CN105969995A - Method for leaching antimony from copper anode slime high-arsenic purified antimony slag - Google Patents
Method for leaching antimony from copper anode slime high-arsenic purified antimony slag Download PDFInfo
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- CN105969995A CN105969995A CN201610352771.6A CN201610352771A CN105969995A CN 105969995 A CN105969995 A CN 105969995A CN 201610352771 A CN201610352771 A CN 201610352771A CN 105969995 A CN105969995 A CN 105969995A
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- antimony
- slag
- arsenic
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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
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/04—Working-up slag
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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
- C22B30/00—Obtaining antimony, arsenic or bismuth
- C22B30/02—Obtaining antimony
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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
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/008—Wet processes by an alkaline or ammoniacal leaching
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- 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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Abstract
The invention relates to a method for leaching antimony from copper anode slime high-arsenic purified antimony slag. The method comprises the steps that the high-arsenic purified antimony slag with the granularity smaller than 2 mm is subjected to ore grinding and then is pretreated after ore grinding; sodium hydroxide and potassium permanganate are added; the leaching temperature and time, the liquid-solid ratio and the stirring speed are controlled; solid-liquid separation is conducted after reaction is over to obtain a pretreatment solution rich in arsenic and pretreatment slag; then sodium hydroxide and sodium sulphide are added into the pretreatment slag; the leaching temperature and time, the liquid-solid ratio and the stirring speed are controlled; and solid-liquid separation is conducted after reaction is over to obtain a leaching solution rich in antimony and leaching slag. The method has the advantages that the antimony leaching rate is high, the arsenic content of the antimony leaching solution is low, the process is simple, and the treatment cost is low.
Description
Technical field
The present invention relates to the improvement of copper anode mud extract technology, a kind of purify Leaching of Antimony antimony slag from copper anode mud height arsenic
Method.
Background technology
At present, first copper anode mud wet method prevailing technology both domestic and external adds hydrochloric acid and sulphuric acid leaches removing impurities in advance, then adjust
The H of joint leachate+To 0.7～0.9g L-1, make the impurity such as arsenic antimony precipitate in entrance slag at a high ph, typically antimony in this slag
Content is higher, and arsenic content is less than antimony content, and its composition is containing about 34.80wt%Sb, 7.70wt%Cu, 7.50wt%As, 1.30
Wt%Pb, is therefore called for short high arsenic and purifies antimony slag.Owing in this slag, arsenic content is up to more than 7%, and the chemical property of arsenic and antimony is very
Close, therefore use Wet-process metallurgy method in high efficiente callback antimony resource process in alkaline leaching system from this antimony slag, arsenic antimony is same
Time leach, exist containing the difficult problems of a large amount of arsenic in antimony leachate, this difficult problem directly results in follow-up arsenic antimony separation circuit and there is cost
Higher pertinacious disease.
Summary of the invention
It is an object of the invention to purify in antimony slag leaching process for copper anode mud height arsenic, there is arsenic content in antimony leachate higher
A difficult problem, it is provided that a kind of method of Leaching of Antimony from copper anode mud height arsenic purification antimony slag, makes antimony leaching rate reach more than 92.00%.
For achieving the above object, the present invention takes techniques below scheme: a kind of purify Leaching of Antimony antimony slag from copper anode mud height arsenic
Method, the step carried out including next coming in order:
(1) ore grinding: high arsenic purification antimony slag is put in ball mill, controls ore pulp mass concentration and ore grinding time, carry out ore grinding,
After making ore grinding, granularity-325 mesh of slag accounts for more than 75% (i.e. the granularity slag amount less than 44 microns accounts for the 75% of slag gross mass)；
(2) pretreatment: the high arsenic after ore grinding purifies allocates sodium hydroxide and potassium permanganate in antimony slag, control liquid-solid ratio, leach temperature
Degree and extraction time, be stirred continuously, carry out solid-liquid separation afterwards, obtain pretreatment fluid and pretreatment slag；
(3) antimony leaches: allocate sodium hydroxide and sodium sulfide in pretreatment slag into, controls liquid-solid ratio, extraction temperature and extraction time,
It is stirred continuously, carries out solid-liquid separation afterwards, obtain antimony leachate；
The most preferably, in described ore grinding step, high arsenic purifies antimony slag ore pulp mass concentration is 45%～50%, it is therefore an objective to control ball milling
In machine, the gravity flow speed of ore pulp is suitable, reaches preferable grinding efficiency；
The most preferably, in described ore grinding step, the high arsenic purification antimony sizing ore deposit time is 5.0min～10.0min, drum's speed of rotation 25
R/min～30r/min.
The most preferably, the naoh concentration in described pre-treatment step is 35g/L～40g/L, and potassium permanganate concentration is 0.08
G/L～0.10g/L, extraction temperature is 78 DEG C～82 DEG C, response time 2h～3h, and liquid-solid ratio is 3.5:1～4.0:1mL/g, and stirring turns
Speed 280r/min～300r/min；
The most preferably, the naoh concentration that described antimony leaches in step is 30g/L～40g/L, and sodium sulfide concentration is 160g/L
～180g/L, extraction temperature is 85 DEG C～90 DEG C, response time 1h～2h, and liquid-solid ratio is 4:1～5:1mL/g, speed of agitator 280
R/min～300r/min.
The most preferably, described high arsenic purifies antimony slag granularity before ore grinding less than 2mm, it is therefore an objective to ensure the product of ball mill ore grinding
Amount and quality.
The antimony leaching rate of the present invention reaches more than 92.00wt%, and antimony leaching rate is high, and in antimony leachate, arsenic content is few, and technique is simple,
Processing cost is low.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is further described, but is not meant to limiting the scope of the invention:
Embodiment 1
Taking the high arsenic containing arsenic 7.65wt%, antimony 34.90wt% and purify antimony slag 1000g, granularity is less than 2mm, and ore pulp mass concentration is
50%, use ball mill to carry out ore grinding, drum's speed of rotation 25r/min, ore grinding time 5min, obtain the high arsenic after ore grinding and purify antimony
Slag ore pulp.
High arsenic after ore grinding purifies the pretreatment leaching condition of antimony slag ore pulp: naoh concentration is 35g/L, potassium permanganate concentration
For 0.10g/L, extraction temperature is 82 DEG C, response time 2h, and liquid-solid ratio (mL/g) is 3.5:1, speed of agitator 280r/min,
Pretreatment carries out solid-liquid separation after terminating, and obtains pretreatment slag and pretreatment fluid, and in pretreatment fluid, arsenic leaching rate is 86.30wt%,
Antimony leaching rate is 2.32wt%.
The antimony leaching condition of pretreatment slag is: naoh concentration is 40g/L, and sodium sulfide concentration is 160g/L, and extraction temperature is
85 DEG C, response time 1h, liquid-solid ratio (mL/g) is 5:1, and speed of agitator 300r/min obtains leached mud and antimony leachate, antimony
Arsenic leaching rate 5.21wt% in leachate, antimony leaching rate 93.23wt%.
The present embodiment respectively obtains the pretreatment fluid rich in arsenic and the antimony leachate rich in antimony, and in these two kinds of leachates, arsenic always leaches
Rate is 91.51wt%, and the total leaching rate of antimony is 95.55wt%；In antimony leaching rate, arsenic content is less, advantageously reduces follow-up arsenic antimony and divides
From purification process cost.
Embodiment 2
Taking the high arsenic containing arsenic 7.84wt%, antimony 35.20wt% and purify antimony slag 1000g, granularity is less than 2mm, and ore pulp mass concentration is
45%, use ball mill to carry out ore grinding, drum's speed of rotation 30r/min, ore grinding time 10min, obtain the high arsenic after ore grinding and purify
Antimony slag ore pulp.
High arsenic after ore grinding purifies the pretreatment leaching condition of antimony slag ore pulp: naoh concentration is 40g/L, potassium permanganate concentration
For 0.08g/L, extraction temperature is 78 DEG C, response time 3h, and liquid-solid ratio (mL/g) is 4.0:1, speed of agitator 300r/min,
Pretreatment carries out solid-liquid separation after terminating, and obtains pretreatment slag and pretreatment fluid, and in pretreatment fluid, arsenic leaching rate is 87.84wt%,
Antimony leaching rate is 2.71wt%.
The antimony leaching condition of pretreatment slag is: naoh concentration is 30g/L, and sodium sulfide concentration is 180g/L, and extraction temperature is
90 DEG C, response time 2h, liquid-solid ratio (mL/g) is 4:1, and speed of agitator 280r/min obtains leached mud and antimony leachate, antimony
Arsenic leaching rate in leachate is 5.32wt%, and antimony leaching rate is 93.98wt%.
The present embodiment respectively obtains the pretreatment fluid rich in arsenic and the antimony leachate rich in antimony, and in these two kinds of leachates, arsenic always leaches
Rate is 93.16wt%, and the total leaching rate of antimony is 96.69wt%；In antimony leaching rate, arsenic content is less, advantageously reduces follow-up arsenic antimony
Separating-purifying process cost.
Embodiment 3
Taking the high arsenic containing arsenic 7.62wt%, antimony 33.67wt% and purify antimony slag 1000g, granularity is less than 2mm, and ore pulp mass concentration is
48%, use ball mill to carry out ore grinding, drum's speed of rotation 28r/min, ore grinding time 8min, obtain the high arsenic after ore grinding and purify antimony
Slag ore pulp.
High arsenic after ore grinding purifies the pretreatment leaching condition of antimony slag ore pulp: naoh concentration is 38g/L, potassium permanganate concentration
For 0.09g/L, extraction temperature is 80 DEG C, response time 2.5h, and liquid-solid ratio (mL/g) is 3.7:1, speed of agitator 290r/min,
Pretreatment carries out solid-liquid separation after terminating, and obtains pretreatment slag and pretreatment fluid, and in pretreatment fluid, arsenic leaching rate is 86.82wt%,
Antimony leaching rate is 2.41wt%.
The antimony leaching condition of pretreatment slag is: naoh concentration is 35g/L, and sodium sulfide concentration is 170g/L, and extraction temperature is
87 DEG C, response time 1.5h, liquid-solid ratio (mL/g) is 4.5:1, and speed of agitator 290r/min obtains leached mud and antimony leachate,
Arsenic leaching rate 5.52wt% in antimony leachate, antimony leaching rate 93.65wt%.
The present embodiment respectively obtains the pretreatment fluid rich in arsenic and the antimony leachate rich in antimony, and in these two kinds of leachates, arsenic always leaches
Rate is 92.34wt%, and the total leaching rate of antimony is 96.06wt%；In antimony leaching rate, arsenic content is less, advantageously reduces follow-up arsenic antimony
Separating-purifying process cost.
Claims (5)
1. one kind purifies the method for Leaching of Antimony antimony slag from copper anode mud height arsenic, it is characterised in that: include the step that next coming in order are carried out
Rapid:
(1) ore grinding: high arsenic purification antimony slag is put in ball mill, controls ore pulp mass concentration and ore grinding time, carry out ore grinding,
After making ore grinding, granularity-325 mesh of slag accounts for more than 75%；
(2) pretreatment: the high arsenic after ore grinding purifies allocates sodium hydroxide and potassium permanganate in antimony slag, control liquid-solid ratio, leach temperature
Degree and extraction time, be stirred continuously, carry out solid-liquid separation afterwards, obtain pretreatment fluid and pretreatment slag；
(3) antimony leaches: allocate sodium hydroxide and sodium sulfide in pretreatment slag into, controls liquid-solid ratio, extraction temperature and extraction time,
It is stirred continuously, carries out solid-liquid separation afterwards, obtain antimony leachate；
In described ore grinding step, high arsenic purifies antimony slag ore pulp mass concentration is 45%～50%；
In described ore grinding step, the high arsenic purification antimony sizing ore deposit time is 5.0min～10.0min；
Naoh concentration in described pre-treatment step is 35g/L～40g/L, and potassium permanganate concentration is 0.08g/L～0.10g/L,
Extraction temperature is 78 DEG C～82 DEG C, response time 2h～3h, and liquid-solid ratio is 3.5:1～4.0:1mL/g；
The naoh concentration that described antimony leaches in step is 30g/L～40g/L, and sodium sulfide concentration is 160g/L～180g/L, leaching
Going out temperature is 85 DEG C～90 DEG C, response time 1h～2h, and liquid-solid ratio is 4:1～5:1mL/g.
A kind of method of Leaching of Antimony from copper anode mud height arsenic purification antimony slag the most according to claim 1, it is characterised in that:
Described high arsenic purifies antimony slag granularity before ore grinding less than 2mm.
A kind of method of Leaching of Antimony from copper anode mud height arsenic purification antimony slag the most according to claim 1, it is characterised in that:
Drum's speed of rotation 25r/min～30r/min.
A kind of method of Leaching of Antimony from copper anode mud height arsenic purification antimony slag the most according to claim 1, it is characterised in that:
Pre-treatment step and antimony leach speed of agitator in step and are 280r/min～300r/min.
A kind of method of Leaching of Antimony from copper anode mud height arsenic purification antimony slag the most according to claim 1, it is characterised in that:
It is embodied as: taking the high arsenic containing arsenic 7.84wt%, antimony 35.20wt% and purify antimony slag 1000g, granularity is less than 2mm, ore pulp matter
Amount concentration is 45%, uses ball mill to carry out ore grinding, drum's speed of rotation 30r/min, and ore grinding time 10min, after obtaining ore grinding
High arsenic purifies antimony slag ore pulp；
High arsenic after ore grinding purifies the pretreatment leaching condition of antimony slag ore pulp: naoh concentration is 40g/L, potassium permanganate concentration
For 0.08g/L, extraction temperature is 78 DEG C, response time 3h, and liquid-solid ratio is 4.0:1mL/g, and speed of agitator 300r/min locates in advance
Reason carries out solid-liquid separation after terminating, and obtains pretreatment slag and pretreatment fluid, and in pretreatment fluid, arsenic leaching rate is 87.84wt%, and antimony soaks
Going out rate is 2.71wt%；
The antimony leaching condition of pretreatment slag is: naoh concentration is 30g/L, and sodium sulfide concentration is 180g/L, and extraction temperature is
90 DEG C, response time 2h, liquid-solid ratio is 4:1mL/g, speed of agitator 280r/min, obtains leached mud and antimony leachate, and antimony soaks
Going out the arsenic leaching rate in liquid is 5.32wt%, and antimony leaching rate is 93.98wt%.
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| CN201610352771.6A CN105969995B (en) | 2016-05-25 | 2016-05-25 | A kind of method of Leaching of Antimony in high arsenic purification antimony slag from copper anode mud |
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| CN201610352771.6A CN105969995B (en) | 2016-05-25 | 2016-05-25 | A kind of method of Leaching of Antimony in high arsenic purification antimony slag from copper anode mud |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112779425A (en) * | 2020-05-20 | 2021-05-11 | 昆明冶金研究院有限公司 | Method for preparing sodium antimonate from stibnite |
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| CN1194237A (en) * | 1997-03-24 | 1998-09-30 | 张至德 | Wet process for preparing industrial pure antimony sulfide by removing load, arsenic, selenium, tin and mercury impurities in antimonic ore |
| CN102965501A (en) * | 2012-12-21 | 2013-03-13 | 江西铜业股份有限公司 | Method for processing copper anode slime in total wet manner |
| CN105063354A (en) * | 2015-08-18 | 2015-11-18 | 北京矿冶研究总院 | Cascade recovery method of arsenic-containing and antimony-containing refractory gold ore |
| CN105274359A (en) * | 2015-10-21 | 2016-01-27 | 北京矿冶研究总院 | Method for extracting and separating valuable metals from secondary lead smelting slag |
-
2016
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Patent Citations (4)
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| CN1194237A (en) * | 1997-03-24 | 1998-09-30 | 张至德 | Wet process for preparing industrial pure antimony sulfide by removing load, arsenic, selenium, tin and mercury impurities in antimonic ore |
| CN102965501A (en) * | 2012-12-21 | 2013-03-13 | 江西铜业股份有限公司 | Method for processing copper anode slime in total wet manner |
| CN105063354A (en) * | 2015-08-18 | 2015-11-18 | 北京矿冶研究总院 | Cascade recovery method of arsenic-containing and antimony-containing refractory gold ore |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112779425A (en) * | 2020-05-20 | 2021-05-11 | 昆明冶金研究院有限公司 | Method for preparing sodium antimonate from stibnite |
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