CN106119567A - A kind of method of gold of purifying metals - Google Patents
A kind of method of gold of purifying metals Download PDFInfo
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- CN106119567A CN106119567A CN201610808559.6A CN201610808559A CN106119567A CN 106119567 A CN106119567 A CN 106119567A CN 201610808559 A CN201610808559 A CN 201610808559A CN 106119567 A CN106119567 A CN 106119567A
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- 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
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Abstract
A kind of method that the invention discloses gold of purifying metals.The present invention purifies metals the method for gold, first thick gold is dissolved in mixed liquor containing chloride ion and hypochlorite ion in acid condition, then is reduced by lysigenous the dissolved gold reducing agent.The product of this dissolving, except the dissolved gold and water, produces without other any waste gas.It addition, the purity of the purified Aurum metallicum of the present invention is not less than 99.99%.
Description
Technical field
The present invention relates to the technical field of metalworking, in particular to a kind of method of gold of purifying metals.
Background technology
The chemical elemental symbol of gold is Au, is a kind of soft, flavous, erosion-resisting noble metal.Gold is jewellery industry, electricity
Sub-industry, modern communication, the important materials of space flight and aviation Ye Deng department.
At present, the method for purification to Aurum metallicum mainly has chloroazotic acid method, Boliden technique (chloridising), extraction, electrolysis
Four kinds.Chloroazotic acid method refers to thick gold is dissolved in chloroazotic acid (hydrochloric acid and nitric acid by thing mass ratio is 4:1 mix), waits to drive away
After nitric acid, restore.Boliden technique refers to be dissolved in hydrochloric acid and chlorine thick gold, restores.Extraction is by molten for thick gold
Solution is in chloroazotic acid, then extracts back extraction, finally reduces.Electrolysis refers to be dissolved in hydrochloric acid thick gold, then electroreduction.
In above prior art, it is big generally to there is waste gas wastewater flow rate in the method for gold of purifying metals, and the pollution to environment is bigger.
It addition, the purity purified is the most limited.
Summary of the invention
In view of this, one aspect of the present invention is a kind of method providing gold of purifying metals, the method more environmental protection, purifies
Purity higher.
A kind of method of gold of purifying metals, comprises the following steps:
(1) make thick gold in acid condition with the mixed liquor generation oxidation reaction containing chloride ion and hypochlorite ion, shape
Become the gold salt solution containing the dissolved gold；
(2) make described the dissolved gold with reducing agent generation reduction reaction, obtain purifying gold.
Further, acid described in step (1) pH is 4～7.
Further, described in step (1), the temperature of oxidation reaction is 40～60 DEG C, the time of oxidation reaction be 90～
120min。
Further, in step (1), being in terms of 1 by the material amount of thick gold, the consumption of chloride ion is 2.5～4, hypochlorous acid from
The consumption of son is 2～3.
Further, reduction reaction described in step (2) includes being reduced by hydrogen peroxide and being reduced by hydrazine afterwards.
Further, described to be reduced the consumption of used hydrogen peroxide by hydrogen peroxide be 2～2.5, with described the dissolved gold
Material amount be 1 meter.
Further, the described temperature reduced by hydrogen peroxide is 55～65 DEG C.
Further, the described temperature reduced by hydrazine is 50～60 DEG C.
Further, the step making described gold salt solution be alkalescence is also included after described step (1) and before step (2)
Suddenly, the pH of described alkalescence is 9.5～10.0.
Further, described thick gold be granularity be the bronze of below 100 mesh.
The present invention purify metals gold method, first thick gold is dissolved in acid condition containing chloride ion and hypochlorous acid
The mixed liquor of ion, more lysigenous the dissolved gold reducing agent is reduced.The product of this dissolving except the dissolved gold and water,
Produce without other any waste gas.It addition, the purity of the purified Aurum metallicum of the present invention is not less than 99.99%.
Detailed description of the invention
For the ease of understanding the present invention, close embodiment below and further illustrate technical scheme.
As used herein, term:
" mass parts " refers to represent the basic measurement unit of the mass ratio relation of multiple component, and 1 part can represent arbitrary list
Position quality, as being expressed as 1g, it is possible to represents 2.689g etc..If we say that the mass parts of component A is a part, the matter of B component
Amount part is b part, then it represents that the quality of component A and mass ratio a:b of B component.Or ground, represents that the quality of component A is aK, B
The quality of component is bK (K is Arbitrary Digit, represents multiplying factor).Can not misread, unlike mass fraction, all groups
The mass parts sum divided is not limited to the restriction of 100 parts.
" one ", " a kind of " and " described " are used interchangeably and refer to one or more.
"and/or" for represent the one or both of illustrated situation all it may happen that, such as, A and/or B includes (A
And B) and (A or B)；
It addition, all numerical value that the scope stated by end points herein is comprised in the range of including this (such as, 1 to 10 bag
Include 1.4,1.9,2.33,5.75,9.98 etc.).
It addition, the statement of " at least one " herein include one and above all numbers (such as, at least 2, at least
4, at least 6, at least 8, at least 10, at least 25, at least 50, at least 100 etc.).
The method of the gold of purifying metals of the present invention, comprises the following steps:
(1) make thick gold in acid condition with the mixed liquor generation oxidation reaction containing chloride ion and hypochlorite ion, shape
Become the gold salt solution containing the dissolved gold；
(2) make described the dissolved gold with reducing agent generation reduction reaction, obtain purifying gold.
In above-mentioned steps (1), the equation of oxidation reaction is 5Cl-+3ClO-+8H++ 2Au=2HAuCl4+3H2O。
Above-mentioned term " the dissolved gold " refers to gold element chemical species in dissolving in water, such as, can include simple metal
Ion, hydrated metal ion, hydroxo complex, complex ions.Equation based on above-mentioned oxidation reaction, the dissolved here
Gold predominantly [AuCl4]-。
Above-mentioned thick gold can be the gold that gold content is not less than 90wt%, and containing silver, aluminum, arsenic, bismuth, sodium, manganese, sodium, selenium, antimony
Deng one or more impurity.The shape of thick gold can be block gold, it is also possible to bronze.For obtaining the speed of higher oxidation reaction,
Thick gold is bronze that granularity is below 100 mesh.Here, for reaching the granularity of below 100 mesh, high pressurewater cleaning can be used
Mode pulverize.With block golden in the embodiment of thick gold, can first block gold be melted, then high-pressure water jet powder
Broken pulverize.
Mixed liquor can be to use the form of aqueous solution.Consumption as water can select according to actual needs.
It is envisaged that can provide the reactant of 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 etc., it is also possible to for hydrochloric acid.
The source that can provide the reactant of chloride ion can be alkali metal or alkaline earth hypochlorite salts, as postassium hypochlorite,
Sodium hypochlorite, magnesium hypochlorite, calcium hypochlorite etc..
The source of above-mentioned acid is only limitted to hydrochloric acid, and the addition as acid is the consumption making pH be 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 be carried out under conditions of stirring, so that reaction is more uniformly distributed.Mode as stirring can use
Mechanical agitation, the rotating speed of stirring can use stirring at low speed, such as 100～300rpm.
The temperature of oxidation reaction is advisable with 40～60 DEG C, such as 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 as the criterion observing that thick gold is completely dissolved.It is referring to property of time 90
～120min, such as 90min, 92min, 95min, 100min, 110min, 115min, 118min or 120min etc..
The reactant of chloride ion can be provided and the reactant consumption of hypochlorite ion can be provided, can be according to above-mentioned reactional equation
Formula can be known to obtain its theoretical value.But, in order to obtain the conversion ratio of higher thick gold, with material amount (the material amount of thick gold
Calculation be, thick golden amount with gold percentage composition product divided by gold atom amount) be 1 meter, it is possible to provide the reactant of chloride ion
Consumption 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；Can
To there is provided the consumption of reactant of hypochlorite ion be 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 list hydrogen peroxide, hydrazine, sulphite, ferrous salt etc., can be the most also other
Conventional reduction agent.Reducing agent of the present invention is preferably used alone hydrogen peroxide and uses hydrazine to reduce.I.e. first by double
Oxygen water reduce most the dissolved gold, then use hydrazine reduction residual the dissolved gold etc..
For hydrogen peroxide reduces, its reaction equation is: 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 consumption of hydrogen peroxide, can know according to above-mentioned reaction equation and obtain its theoretical value.But, higher for obtaining
The dissolved gold conversion ratio, the consumption of hydrogen peroxide is preferred with 2～2.5, such as 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 material amount of the dissolved gold.Here, the material amount of the dissolved gold is in thick gold
The material amount of gold, it is assumed that thick gold has the most all dissolved.
For using hydrazine reduction, its reaction equation is: 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 consumption of hydrogen peroxide, can know according to above-mentioned reaction equation and obtain its theoretical value.But, higher for obtaining
The dissolved gold conversion ratio, the consumption of hydrogen peroxide is preferred with 0.85～1.2, such as 0.85,0.90,0.95,1.0,1.1,
1.15,1.18,1.19 or 1.2, preferably 0.95, the material amount solving state gold by residual is in terms of 1.Here, the material of the dissolved gold
Amount is in thick gold the material amount of gold, it is assumed that thick gold has the most all dissolved.
The step making described gold salt solution be alkalescence can also be included, with one after step (1) and before step (2)
Aspect removes unreacted hydrochloric acid.Additionally, it is anti-also by providing the impurity such as hydroxide ion and the aluminium ion in gold salt solution
Hydroxide should be generated precipitate to reach the removal to these impurity elements.
Alkali can use the such as conventional alkaline such as sodium hydroxide, potassium hydroxide.The consumption of alkali is 9.5～10.0 to be advisable with pH, example
Such as 9.5,9.6,9.8,10.0 etc..As for the concentration of alkali, as a example by alkali is as sodium hydroxide, its concentration is 3mol/L.
After the reduction reaction of step (2), the golden simple substance that in gold salt solution, contained the dissolved gold is reduced into is to precipitate shape
Formula separates out from solution, and filtrable mode isolates solid gold.Can be recycled as filtrate (containing chloride ion).Reclaim
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 liter.
The present invention does not addresses part and is applicable to prior art.
The specific embodiment of the present invention is given below, but specific embodiment is merely to be described in further detail this explanation,
It is not limiting as the claims of the present patent application.
Embodiment 1
Step one, powder process.Specifically, thick gold bullion is melted, pulverized with High-Pressure Water and made granularity less than 100 mesh
The thick bronze of leukorrhagia.
Step 2, dissolving.Specifically, to by sodium chloride and sodium hypochlorite mixed solution put into above-mentioned thick bronze, wherein,
Be in terms of 1 by the material amount of thick gold, the consumption of sodium chloride be the consumption of 2.5 hypochlorite ions be 2, then be stirred continuously stirring reaction
90min, gold is completely dissolved, and course of reaction dropping hydrochloric acid maintains pH to be 4.
Step 3, remove impurity.Specifically, with 3mol/L NaOH adjustment pH value to 9.5, and it is incubated 30min.
Step 4, filtration.Specially filter out the precipitation in solution system (including silver chloride, hydroxide precipitation etc.).
Step 5, hydrogen peroxide reduce.Specifically, the material amount by described the dissolved gold is in terms of 1, use 2 hydrogen peroxide reduction
Through the gold salt solution that step 4 processes, maintain solution temperature to be not less than 60 DEG C, restore major part gold.
Step 6, hydrazine reduce.Specifically, reduced by residual gold hydrazine, maintain temperature 50 C, after the assay was approved mistake
Filter.
Step 7, filtrate send electrolysis bath electrolytic regeneration.Filtrate is neutralized to Neutral Electrolysis terminal with 10mol/L NaOH:
NaClO concentration >=100 grams per liter, NaCl concentration >=100 grams per liter.
Step 8, system a little bronze wash water, mainly containing NaCl, concentrated is incorporated to electrolysis bath.Also can separate out NaCl to store.
Embodiment 2
Step one, powder process.Specifically, thick gold bullion is melted, pulverized with High-Pressure Water and made granularity less than 100 mesh
Following thick bronze.
Step 2, dissolving.Specifically, to by sodium chloride and sodium hypochlorite mixed solution put into above-mentioned thick bronze, wherein,
Be in terms of 1 by the material amount of thick gold, the consumption of sodium chloride be the consumption of 4 hypochlorite ions be 3, then be stirred continuously stirring reaction
120min, gold is completely dissolved, and course of reaction dropping hydrochloric acid maintains pH to be 4.
Step 3, remove impurity.Specifically, with 3mol/L NaOH adjustment pH value to 9.5, and it is incubated 30min.
Step 4, filtration.Specially filter out the precipitation in solution system (including silver chloride, hydroxide precipitation etc.).
Step 5, hydrogen peroxide reduce.Specifically, the material amount by described the dissolved gold is in terms of 1, use 2～2.5 hydrogen peroxide
The gold salt solution that reduction processes through step 4, maintains solution temperature to be not less than 60 DEG C, restores major part gold.
Step 6, hydrazine reduce.Specifically, reduced by residual gold hydrazine, maintain temperature 60 C, after the assay was approved mistake
Filter.
Step 7, filtrate send electrolysis bath electrolytic regeneration.Filtrate is neutralized to Neutral Electrolysis terminal with 10mol/L NaOH:
NaClO concentration >=100 grams per liter, NaCl concentration >=100 grams per liter.
Step 8, system a little bronze wash water, mainly containing NaCl, concentrated is incorporated to electrolysis bath.Also can separate out NaCl to store.
Embodiment 3
Step one, powder process.Specifically, thick gold bullion is melted, pulverized with High-Pressure Water and made granularity less than 100 mesh
The thick bronze of leukorrhagia.
Step 2, dissolving.Specifically, to by sodium chloride and sodium hypochlorite mixed solution put into above-mentioned thick bronze, wherein,
Be in terms of 1 by the material amount of thick gold, the consumption of sodium chloride be the consumption of 2.5 hypochlorite ions be 2, then be stirred continuously stirring reaction
100min, gold is completely dissolved, and course of reaction dropping hydrochloric acid maintains pH to be 7.
Step 3, remove impurity.Specifically, with 3mol/L NaOH adjustment pH value to 10.0, and it is incubated 30min.
Step 4, filtration.Specially filter out the precipitation in solution system (including silver chloride, hydroxide precipitation etc.).
Step 5, hydrogen peroxide reduce.Specifically, the material amount by described the dissolved gold is in terms of 1, use 2.5 hydrogen peroxide also
The former gold salt solution processed through step 4, maintains solution temperature to be not less than 60 DEG C, restores major part gold.
Step 6, hydrazine reduce.Specifically, reduced by residual gold hydrazine, maintain temperature 60 C, after the assay was approved mistake
Filter.
Step 7, filtrate send electrolysis bath electrolytic regeneration.Filtrate is neutralized to Neutral Electrolysis terminal with 10mol/L NaOH:
NaClO concentration >=100 grams per liter, NaCl concentration >=100 grams per liter.
Step 8, system a little bronze wash water, mainly containing NaCl, concentrated is incorporated to electrolysis bath.Also can separate out NaCl to store.
Embodiment 4
Step one, powder process.Specifically, thick gold bullion is melted, pulverized with High-Pressure Water and made granularity less than 100 mesh
The thick bronze of leukorrhagia.
Step 2, dissolving.Specifically, to by sodium chloride and sodium hypochlorite mixed solution put into above-mentioned thick bronze, wherein,
Be in terms of 1 by the material amount of thick gold, the consumption of sodium chloride be the consumption of 3.7 hypochlorite ions be 2.5, then be stirred continuously stirring reaction
100min, gold is completely dissolved, and course of reaction dropping hydrochloric acid maintains pH to be 5.5.
Step 3, remove impurity.Specifically, with 3mol/L NaOH adjustment pH value to 9.8, and it is incubated 30min.
Step 4, filtration.Specially filter out the precipitation in solution system (including silver chloride, hydroxide precipitation etc.).
Step 5, hydrogen peroxide reduce.Specifically, the material amount by described the dissolved gold is in terms of 1, use 2.25 hydrogen peroxide also
The former gold salt solution processed through step 4, maintains solution temperature to be not less than 60 DEG C, restores major part gold.
Step 6, hydrazine reduce.Specifically, reduced by residual gold hydrazine, maintain temperature 55 DEG C, mistake after the assay was approved
Filter.
Step 7, filtrate send electrolysis bath electrolytic regeneration.Filtrate is neutralized to Neutral Electrolysis terminal with 10mol/L NaOH:
NaClO concentration >=100 grams per liter, NaCl concentration >=100 grams per liter.
Step 8, system a little bronze wash water, mainly containing NaCl, concentrated is incorporated to electrolysis bath.Also can separate out NaCl to store.
Embodiment 5
Step one, powder process.Specifically, thick gold bullion is melted, pulverized with High-Pressure Water and made granularity less than 100 mesh
The thick bronze of leukorrhagia.
Step 2, dissolving.Specifically, to by sodium chloride and sodium hypochlorite mixed solution put into above-mentioned thick bronze, wherein,
Be in terms of 1 by the material amount of thick gold, the consumption of sodium chloride be the consumption of 3.5 hypochlorite ions be 2.3, then be stirred continuously stirring reaction
100min, gold is completely dissolved, and course of reaction dropping hydrochloric acid maintains pH to be 4～7.
Step 3, remove impurity.Specifically, with 3mol/L NaOH adjustment pH value to 9.8, and it is incubated 30min.
Step 4, filtration.Specially filter out the precipitation in solution system (including silver chloride, hydroxide precipitation etc.).
Step 5, hydrogen peroxide reduce.Specifically, the material amount by described the dissolved gold is in terms of 1, use 2～2.5 hydrogen peroxide
The gold salt solution that reduction processes through step 4, maintains solution temperature to be not less than 60 DEG C, restores major part gold.
Step 6, hydrazine reduce.Specifically, reduced by residual gold hydrazine, maintain temperature 55 DEG C, mistake after the assay was approved
Filter.
Step 7, filtrate send electrolysis bath electrolytic regeneration.Filtrate is neutralized to Neutral Electrolysis terminal with 10mol/L NaOH:
NaClO concentration >=100 grams per liter, NaCl concentration >=100 grams per liter.
Step 8, system a little bronze wash water, mainly containing NaCl, concentrated is incorporated to electrolysis bath.Also can separate out NaCl to store.
After tested, the Aurum metallicum content purified through method of purification of the present invention is more than 99.99%, and its 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 |
Owing to the numerical range of each technological parameter involved in the present invention can not all embody in the above-described embodiments,
As long as but the most envisioned any numerical value fallen in this numerical range above-mentioned of those skilled in the art all can implement this
Invention, the most also includes the combination in any of occurrence in the range of some numerical value.Herein, for the consideration of length, eliminate to
Going out the embodiment of occurrence in certain one or more numerical range, this disclosure being not to be construed as technical scheme is not filled
Point.
Applicant states, the present invention illustrates detailed process equipment and the technological process of the present invention by above-described embodiment,
But the invention is not limited in above-mentioned detailed process equipment and technological process, i.e. do not mean that the present invention have to rely on above-mentioned in detail
Process equipment and technological process could be implemented.Person of ordinary skill in the field it will be clearly understood that any improvement in the present invention,
The equivalence of raw material each to product of the present invention is replaced and the interpolation of auxiliary element, concrete mode selection etc., falls in the protection of the present invention
In the range of.
Claims (10)
1. the method for a gold of purifying metals, it is characterised in that comprise the following steps:
(1) making thick gold in acid condition with the mixed liquor generation oxidation reaction containing chloride ion and hypochlorite ion, formation contains
There is the gold salt solution of the dissolved gold；
(2) make described the dissolved gold with reducing agent generation reduction reaction, obtain gold.
Method the most according to claim 1, it is characterised in that pH acid described in step (1) is 4～7.
Method the most according to claim 1, it is characterised in that described in step (1), the temperature of oxidation reaction is 40～60
DEG C, the time of oxidation reaction is 90～120min.
Method the most according to claim 1, it is characterised in that in step (1), is in terms of 1 by the material amount of thick gold, chloride ion
Consumption be 2.5～4, the consumption of hypochlorite ion is 2～3.
Method the most according to claim 1, it is characterised in that described in step (2), reduction reaction includes by hydrogen peroxide also
Former and being reduced by hydrazine afterwards.
Method the most according to claim 5, it is characterised in that the described consumption being reduced used hydrogen peroxide by hydrogen peroxide
It is 2～2.5, is in terms of 1 by the material amount of described the dissolved gold.
Method the most according to claim 5, it is characterised in that the described temperature reduced by hydrogen peroxide is 55～65 DEG C.
Method the most according to claim 5, it is characterised in that the described temperature reduced by hydrazine is 50～60 DEG C.
Method the most according to claim 5, it is characterised in that also include after described step (1) and before step (2)
The step making described gold salt solution be alkalescence, the pH of described alkalescence is 9.5～10.0.
Method the most according to claim 5, it is characterised in that described thick gold be granularity be the bronze of below 100 mesh.
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| CN107354308A (en) * | 2017-07-28 | 2017-11-17 | 许良秋 | A kind of method for gold of purifying metals |
| TWI626217B (en) * | 2017-01-24 | 2018-06-11 | 健鼎科技股份有限公司 | Method Of Making Inorganic Gold Compound |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| TWI626217B (en) * | 2017-01-24 | 2018-06-11 | 健鼎科技股份有限公司 | Method Of Making Inorganic Gold Compound |
| US10046976B1 (en) | 2017-01-25 | 2018-08-14 | Tripod Technology Corporation | Method of making inorganic gold compound |
| CN107354308A (en) * | 2017-07-28 | 2017-11-17 | 许良秋 | A kind of method for gold of purifying metals |
| CN107354308B (en) * | 2017-07-28 | 2019-09-24 | 许良秋 | A method of gold of purifying metals |
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