C, 42 DEG C, 45 DEG C, 50 DEG C, 55 DEG C, 58 DEG C,
59 DEG C or 60 DEG C etc..As for the time of oxidation reaction, it is subject to and observes that thick gold is completely dissolved.It is the time property of can refer to 90
~120min, such as 90min, 92min, 95min, 100min, 110min, 115min, 118min or 120min.
It can provide the reactant of chloride ion and can provide the reactant dosage of hypochlorite ion, it can be according to above-mentioned reactional equation
Formula is knowable to obtain its theoretical value.However, in order to obtain the conversion ratio of higher thick gold, with the amount of substance (amount of substance of thick gold
Calculation be that thick golden amount and golden percentage composition product are divided by gold atom amount) be 1 meter, it is possible to provide the reactant of chloride ion
Dosage be preferably 2.5~4, such as 2.5,2.55,2.6,2.8,3,3.5,3.7,3.8,3.9 or 4 etc., preferably 3.5；It can
The dosage for providing the reactant of hypochlorite ion is preferably 2~3, such as 2,2.05,2.1,2.2,2.3,2.4,2.5,2.8,
2.9 or 3 etc., preferably 2.3.
In step (2), reducing agent can enumerate hydrogen peroxide, hydrazine, sulphite, ferrous salt etc., certainly can also be other
Conventional reduction agent.Reducing agent of the present invention is preferably used alone hydrogen peroxide and is restored using hydrazine.I.e. first using double
Oxygen water restores most solubilised state gold, then restores remaining solubilised state gold etc. using hydrazine.
For hydrogen peroxide reduction, reaction equation are as follows: 2HAuCl4+3H2O2=2Au+3O2+8HCl.The temperature of reduction
Degree is advisable with 55~65 DEG C, such as 55 DEG C, 56 DEG C, 58 DEG C, 60 DEG C, 62 DEG C, 63 DEG C, 64 DEG C or 65 DEG C, preferably 60 DEG C etc..In
At a temperature of this, the time of reduction can elect according to actual needs.
The dosage of hydrogen peroxide can obtain its theoretical value according to above-mentioned reaction equation is knowable.However, higher to obtain
Solubilised state gold conversion ratio, the dosage of hydrogen peroxide is preferred with 2~2.5, for example, 2,2.05,2.1,2.2,2.25,2.3,2.4,
2.45 or 2.5, preferably 2.25, it is in terms of 1 by the amount of substance of solubilised state gold.Here, the amount of substance of solubilised state gold is in thick gold
The amount of substance of gold, it is assumed that thick gold has all dissolved.
For using hydrazine to restore, reaction equation are as follows: 4HAuCl4+3N2H4=4Au+3N2+16HCL.Reduction
Temperature be advisable with 50~60 DEG C, such as 50 DEG C, 51 DEG C, 53 DEG C, 55 DEG C, 58 DEG C, 59 DEG C or 60 DEG C, preferably 60 DEG C etc..In
At a temperature of this, the time of reduction can elect according to actual needs.
The dosage of hydrogen peroxide can obtain its theoretical value according to above-mentioned reaction equation is knowable.However, higher to obtain
Solubilised state gold conversion ratio, the dosage of hydrogen peroxide is preferred with 0.85~1.2, for example, 0.85,0.90,0.95,1.0,1.1,
1.15,1.18,1.19 or 1.2, preferably 0.95, the amount of substance to remain solution state gold is in terms of 1.Here, the substance of solubilised state gold
Amount is amount of substance golden in thick gold, it is assumed that thick gold has all dissolved.
It can also include the steps that making the gold salt solution alkalinity after step (1) and before step (2), with one
Aspect removes unreacted hydrochloric acid.In addition, can also be anti-by providing the impurity such as hydroxide ion and aluminium ion in gold salt solution
Hydroxide precipitating should be generated to reach the removal to these impurity elements.
The conventional alkali such as sodium hydroxide, potassium hydroxide can be used in alkali.The dosage of alkali is advisable with pH for 9.5~10.0, example
Such as 9.5,9.6,9.8,10.0.As for the concentration of alkali, by taking alkali is sodium hydroxide as an example, concentration 3mol/L.
After the reduction reaction of step (2), the golden simple substance that contained solubilised state gold is reduced into gold salt solution is to precipitate shape
Formula is precipitated from solution, and the mode that may filter that isolates solid gold.It can be recycled as filtrate (containing chloride ion).Recycling
The form of electrolysis can be used.Filtrate is neutralized to neutrality with 10mol/L alkali (such as sodium hydroxide), electrolysis terminal be NaClO concentration >=
100 grams per liters, NaCl concentration >=100 grams per liters.
The present invention does not address place and is suitable for the prior art.
It is given below specific embodiments of the present invention, but specific embodiment is merely to be described in further detail this explanation,
It is not intended to limit the claims of the present patent application.
Embodiment 1
Step 1: powder processed.Specifically, thick gold bullion is melted, is crushed with high pressure water flow and granularity is made no more than 100 mesh
The thick bronze of leukorrhagia.
Step 2: dissolution.Specifically, putting into above-mentioned thick bronze to by the mixed solution of sodium chloride and sodium hypochlorite, wherein
Amount of substance by thick gold is in terms of 1, and the dosage of sodium chloride is that the dosage of 2.5 hypochlorite ions is 2, then is stirred continuously and is stirred to react
90min, gold are completely dissolved, and it is 4 that reaction process, which is added dropwise hydrochloric acid and maintains pH,.
Step 3: removal of impurities.Specifically, with 3mol/L NaOH adjustment pH value to 9.5, and keep the temperature 30min.
Step 4: filtering.Specially filter out the precipitating (including silver chlorate, hydroxide precipitating etc.) in solution system.
Step 5: hydrogen peroxide restores.Specifically, being to be restored in terms of 1 using 2 hydrogen peroxide by the amount of substance of the solubilised state gold
The gold salt solution handled through step 4 maintains solution temperature to be not less than 60 DEG C, restores most of gold.
Step 6: hydrazine restores.Specifically, residual gold is restored with hydrazine, temperature 50 C is maintained, after the assay was approved mistake
Filter.
Step 7: filtrate send electrolytic cell electrolytic regeneration.Filtrate is neutralized to Neutral Electrolysis terminal with 10mol/L NaOH:
NaClO concentration >=100 grams per liters, NaCl concentration >=100 grams per liters.
Step 8: a little bronze wash water of system mainly contains NaCl, it is concentrated to be incorporated to electrolytic cell.NaCl storage can also be precipitated.
Embodiment 2
Step 1: powder processed.Specifically, thick gold bullion is melted, is crushed with high pressure water flow and granularity is made no more than 100 mesh
Thick bronze below.
Step 2: dissolution.Specifically, putting into above-mentioned thick bronze to by the mixed solution of sodium chloride and sodium hypochlorite, wherein
Amount of substance by thick gold is in terms of 1, and the dosage of sodium chloride is that the dosage of 4 hypochlorite ions is 3, then is stirred continuously and is stirred to react
120min, gold are completely dissolved, and it is 4 that reaction process, which is added dropwise hydrochloric acid and maintains pH,.
Step 3: removal of impurities.Specifically, with 3mol/L NaOH adjustment pH value to 9.5, and keep the temperature 30min.
Step 4: filtering.Specially filter out the precipitating (including silver chlorate, hydroxide precipitating etc.) in solution system.
Step 5: hydrogen peroxide restores.Specifically, being in terms of 1, using 2~2.5 hydrogen peroxide by the amount of substance of the solubilised state gold
The gold salt solution handled through step 4 is restored, maintains solution temperature to be not less than 60 DEG C, restores most of gold.
Step 6: hydrazine restores.Specifically, residual gold is restored with hydrazine, temperature 60 C is maintained, after the assay was approved mistake
Filter.
Step 7: filtrate send electrolytic cell electrolytic regeneration.Filtrate is neutralized to Neutral Electrolysis terminal with 10mol/L NaOH:
NaClO concentration >=100 grams per liters, NaCl concentration >=100 grams per liters.
Step 8: a little bronze wash water of system mainly contains NaCl, it is concentrated to be incorporated to electrolytic cell.NaCl storage can also be precipitated.
Embodiment 3
Step 1: powder processed.Specifically, thick gold bullion is melted, is crushed with high pressure water flow and granularity is made no more than 100 mesh
The thick bronze of leukorrhagia.
Step 2: dissolution.Specifically, putting into above-mentioned thick bronze to by the mixed solution of sodium chloride and sodium hypochlorite, wherein
Amount of substance by thick gold is in terms of 1, and the dosage of sodium chloride is that the dosage of 2.5 hypochlorite ions is 2, then is stirred continuously and is stirred to react
100min, gold are completely dissolved, and it is 7 that reaction process, which is added dropwise hydrochloric acid and maintains pH,.
Step 3: removal of impurities.Specifically, with 3mol/L NaOH adjustment pH value to 10.0, and keep the temperature 30min.
Step 4: filtering.Specially filter out the precipitating (including silver chlorate, hydroxide precipitating etc.) in solution system.
Step 5: hydrogen peroxide restores.Specifically, being in terms of 1, also using 2.5 hydrogen peroxide by the amount of substance of the solubilised state gold
The gold salt solution that original is handled through step 4 maintains solution temperature to be not less than 60 DEG C, restores most of gold.
Step 6: hydrazine restores.Specifically, residual gold is restored with hydrazine, temperature 60 C is maintained, after the assay was approved mistake
Filter.
Step 7: filtrate send electrolytic cell electrolytic regeneration.Filtrate is neutralized to Neutral Electrolysis terminal with 10mol/L NaOH:
NaClO concentration >=100 grams per liters, NaCl concentration >=100 grams per liters.
Step 8: a little bronze wash water of system mainly contains NaCl, it is concentrated to be incorporated to electrolytic cell.NaCl storage can also be precipitated.
Embodiment 4
Step 1: powder processed.Specifically, thick gold bullion is melted, is crushed with high pressure water flow and granularity is made no more than 100 mesh
The thick bronze of leukorrhagia.
Step 2: dissolution.Specifically, putting into above-mentioned thick bronze to by the mixed solution of sodium chloride and sodium hypochlorite, wherein
Amount of substance by thick gold is in terms of 1, and the dosage of sodium chloride is that the dosage of 3.7 hypochlorite ions is 2.5, then is stirred continuously and is stirred to react
100min, gold are completely dissolved, and it is 5.5 that reaction process, which is added dropwise hydrochloric acid and maintains pH,.
Step 3: removal of impurities.Specifically, with 3mol/L NaOH adjustment pH value to 9.8, and keep the temperature 30min.
Step 4: filtering.Specially filter out the precipitating (including silver chlorate, hydroxide precipitating etc.) in solution system.
Step 5: hydrogen peroxide restores.Specifically, being in terms of 1, also using 2.25 hydrogen peroxide by the amount of substance of the solubilised state gold
The gold salt solution that original is handled through step 4 maintains solution temperature to be not less than 60 DEG C, restores most of gold.
Step 6: hydrazine restores.Specifically, residual gold is restored with hydrazine, 55 DEG C of temperature are maintained, after the assay was approved mistake
Filter.
Step 7: filtrate send electrolytic cell electrolytic regeneration.Filtrate is neutralized to Neutral Electrolysis terminal with 10mol/L NaOH:
NaClO concentration >=100 grams per liters, NaCl concentration >=100 grams per liters.
Step 8: a little bronze wash water of system mainly contains NaCl, it is concentrated to be incorporated to electrolytic cell.NaCl storage can also be precipitated.
Embodiment 5
Step 1: powder processed.Specifically, thick gold bullion is melted, is crushed with high pressure water flow and granularity is made no more than 100 mesh
The thick bronze of leukorrhagia.
Step 2: dissolution.Specifically, putting into above-mentioned thick bronze to by the mixed solution of sodium chloride and sodium hypochlorite, wherein
Amount of substance by thick gold is in terms of 1, and the dosage of sodium chloride is that the dosage of 3.5 hypochlorite ions is 2.3, then is stirred continuously and is stirred to react
100min, gold are completely dissolved, and it is 4~7 that reaction process, which is added dropwise hydrochloric acid and maintains pH,.
Step 3: removal of impurities.Specifically, with 3mol/L NaOH adjustment pH value to 9.8, and keep the temperature 30min.
Step 4: filtering.Specially filter out the precipitating (including silver chlorate, hydroxide precipitating etc.) in solution system.
Step 5: hydrogen peroxide restores.Specifically, being in terms of 1, using 2~2.5 hydrogen peroxide by the amount of substance of the solubilised state gold
The gold salt solution handled through step 4 is restored, maintains solution temperature to be not less than 60 DEG C, restores most of gold.
Step 6: hydrazine restores.Specifically, residual gold is restored with hydrazine, 55 DEG C of temperature are maintained, after the assay was approved mistake
Filter.
Step 7: filtrate send electrolytic cell electrolytic regeneration.Filtrate is neutralized to Neutral Electrolysis terminal with 10mol/L NaOH:
NaClO concentration >=100 grams per liters, NaCl concentration >=100 grams per liters.
Step 8: a little bronze wash water of system mainly contains NaCl, it is concentrated to be incorporated to electrolytic cell.NaCl storage can also be precipitated.
After tested, the metal gold content purified through method of purification of the present invention is greater than 99.99%, and impurity content is as follows
Table:
| Impurity element | Content (%) |
| Ag | 0.00017 |
| Al | 0.00012 |
| As | 0.00058 |
| Bi | ﹤ 0.00002 |
| Cd | ﹤ 0.00002 |
| Cr | ﹤ 0.00011 |
| Cu | ﹤ 0.00004 |
| Fe | 0.00079 |
| Ir | 0.00002 |
| Mg | 0.00005 |
| Mn | ﹤ 0.00002 |
| Na | ﹤ 0.00006 |
| Ni | 0.00011 |
| Pb | 0.00004 |
| Pd | 0.00004 |
| Pt | 0.00011 |
| Rh | ﹤ 0.00002 |
| Sb | 0.00004 |
| Se | ﹤ 0.00006 |
| Sn | ﹤ 0.00012 |
| Te | ﹤ 0.00002 |
| Ti | ﹤ 0.00002 |
| Zn | 0.00006 |
The numberical range of each technological parameter as involved in the present invention can not all embody in the above-described embodiments,
As long as but those skilled in the art's envisioned any numerical value fallen into the above-mentioned numberical range completely can be implemented this
Invention also includes any combination of occurrence in several numberical ranges certainly.Herein, due to space considerations, be omitted to
Out in certain one or more numberical range occurrence embodiment, this disclosure for being not to be construed as technical solution of the present invention do not fill
Point.
The Applicant declares that the present invention is explained by the above embodiments detailed process equipment and process flow of the invention,
But the present invention is not limited to the above detailed process equipment and process flow, that is, it is above-mentioned detailed not mean that the present invention must rely on
Process equipment and process flow could be implemented.It should be clear to those skilled in the art, any improvement in the present invention,
Addition, concrete mode selection of equivalence replacement and auxiliary element to each raw material of product of the present invention etc., fall in protection of the invention
In range.
Claims (7)
1. a kind of method for gold of purifying metals, which comprises the following steps:
(1) thick gold bullion is melted, is crushed with high pressure water flow and 100 mesh of granularity thick bronze below is made；
(2) make the thick bronze that oxidation reaction occur with the mixed solution of sodium chloride and sodium hypochlorite in acid condition, formed
Gold salt solution containing solubilised state gold, and make using hydrochloric acid the pH 4~7 of the acidity；
(3) make the solubilised state gold that reduction reaction occur with reducing agent, obtain gold, the reduction reaction successively use hydrogen peroxide and
Hydrazine is restored；
(4) it is filtered after the reduction reaction and send filtrate to electrolytic cell electrolytic regeneration, wherein the filtrate uses 10mol/L
NaOH is neutralized to neutrality, and the terminal of the electrolysis: NaClO concentration >=100 grams per liters, NaCl concentration >=100 grams per liters.
2. the method according to claim 1, wherein the temperature of oxidation reaction described in step (2) is 40~60
DEG C, the time of oxidation reaction is 90~120min.
3. the method according to claim 1, wherein in step (2), the amount by the substance of thick gold is in terms of 1, chlorine from
The dosage of son is 2.5~4, and the dosage of hypochlorite ion is 2~3.
4. the method according to claim 1, wherein the dosage for being restored used hydrogen peroxide by hydrogen peroxide
It is 2~2.5, is in terms of 1 by the amount of the substance of the solubilised state gold.
5. the method according to claim 1, wherein the temperature restored by hydrogen peroxide is 55~65 DEG C.
6. the method according to claim 1, wherein the temperature restored by hydrazine is 50~60 DEG C.
7. the method according to claim 1, wherein further including after the step (2) and before step (3)
Make the step of the gold salt solution alkalinity, the pH of the alkalinity is 9.5~10.0.
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