CN109055715A - A kind of gold refining acid waste water multielement composite recovery process - Google Patents
A kind of gold refining acid waste water multielement composite recovery process Download PDFInfo
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Abstract
A kind of gold refining acid waste water multielement composite recovery process includes the following steps: that gold refining acid waste water feeding carbon adsorption slot is carried out circulation carbon adsorption until gold grade obtains gold loaded carbon, gold loaded carbon sends to parsing lower than 0.2mg/L in liquid by (1)；(2) liquid of the gold grade lower than 0.2mg/L be sequentially sent to No. 1, No. 2, metal ion displacement reaction is carried out in No. 3 storage tanks, drained into outside the supernatant in No. 3 storage tanks between water treatment vehicle and carry out water process；For sediment in No. 3 storage tanks in 600 ± 10 DEG C of 3.5 ~ 4.5h of drying, mercury vapour is cooled into liquid mercury, and borax is added into the slag after drying and soda ash is refined greatly；(3) the big refining slag after big refining sends to ball milling, ore matching, and the alloy after big refining pours into anode, is electrolysed, cathode output fine copper after electrolysis, and anode generates the earth of positive pole；The earth of positive pole handles to obtain gold and silver and waste residue through superchlorination, and waste residue returns to big refining.
Description
Technical field
The invention belongs to field of hydrometallurgy, and in particular to a kind of gold refining acid waste water multielement composite recovery process.
Background technique
It is lower and contain heavy metal that non-ferrous metal industry can generate pH during metal mine exploitation, ore dressing, smelting etc.
Acid waste water can corrode the infrastructure such as sewer pipe, water conservancy project structure such as without processing, heavy metal therein can be serious
Polluted surface water, underground water or soil influence the growth and breeding of animals and plants and the growth of crops, strong to environmental quality and human body
The huge harm of Kang Zaocheng.Mainly there are three classes for the common processing method of acid waste water containing heavy metal:
(1) heavy metal ions in wastewater is removed by chemical reaction.Including chemical precipitation, redox, a macromolecule huge sum of money
Belong to trapping agent method etc.；
(2) under the premise of not changing Chemical Forms of Heavy Metals, the effects of being adsorbed, be concentrated and being separated to it, is from water body
It removes.Including the methods of absorption, ion exchange, UF membrane；
(3) weight in the effects of biology such as algae, fungi and bacterium passes through bioflocculation, biological adsorption, plant absorption removal waste water
Metal.
Chemical precipitation method is current development time longest, a kind of removal weight that technique is more mature, most effective and application range is most wide
The method of metal.
During gold refining, the acid waste water situation of our company generation:
| Essential element | Au(mg/L) | Ag(mg/L) | Cu(g/L) | Hg(mg/L) |
| Quantity | 0.2~3.0 | 10~30 | 0.5~2.5 | 0.2~2.0 |
Monthly outlet about 4~6 times of gold refining acid waste water, each outlet about 40~60m3, outdoor carbon adsorption trough is drained into outside to carry out
After circulation absorption, after liquid Gold grade is up to standard, it is neutralized between outlet water treatment vehicle.This processing is not only time-consuming, more
It is important that only recycled to gold, in waste water heavy metal Hg and noble silver do not recycled effectively.
Summary of the invention
The purpose of the present invention is to provide a kind of gold refining acid waste water multielement composite recovery process.This method is effective
The gold, silver recycled in acid waste water, copper and mercury.
Based on above-mentioned purpose, the present invention is adopted the following technical scheme that:
A kind of gold refining acid waste water multielement composite recovery process, includes the following steps:
(1) gold refining acid waste water feeding carbon adsorption slot is subjected to circulation carbon adsorption until in liquid gold grade lower than 0.2mg/L,
Gold loaded carbon is obtained simultaneously, gold loaded carbon sends to parsing；
(2) liquid of the gold grade lower than 0.2mg/L is sequentially sent to No. 1, No. 2, No. 3 storage tank (two with the flow velocity of 1.0 ~ 2.0m/s
Storage tank is just enough, and 3 storage tanks are manageable more thoroughly) in reacted, water process is drained into outside the supernatant in No. 3 storage tanks
Workshop carries out water process；For sediment in No. 3 storage tanks in 600 ± 10 DEG C of 3.5 ~ 4.5h of drying, mercury vapour is cooled into liquid mercury,
Borax is added into the slag after drying and soda ash is refined greatly；
(3) the big refining slag after big refining sends to ball milling, ore matching, and the alloy after big refining pours into anode, is Cu in electrolyte composition2+
35~40g/L, H+190~230g/L, SO4 2-225~270g/L, current density are 150~190A/m2, tank voltage be 1.8~
It is carried out under 2.2V electrolysis 18 ~ 22 hours, cathode output fine copper after electrolysis, anode generates the earth of positive pole；The earth of positive pole is handled through superchlorination
Gold and silver and waste residue are obtained, waste residue returns to big refining.
Further, the volume of No. 1, No. 2, No. 3 storage tank is 80m3, processing time of the liquid in each storage tank
It is 1.5 ~ 2 hours, No. 1 storage tank can about displace 65% of contained total metal mass in liquid, and No. 2 storage tanks can about displace liquid
The 25% of contained total metal mass in body, No. 3 storage tanks about can in replacement fluid contained total metal mass 5%.
Further, the sediment of previous No. 2 storage tanks is added into No. 1 storage tank, previous No. 3 storages are added into No. 2 storage tanks
Iron powder and Na are added into No. 3 storage tanks for the sediment of tank2S(iron powder is used for and displacement reaction occurs for some metal ions to set
Swap out a part of metal, gold, silver, copper and mercury in main replacement fluid, and Na is added2The purpose of S refers to S2-It is raw with a part of metal
Sulphidisation precipitating, such as becomes HgS for Hg.).
Preferably, 60m is handled in step (1)3Previous No. 2 storage tanks need to be added when gold refining acid waste water into No. 1 storage tank
10 ~ 15kg of sediment, 20 ~ 25kg of sediment of previous No. 3 storage tanks is added into No. 2 storage tanks, iron powder is added into No. 3 storage tanks
20 ~ 25kg and Na2S10 ~ 15kg, such as 2, No. 3 storage tank sediments are insufficient, can be replaced with iron powder and vulcanized sodium, but stored up to No. 1
The quality of addition iron powder and vulcanized sodium is the half of No. 3 storage tank dosages in tank and No. 2 storage tanks.Iron powder market purchase, it is desirable that -200
Mesh accounts for 75wt% or more (i.e. partial size 0.074mm is below accounts for 75% or more).
Further, detailed process is as follows for the big refining: according to slag, borax, the soda ash mass ratio 1:0.3 after drying:
The addition of 0.2(borax and soda ash improves molten slag mobility for reducing the fusing point of slag in smelting process) ingredient, intermediate frequency furnace is added
In 1800 ~ 1900 DEG C of progress meltings, obtain melting liquid, melting liquid poured into crouching tank, take out what crouching tank lower part was formed after cooling
Alloy is put into intermediate frequency furnace melts again by alloy, and metal liquid pours into the anode dimension needed when cathode copper after fusing.
Further, the process of the chlorination processing is as follows:
A. acidleach: being added hydrochloric acid according to volume ratio 2:1 into reaction kettle and water obtain dilute hydrochloric acid solution, add the earth of positive pole, sun
The quality of pole mud and the mass ratio of dilute hydrochloric acid solution are 1 ︰ (2.5 ~ 4.5), and 85 ~ 95 DEG C are leached 2.5 ~ 3.5 hours, slag-liquid separation；
B. chlorination: hydrochloric acid is added according to volume ratio 2:1 into reaction kettle and water obtains dilute hydrochloric acid solution, is heated under stirring
The slag charge that a step is isolated is added at 80 DEG C, keeps at 80 DEG C, sodium chlorate is added, sodium chlorate dosage is golden amount in the earth of positive pole
1.5-2.5 times, 90-95 DEG C is stirred to react 2 ~ 4 hours, end of reaction, stand 15-30 minute, start slag-liquid separation, liquid oneself
It flows into reduction reaction kettle, slag investment displacement kettle adds iron replacement to go out silver；
C. it restores: being warming up to 85 DEG C or more addition sodium sulfites in agitating and heating from the liquid flowed into reduction reaction kettle and carry out
Reduction, the additional amount of sodium sulfite are 1.5-2.5 times of golden amount in liquid, when in supernatant gold content in 3mg/L hereinafter, being
Reaction can be terminated, is separated by solid-liquid separation, liquid sends to charcoal absorption, and solid is bronze, is added in intermediate frequency furnace after drying and melts out ingot.
Further, the concentration of the hydrochloric acid is 29 ~ 35wt%.
The present invention carries out the recycling of gold, silver, four kinds of copper, mercury elements to gold refining acid waste water simultaneously, rationally distributed, various
The rate of recovery of element is high, sets up 1,2, No. 3 storage tank, so that the metal ion in spent acid is made to be sufficiently displaced from or be precipitated, and
By 600 ± 10 DEG C of 3.5 ~ 4.5h of drying in the present invention, HgS is set to resolve into Hg steam, to carry out effective recycling to Hg.
About 3.8 tons of copper can be recycled after this technological transformation from gold refining acidity efflux wastewater every year, recycle about 1.5 tons of mercury,
Gold about 3kg, silver about 15kg are recycled, creates about more than 120 ten thousand yuan of economic value.
Detailed description of the invention
Fig. 1 is process flow chart of the invention.
Specific embodiment
Below in conjunction with specific embodiments and the drawings, further details of the technical solution of the present invention, but of the invention
Protection scope is not limited thereto.
Embodiment 1
A kind of gold refining acid waste water (pH value 1 ~ 2, Au 2.0 mg/L, Ag 30mg/L, Cu 2.0g/L, Hg 2.0mg/L) is more
Element comprehensive recycling process, as shown in Figure 1, including the following steps:
(1) by gold refining acid waste water 60m3Feeding carbon adsorption slot (adsorption tank once fills 3 tons of almond charcoal, runs about one-year age,
Adsorption cycle is more than 3 days, gold grade is up to 1500g/ ton) carry out circulation carbon adsorption up to gold grade 0.10mg/L in liquid, simultaneously
Gold loaded carbon is obtained, gold loaded carbon sends to parsing；
(2) gold grade is that the liquid of 0.10mg/L is sequentially sent to No. 1, No. 2, No. 3 storage tank (bodies of each storage tank with the flow velocity of 2m/s
Product is 80m3) in carry out metal ion displacement reaction, sediment 10kg(1 of previous No. 2 storage tanks is added into No. 1 storage tank
The recycling of each moon tissue of storage tank sediment is primary, and the sediment of recycling is put into titanium slot and is sent into industrial resistance furnace), it is stored up to No. 2
The sediment 25kg of previous No. 3 storage tanks is added in tank, iron powder 25kg and Na are added into No. 3 storage tanks2S 15kg, liquid is each
The processing time in storage tank is 2 hours, and No. 1 storage tank can about displace 65% of contained total metal mass in liquid, No. 2 storage tanks
Can about displace 25% of contained total metal mass in liquid, No. 3 storage tanks about can in replacement fluid contained total metal mass 5%.
Supernatant in No. 3 storage tanks carries out water process between draining into water treatment vehicle outside；Sediment in No. 3 storage tanks is at 600 DEG C
It dries 4h demercuration (mercury boiling point is 356.73 DEG C), mercury vapour is cooled into liquid mercury, and borax and pure is added into the slag after drying
Alkali is refined greatly, and detailed process is as follows: according to the slag after drying, borax, soda ash mass ratio 1:0.3:0.2 ingredient, intermediate frequency is added
1900 DEG C of progress meltings, obtain melting liquid, melting liquid are poured into crouching tank in furnace, and the alloy that crouching tank lower part is formed is taken out after cooling
Alloy, is put into intermediate frequency furnace melts again by (utilizing gravity, slag is different with the density of alloy, and alloy deposition is in crouching tank lower part)
Change, metal liquid pours into the anode dimension needed when cathode copper after fusing；
(3) the big refining slag after big refining sends to ball milling, ore matching, and the alloy after big refining pours into anode, is Cu in electrolyte composition2+
35g/L, H+220g/L, SO4 2- 255g/L, current density 190A/m2, tank voltage is that electrolysis 22 hours is carried out under 2.2V, electrolysis
Cathode output fine copper (purity Cu >=99.5%) afterwards, anode generate the earth of positive pole (mainly gold and silver)；The earth of positive pole is handled through superchlorination
To gold and silver and waste residue, waste residue returns to big refining；
The process of the chlorination processing is as follows:
A. acidleach: 600L30wt% hydrochloric acid is added into reaction kettle and 300L water obtains dilute hydrochloric acid solution, adds 300kg anode
Mud, 90 DEG C are leached 3 hours, slag-liquid separation；
B. chlorination: 600L30wt% hydrochloric acid is added into reaction kettle and 300L water obtains dilute hydrochloric acid solution, is heated under stirring
The slag charge that a step is isolated is added at 50 DEG C, when temperature rises to 80 DEG C, sodium chlorate is added, sodium chlorate dosage is in the earth of positive pole
2 times of golden amount, 90 DEG C are stirred to react 2.5 hours, end of reaction, stand 30 minutes, start slag-liquid separation, and liquid self-flowing enters
In reduction reaction kettle, slag investment displacement kettle adds iron replacement to go out silver, and the waste residue of generation returns to big refining；
C. restore: from flow into reduction reaction kettle in liquid, heat under stiring, be warming up to 85 DEG C or more addition sodium sulfites into
Row reduction, the additional amount of sodium sulfite are 2 times of golden amount in liquid, when in supernatant gold content in 3mg/L hereinafter, can be whole
It only reacts, is separated by solid-liquid separation, gold 0.2 mg/L, silver-colored 10mg/L, copper 0.5g/L in liquid, mercury 0.2mg/L, pH value are 3 ~ 4, gold recycling
Rate 96%, silver raising recovery rate 83%, copper recovery 93%, the mercury rate of recovery 90%；Liquid sends to charcoal absorption, and solid is bronze, after drying
It is added in intermediate frequency furnace and melts out ingot.
About 3.8 tons of copper can be recycled from gold refining acidity efflux wastewater every year according to above-mentioned processing step, recycles mercury about 1.5
Ton recycles gold about 3kg, silver about 15kg, creates about more than 120 ten thousand yuan of economic value.
Embodiment 2
A kind of gold refining acid waste water (pH value 1 ~ 2, Au 3.0mg/L, Ag 20mg/L, Cu 2.5g/L, Hg 1.5mg/L) is polynary
Plain comprehensive recycling process, as shown in Figure 1, including the following steps:
(1) by gold refining acid waste water 60m3Feeding carbon adsorption slot (adsorption tank once fills 3 tons of almond charcoal, runs about one-year age,
Adsorption cycle is more than 3 days, gold grade is up to 1500g/ ton) carry out circulation carbon adsorption up to gold grade 0.15mg/L in liquid, simultaneously
Gold loaded carbon is obtained, gold loaded carbon sends to parsing；
(2) gold grade is that the liquid of 0.15mg/L is sequentially sent to No. 1, No. 2, No. 3 storage tank (bodies of each storage tank with the flow velocity of 1m/s
Product is 80m3) in carry out metal ion displacement reaction, sediment 15kg(1 of previous No. 2 storage tanks is added into No. 1 storage tank
The recycling of each moon tissue of storage tank sediment is primary, and the sediment of recycling is put into titanium slot and is sent into industrial resistance furnace), it is stored up to No. 2
The sediment 20kg of previous No. 3 storage tanks is added in tank, iron powder 20kg and Na are added into No. 3 storage tanks2S 10kg, liquid is each
The processing time in storage tank is 1.5 hours, and No. 1 storage tank can about displace 65% of contained total metal mass in liquid, No. 2 storages
Tank can about displace 25% of contained total metal mass in liquid, and No. 3 storage tanks about can contained total metal mass in replacement fluid
5%。
Supernatant in No. 3 storage tanks carries out water process between draining into water treatment vehicle outside；Sediment in No. 3 storage tanks is at 600 DEG C
It dries 4h demercuration (mercury boiling point is 356.73 DEG C), mercury vapour is cooled into liquid mercury, and borax and pure is added into the slag after drying
Alkali is refined greatly, and detailed process is as follows: according to the slag after drying, borax, soda ash mass ratio 1:0.3:0.2 ingredient, intermediate frequency is added
1850 DEG C of progress meltings, obtain melting liquid, melting liquid are poured into crouching tank in furnace, and the alloy that crouching tank lower part is formed is taken out after cooling
Alloy, is put into intermediate frequency furnace melts again by (utilizing gravity, slag is different with the density of alloy, and alloy deposition is in crouching tank lower part)
Change, metal liquid pours into the anode dimension needed when cathode copper after fusing；
(3) the big refining slag after big refining sends to ball milling, ore matching, and the alloy after big refining pours into anode, is Cu in electrolyte composition2+
40g/L, H+200g/L, SO4 2- 240g/L, current density 150A/m2, tank voltage is that electrolysis 20 hours is carried out under 2.0V, electrolysis
Cathode output fine copper (purity Cu >=99.5%) afterwards, anode generate the earth of positive pole (mainly gold and silver)；The earth of positive pole is handled through superchlorination
To gold and silver and waste residue, waste residue returns to big refining；
The process of the chlorination processing is as follows:
A. acidleach: 600L30wt% hydrochloric acid is added into reaction kettle and 300L water obtains dilute hydrochloric acid solution, adds 300kg anode
Mud, 90 DEG C are leached 3 hours, slag-liquid separation；
B. chlorination: 600L30wt% hydrochloric acid is added into reaction kettle and 300L water obtains dilute hydrochloric acid solution, is heated under stirring
The slag charge that a step is isolated is added at 50 DEG C, when temperature rises to 80 DEG C, sodium chlorate is added, sodium chlorate dosage is in the earth of positive pole
2 times of golden amount, 90 DEG C are stirred to react 2.5 hours, end of reaction, stand 30 minutes, start slag-liquid separation, and liquid self-flowing enters also
In original reactor, slag investment displacement kettle adds iron replacement to go out silver, and the waste residue of generation returns to big refining；
C. restore: from flow into reduction reaction kettle in liquid, heat under stiring, be warming up to 85 DEG C or more addition sodium sulfites into
Row reduction, the additional amount of sodium sulfite are 2 times of golden amount in liquid, when in supernatant gold content in 3mg/L hereinafter, can be whole
It only reacts, is separated by solid-liquid separation, gold 0.15 mg/L, silver-colored 8mg/L, copper 0.4g/L in liquid, mercury 0.15mg/L, pH value are 3 ~ 4, and gold returns
Yield 98%, silver raising recovery rate 85%, copper recovery 95%, the mercury rate of recovery 90%；Liquid sends to charcoal absorption, and solid is bronze, drying
It is added in intermediate frequency furnace afterwards and melts out ingot.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (7)
1. a kind of gold refining acid waste water multielement composite recovery process, characterized in that include the following steps:
(1) gold refining acid waste water feeding carbon adsorption slot is subjected to circulation carbon adsorption until in liquid gold grade lower than 0.2mg/L,
Gold loaded carbon is obtained simultaneously, gold loaded carbon sends to parsing；
(2) liquid of the gold grade lower than 0.2mg/L be sequentially sent to No. 1, No. 2, reacted in No. 3 storage tanks, it is upper in No. 3 storage tanks
Clear liquid carries out water process between draining into water treatment vehicle outside；In 600 ± 10 DEG C of 3.5 ~ 4.5h of drying, mercury steams sediment in No. 3 storage tanks
Gas is cooled into liquid mercury, and borax is added into the slag after drying and soda ash is refined greatly；
(3) the big refining slag after big refining sends to ball milling, ore matching, and the alloy after big refining pours into anode, is Cu in electrolyte composition2+35
~40g/L, H+190~230g/L, SO4 2-225~270g/L, current density are 150~190A/m2, tank voltage be 1.8~
It is carried out under 2.2V electrolysis 18 ~ 22 hours, cathode output fine copper after electrolysis, anode generates the earth of positive pole；The earth of positive pole is handled through superchlorination
Gold and silver and waste residue are obtained, waste residue returns to big refining.
2. gold refining acid waste water multielement composite recovery process according to claim 1, characterized in that into No. 1 storage tank
The sediment of previous No. 2 storage tanks is added, the sediment of previous No. 3 storage tanks is added into No. 2 storage tanks, iron is added into No. 3 storage tanks
Powder and Na2S。
3. gold refining acid waste water multielement composite recovery process according to claim 2, characterized in that place in step (1)
Manage 60m310 ~ 15kg of sediment of previous No. 2 storage tanks need to be added when gold refining acid waste water into No. 1 storage tank, into No. 2 storage tanks
20 ~ 25kg of sediment of previous No. 3 storage tanks is added, iron powder 20 ~ 25kg and Na are added into No. 3 storage tanks210 ~ 15kg of S, waste water
The processing time in each storage tank is 1.5 ~ 2 hours.
4. the gold refining acid waste water multielement composite recovery process according to Claims 2 or 3, characterized in that the iron powder
Middle partial size 0.074mm or less accounts for 75wt% or more.
5. gold refining acid waste water multielement composite recovery process according to claim 1, characterized in that the tool of the big refining
Body process is as follows: according to the slag after drying, borax, soda ash mass ratio 1:0.3:0.2 ingredient, being added 1800 ~ 1900 in intermediate frequency furnace
DEG C melting is carried out, obtains melting liquid, melting liquid is poured into crouching tank, the alloy that crouching tank lower part is formed is taken out after cooling, again will
Alloy, which is put into intermediate frequency furnace, to be melted, and metal liquid pours into the anode dimension needed when cathode copper after fusing.
6. gold refining acid waste water multielement composite recovery process according to claim 1, characterized in that the chlorination processing
Process it is as follows:
A. acidleach: being added hydrochloric acid according to volume ratio 2:1 into reaction kettle and water obtain dilute hydrochloric acid solution, add the earth of positive pole, sun
The quality of pole mud and the mass ratio of dilute hydrochloric acid solution are 1 ︰ (2.5 ~ 4.5), and 85 ~ 95 DEG C are leached 2.5 ~ 3.5 hours, slag-liquid separation；
B. chlorination: hydrochloric acid is added according to volume ratio 2:1 into reaction kettle and water obtains dilute hydrochloric acid solution, is heated under stirring
The slag charge that a step is isolated is added at 80 DEG C, keeps at 80 DEG C, sodium chlorate is added, sodium chlorate dosage is golden amount in the earth of positive pole
1.5-2.5 times, 90-95 DEG C is stirred to react 2 ~ 4 hours, end of reaction, stand 15-30 minute, start slag-liquid separation, liquid oneself
It flows into reduction reaction kettle, slag investment displacement kettle adds iron replacement to go out silver；
C. it restores: being warming up to 85 DEG C or more addition sodium sulfites in agitating and heating from the liquid flowed into reduction reaction kettle and carry out
Reduction, the additional amount of sodium sulfite are 1.5-2.5 times of golden amount in liquid, when in supernatant gold content in 3mg/L hereinafter, being
Reaction can be terminated, is separated by solid-liquid separation, liquid sends to charcoal absorption, and solid is bronze, is added in intermediate frequency furnace after drying and melts out ingot.
7. gold refining acid waste water multielement composite recovery process according to claim 6, characterized in that the hydrochloric acid it is dense
Degree is 29 ~ 35wt%.
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| CN1718784A (en) * | 2005-07-07 | 2006-01-11 | 孙涛 | Method of recovery copper, nickel and noble metal in waste water and slag by combined technology of wet method and fire method |
| CN101451190A (en) * | 2007-11-30 | 2009-06-10 | 灵宝市金源矿业有限责任公司 | Novel method for separating gold and silver from gold mud |
| CN102286663A (en) * | 2011-08-19 | 2011-12-21 | 北京矿冶研究总院 | Treatment method of copper-containing gold mud |
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| CN1718784A (en) * | 2005-07-07 | 2006-01-11 | 孙涛 | Method of recovery copper, nickel and noble metal in waste water and slag by combined technology of wet method and fire method |
| CN101451190A (en) * | 2007-11-30 | 2009-06-10 | 灵宝市金源矿业有限责任公司 | Novel method for separating gold and silver from gold mud |
| CN102286663A (en) * | 2011-08-19 | 2011-12-21 | 北京矿冶研究总院 | Treatment method of copper-containing gold mud |
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