CN106868320B - A kind of high stability consolidates the preparation method of arsenic mineral - Google Patents
A kind of high stability consolidates the preparation method of arsenic mineral Download PDFInfo
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- CN106868320B CN106868320B CN201611195704.4A CN201611195704A CN106868320B CN 106868320 B CN106868320 B CN 106868320B CN 201611195704 A CN201611195704 A CN 201611195704A CN 106868320 B CN106868320 B CN 106868320B
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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
- C22B30/04—Obtaining 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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
Abstract
The present invention relates to the preparation methods that a kind of high stability consolidates arsenic mineral, will contain high arsenic solution dearsenification and be solidified, arsenic containing solution is made to obtain harmless treatment.The present invention by the trivalent arsenic in arsenic containing solution after catalysis oxidation is pentavalent arsenic, oxidated solution using lime sink arsenic method and distribution crystallisation, regulation growth method, any one of three kinds of hydro-thermal method combine, synthesize the solid arsenic mineral of high stable, can directly store up.It first passes through the heavy arsenic method of lime and obtains calcium arsenate, calcium arsenate is changed into the solid arsenic mineral of high stability using distribution crystallisation, regulation growth method, any one of three kinds of hydro-thermal method again, toxicity leaching meets GB5085.3-2007 (solid waste judging standard-leaching characteristic identification) regulation.Present invention process process is short, and arsenic effect of sinking is good, sink after arsenic liquid can direct emission, the solid arsenic mineral stability of synthesis is high, can stablize stockpiling under the conditions of wide ph range 2~11 and strong reducing property.
Description
Technical field
The invention belongs to mineral As retention field, it is related to the preparation method that a kind of high stability consolidates arsenic mineral.
Background technique
Arsenic is a kind of hypertoxic element, and has high carcinogenic, and extensive association is in various non-ferrous metal metallurgy process systems.Closely
Over 30 years, as China's non-ferrous metal industry develops rapidly, arsenic pollution problem is more severe, seriously threatens the life of people
Health.Therefore, carrying out arsenic pollution Controlling research is a urgent and significant project.
As retention mainly includes that encapsulating and mineral consolidate two class of arsenic at present.Encapsulating is exactly to use the materials such as cement, glass, to containing
Arsenic material is coated, and stockpiling can be stablized.This method solid waste amount is big, at high cost, it is difficult to be widely applied.Mineral consolidate arsenic
The high arsenic-containing ores of stability are converted by arsenic to store up.Gu the selection of arsenic mineral, should from leach stability, mineral arsenic content,
Leach product toxicity, the many-sided choosing comprehensively of preparation complexity and cost etc..Primary and secondary arsenic mineral, although sum is up to
More than 300, but " choosing of satisfaction " that wherein can be used to consolidate arsenic belongs to rare in fact.In Ca (II)-As (V)-H2In O system, different items
A series of calcium arsenate mineral, high stability can be synthesized under part；But solubility is larger in acid condition for calcium arsenate, and
Ca (II) ion therein can be with solubilised state CO2Reaction generates calcium carbonate and releases arsenic again.Therefore, calcium arsenate class mineral
And solid arsenic mineral should not be used as.In Fe (III)-As (V)-H2In O system, change reaction condition can prepare it is a series of composition,
Crystal form and the different precipitated ferric arsenate of crystallinity.Wherein, scorodite (FeAsO4·2H2O), because its stability is high, theory arsenic content
Up to 32%, it is easy to the aqueous low advantage of solid-liquor separation, slag in crystalline state, is best arsenic mineral admittedly generally acknowledged at present.
The preparation method of scorodite is broadly divided into three categories at present: hydro-thermal method, non-pressure process and improvement non-pressure process.Wherein hydro-thermal
For method due to the high temperature and pressure of needs, energy consumption is larger, it is difficult to industrial application；Non-pressure process prepares scorodite, but its period under normal pressure
It is longer；It improves non-pressure process and degree of supersaturation is controlled by slow iron protoxide ion under the conditions of normal pressure, 75~90 DEG C, at 7 hours
It is inside prepared for high-crystallinity scorodite, is best preparation method generally acknowledged at present.Scorodite has stronger stability, previous
Research in arsenic leaching concentration most down to 0.5mg/L, but this is only limitted under faintly acid (pH value 2~6) and oxidizing condition, and
It is poor to leach stability for highly acid or basic region or under reductive condition.Therefore, further research is prepared to alkalinity
Scorodite with strong reducing property ambient stable be very it is necessary to.
In the patent announced at present, Japanese same and mining industry Co., Ltd patent of invention (CN 102153145 A, CN
101952204 A) to be put forward for the first time with ferrous iron be source of iron, arsenic containing solution is handled, and scorodite and iron arsenate powder is prepared,
The heavy arsenic of this method is thorough, simple and convenient, but the scorodite and ferric arsenate prepared only can be steady in relatively narrow pH (2~6) range
Fixed stockpiling, the toxicity of arsenic leaches the limit far more than GB5085.3-2007 national Specification under the conditions of alkalinity or strong reducing property
It is worth (< 5mg/L).
Summary of the invention
The purpose of the present invention is to provide the preparation methods that a kind of high stability consolidates arsenic mineral, and one kind can be prepared and exist
Stable solid arsenic mineral under the conditions of wide pH range and strong reducing property.Simple process of the invention, easy to operate, the solid arsenic minerals of preparation
Object arsenic content is higher, and toxicity leaching concentration is very low, and stable region field width, can stablize stockpiling under the conditions of strong reducing property.
To achieve the purpose of the present invention, the following technical schemes are provided:
A kind of high stability consolidates the preparation method of arsenic mineral, comprising the following steps:
(1) arsenic containing solution catalysis oxidation
By way of catalysis oxidation, oxidizing gas and catalyst are added into arsenic containing solution, by the As in solution3+Turn
Become As5+；
(2) the heavy arsenic of oxidated solution
Solution ph after oxidation obtained by step (1) is adjusted to 1.5~3, CaO, Ca are added in a manner of continuous charging
(OH)2One or both of as heavy arsenical, make 2~8:1 of molar ratio of Ca and As in the solution, sedimentation time 5
~10 hours, reaction temperature was 10 DEG C~90 DEG C；It reacts and calcium arsenate is made；
(3) solid arsenic mineral is synthesized
Using distribution crystallisation, regulation growth method, any Arsenic fixation method in three kinds of hydro-thermal method by arsenic obtained by step (2)
Sour calcium synthesizes solid arsenic mineral.
In step (1), the main component of the arsenic containing solution includes: 5~100g/L of As, Sb 0.5g/L~3g/L, Pb
10~120g/L of 50ppm~800ppm, Sn 2ppm~200ppm, Te 10~500ppm, NaOH.
Oxidizing gas described in step (1) is oxygen, air or oxygen-enriched air；Preferably, the oxidizing gas
Gas flow is controlled in 1~20L/min.
Catalyst described in step (1) is KMnO4；Preferably, the molar ratio of As and Mn is controlled in 5:1~50:1.
The temperature of the control of catalytic oxidation system described in step (1) is 30 DEG C~120 DEG C.
The condition of the control of distribution crystallisation described in step (3) is that addition molysite is molten into reaction system obtained by step (2)
Liquid controls the molar ratio of Fe and As in reaction system in 1~5:1, while neutralizer regulation reaction is added in pH value 1.5~3
Under the conditions of carry out, make Fe3+With AsO4 3-Reaction generates the solid arsenic mineral of high stability；The iron salt solutions include: ferric sulfate solution
At least one of liquid, ferric chloride solution or iron nitrate solution.
Preferably, distribution other control conditions of crystallisation be, reaction temperature be room temperature~120 DEG C, the reaction time be 2h~
10h, mixing speed 50r/min~500r/min.
The condition of the control of regulation growth method described in step (3) is to add ferrous salt into reaction system obtained by step (2)
Solution controls the molar ratio of Fe and As in reaction system in 1~5:1, oxidizing gas is passed through, by Fe2+It is oxidized to Fe3+, together
When be added neutralizer regulation reaction carried out under the conditions of pH value 1.5~3, make Fe3+With AsO4 3-Reaction generates the solid arsenic of high stability
Mineral；
Preferably, regulation other control conditions of growth method be, reaction temperature be room temperature~120 DEG C, the reaction time be 2h~
10h, mixing speed 50r/min~500r/min.
The condition of the control of hydro-thermal method described in step (3) is that step (2) products therefrom is placed in reaction kettle to carry out solid arsenic
Processing, iron salt solutions are added into reaction system, control the molar ratio of Fe and As in reaction system in 1~5:1, regulation reaction
It is carried out under the conditions of pH value 1.5~3, makes Fe3+With AsO4 3-Reaction generates the solid arsenic mineral of high stability；
Preferably, other control conditions of hydro-thermal method are that reaction temperature is 100 DEG C~200 DEG C, and the reaction time is 2h~10h,
Mixing speed 50r/min~500r/min.
Preferably, be distributed iron salt solutions described in crystallisation and hydro-thermal method include: ferrum sulfuricum oxydatum solutum, ferric chloride solution or
At least one of iron nitrate solution；
Preferably, regulating and controlling ferrous salt solution described in growth method includes: ferrous sulfate solution, solution of ferrous chloride or nitre
At least one of sour ferrous iron solution；
Distribution crystallisation, regulation growth method described in neutralizer include: in sodium carbonate, sodium bicarbonate or sodium hydroxide extremely
Few one kind.
Preferably, the addition rate of iron salt solutions or the ferrous salt solution is 5-30ml/min.
The purpose that neutralizer is added is the H of neutralization reaction release+, therefore the additional amount of neutralizer is so that the H that reaction discharges+Quilt
Subject to neutralization.
Preferably, the addition rate of the neutralizer is 5-30ml/min.
Iron salt solutions or ferrous salt solution is added as heavy arsenical in the present invention in a manner of continuous charging, while being added certain
The sodium carbonate of concentration or other alkaline compound solutions react consolidating for synthesizing high-stability as neutralizer, then with the arsenic in solution
Arsenic mineral.
As a kind of specific embodiment of the invention:
Specifically comprise the following steps (process can refer to shown in Fig. 1):
1, oxidizing gas is added into arsenic containing solution by way of catalysis oxidation for arsenic containing solution catalysis oxidation process
And catalyst, by the As in solution3+It is transformed into As5+；
2, oxidated solution consolidates arsenic process, the solution ph after oxidation obtained by step (1) is adjusted to 1.5~3, with continuous charging
Mode CaO, Ca (OH) is added2One or both of as heavy arsenical, make the molar ratio 2 of Ca and As in the solution~
8:1, sedimentation time are 5~10 hours, and reaction temperature is 10 DEG C~90 DEG C；
3, solid arsenic mineral process is synthesized, using any Arsenic fixation method in distribution crystallisation, regulation growth method, hydro-thermal method
Calcium arsenate obtained by step (2) is synthesized into solid arsenic mineral.
Advantages of the present invention:
(1) present invention process is simple, easy to operate, agents useful for same molysite, and oxygen is laboratory common experimental material, instead
Mild condition is answered, it is low for equipment requirements.
(2) solid arsenic mineral crystallinity prepared by the present invention is high, is easy to solid-liquor separation.
(3) the solid arsenic mineral that the present invention prepares is because its crystallinity is high, BET specific surface area is small, stable region field width, and has
Standby high stability.And the leaching concentration of its arsenic is lower than 0.5mg/L, is lower than GB5085.3-2007 (solid waste judging standard-
Leaching characteristic identification) regulation, it can store up safely, solve solid arsenic mineral and be difficult to stablize under alkalinity and reductive condition and store up this
One problem.
In short, the reasonable process of the present invention is arranged in pairs or groups, by the conditional parameter in each process of strict control, synthesize highly crystalline
Degree, bulky grain, high stability consolidate arsenic mineral, can be in wide ph range (2~11) and strong reducing property item Gu arsenic mineral stability is high
Stablize stockpiling under part, reduce the cost of arsenic processing, has achieved the purpose that environmental protection, economical, energy conservation, high security, realized the nothing of arsenic
Evilization.
Detailed description of the invention
Fig. 1 the method for the present invention process flow diagram.
Specific embodiment
The following examples are used to illustrate the present invention, but are not intended to limit the scope of the present invention..
Embodiment 1
Main component includes: As 60g/L, Sb 1.1g/L, Pb 235ppm, Sn 38.5ppm, Te in arsenic containing solution
24.4ppm, NaOH 30g/L.
A kind of high stability consolidates the preparation method of arsenic mineral, comprising the following steps: arsenic containing solution uses the side of catalysis oxidation
Method is by As3+It is oxidized to As5+, the condition of control is oxygen flow 5L/min, and KMnO is added4Make As/Mn molar ratio for catalyst
Control is controlled in 10:1, catalytic oxidation system temperature at 90 DEG C, the results showed that, As3+Conversion ratio be 98.45%.
The pH value of oxidated solution is adjusted to 1.5, CaO and Ca (OH) are added in a manner of continuous charging2As heavy arsenical,
Ca/As molar ratio is 5, and the sedimentation time is 6 hours, and reaction temperature is 60 DEG C, generates calcium arsenate.Solid arsenic mineral is synthesized using distribution
Crystallisation, control condition are iron nitrate solution to be added, while sodium carbonate is added, and make Fe3+With AsO4 3-React synthesizing high-stability
Gu arsenic mineral；Fe/As molar ratio is 2.5, and reaction temperature is 85 DEG C, reaction time 4h, mixing speed 200r/min.Ferric nitrate
The addition speed control of solution is in 2.5ml/min, and the addition speed control of sodium carbonate is in 2.5ml/min.The high stability of synthesis
Gu arsenic mineral carries out toxicity leaching, the leaching of arsenic according to GB5085.3-2007 (solid waste judging standard-leaching characteristic identification)
Concentration is 0.13mg/L out, can safety and stability stockpiling less than the limit value of the standard.
Embodiment 2
Main component includes: As 76g/L, Sb 0.8g/L, Pb 96.7ppm, Sn 27.5ppm, Te in arsenic containing solution
38.7ppm, NaOH 25g/L.
A kind of high stability consolidates the preparation method of arsenic mineral, comprising the following steps: arsenic containing solution uses the side of catalysis oxidation
Method is by As3+It is oxidized to As5+, the condition of control is oxygen flow 10L/min, and KMnO is added4Make As/Mn moles for catalyst
Than control in 40:1, catalytic oxidation system temperature is controlled at 30 DEG C, the results showed that, As3+Conversion ratio be 92.31%；
The pH value of oxidated solution is adjusted to 2, CaO and Ca (OH) are added in a manner of continuous charging2As heavy arsenical, Ca/
As molar ratio is 8, and the sedimentation time is 8 hours, and reaction temperature is 90 DEG C, generates calcium arsenate.Solid arsenic mineral is synthesized using regulation life
Regular way, control condition are that ferrous nitrate solution is added, and oxygen are passed through, by Fe2+It is oxidized to Fe3+, while sodium carbonate is added, make Fe3+
With AsO4 3-React the solid arsenic mineral of synthesizing high-stability；Oxygen flow 5L/min, Fe/As molar ratio is 5, reaction temperature 120
DEG C, reaction time 3h, mixing speed 350r/min.The addition speed control of ferrous nitrate solution is in 10ml/min, sodium carbonate
Addition speed control in 10ml/min.The high stability of synthesis consolidates arsenic mineral, and according to GB5085.3-2007, (solid waste reflects
Other standard-leaching characteristic identification) toxicity leaching is carried out, the leaching concentration of arsenic is that 0.77mg/L can less than the limit value of the standard
Safety and stability stockpiling.
Embodiment 3
Main component includes: As 50g/L, Sb 1.8g/L, Pb 186ppm, Sn 34.7ppm, Te in arsenic containing solution
27.8ppm, NaOH 5g/L.
A kind of high stability consolidates the preparation method of arsenic mineral, comprising the following steps: arsenic containing solution uses the side of catalysis oxidation
Method is by As3+It is oxidized to As5+, the condition of control is oxygen flow 1L/min, and KMnO is added4Make As/Mn molar ratio for catalyst
Control is controlled in 20:1, catalytic oxidation system temperature at 120 DEG C, the results showed that, As3+Conversion ratio be 89.36%
The pH value of oxidated solution is adjusted to 1.5, CaO and Ca (OH) are added in a manner of continuous charging2As heavy arsenical,
Ca/As molar ratio is 5, and the sedimentation time is 10 hours, and reaction temperature is 60 DEG C, generates calcium arsenate.It synthesizes solid arsenic mineral and uses water
Thermal method, control condition are that calcium arsenate is placed in reaction kettle, and ferrum sulfuricum oxydatum solutum is added into kettle, control its Fe/As molar ratio
It is 3, Fe3+With AsO4 3-React the solid arsenic mineral of synthesizing high-stability；Other control conditions are that reaction temperature is 120 DEG C, reaction
Time is 4h, mixing speed 350r/min.The high stability of synthesis consolidates arsenic mineral, and according to GB5085.3-2007, (solid waste reflects
Other standard-leaching characteristic identification) toxicity leaching is carried out, the leaching concentration of arsenic is that 0.54mg/L can less than the limit value of the standard
Safety and stability stockpiling.
Although above having used general explanation, specific embodiment and test, the present invention is made to retouch in detail
It states, but on the basis of the present invention, it can be made some modifications or improvements, this is apparent to those skilled in the art
's.Therefore, these modifications or improvements without departing from theon the basis of the spirit of the present invention, belong to claimed
Range.
Claims (9)
1. the preparation method that a kind of high stability consolidates arsenic mineral, which comprises the following steps:
(1) arsenic containing solution catalysis oxidation
By way of catalysis oxidation, oxidizing gas and catalyst are added into arsenic containing solution, by the As in solution3+It is transformed into
As5+；
(2) the heavy arsenic of oxidated solution
Solution ph after oxidation obtained by step (1) is adjusted to 1.5~3, CaO, Ca (OH) is added in a manner of continuous charging2In
It is one or two kinds of make 2~8:1 of molar ratio of Ca and As in the solution as heavy arsenical, the sedimentation time is small for 5~10
When, reaction temperature is 10 DEG C~90 DEG C；It reacts and calcium arsenate is made；
(3) solid arsenic mineral is synthesized
Calcium arsenate obtained by step (2) is synthesized using any Arsenic fixation method in distribution crystallisation, regulation growth method, hydro-thermal method
Gu arsenic mineral；
The condition of the distribution crystallisation control is to add iron salt solutions into reaction system obtained by step (2), make reaction system
The molar ratio of middle Fe and As is controlled in 1~5:1, while neutralizer regulation reaction is added and carries out under the conditions of pH value 1.5~3, is made
Fe3+With AsO4 3-Reaction generates the solid arsenic mineral of high stability；The addition rate of the iron salt solutions is 5-30mL/min；It is described
Neutralizer includes: at least one of sodium carbonate, sodium bicarbonate or sodium hydroxide；The additional amount of the neutralizer is so that reaction is released
The H put+Subject to being neutralized；The addition rate of the neutralizer is 5-30ml/min；
The condition of the regulation growth method control is to add ferrous salt solution into reaction system obtained by step (2), make reactant
The molar ratio of Fe and As is controlled in 1~5:1 in system, oxidizing gas is passed through, by Fe2+It is oxidized to Fe3+, while neutralizer is added
Regulation reaction carries out under the conditions of pH value 1.5~3, makes Fe3+With AsO4 3-Reaction generates the solid arsenic mineral of high stability；The Asia
The addition rate of iron salt solutions is 5-30mL/min；The neutralizer include: in sodium carbonate, sodium bicarbonate or sodium hydroxide extremely
Few one kind；The additional amount of the neutralizer is so that the H that reaction discharges+Subject to being neutralized；The addition rate of the neutralizer is
5-30ml/min；
The condition of the hydro-thermal method control is that step (2) products therefrom is placed in reaction kettle to carry out solid arsenic processing, to reactant
Iron salt solutions are added in system, control the molar ratio of Fe and As in reaction system in 1~5:1, regulation reaction is in pH value 1.5~3
Under the conditions of carry out, make Fe3+With AsO4 3-Reaction generates the solid arsenic mineral of high stability.
2. the preparation method that high stability according to claim 1 consolidates arsenic mineral, it is characterised in that: described in step (1)
The main component of arsenic containing solution includes: 5~100g/L of As, Sb 0.5g/L~3g/L, Pb 50ppm~800ppm, Sn 2ppm
10~120g/L of~200ppm, Te 10~500ppm, NaOH.
3. the preparation method that high stability according to claim 1 or 2 consolidates arsenic mineral, which is characterized in that institute in step (1)
Stating oxidizing gas is oxygen, air or oxygen-enriched air.
4. the preparation method that high stability according to claim 3 consolidates arsenic mineral, which is characterized in that the oxidizing gas
Gas flow control in 1~20L/min.
5. according to claim 1,2,4 described in any item high stabilities consolidate the preparation method of arsenic mineral, which is characterized in that step
(1) catalyst described in is KMnO4。
6. the preparation method that high stability according to claim 5 consolidates arsenic mineral, which is characterized in that in step (1) As with
The molar ratio of Mn is controlled in 5:1~50:1.
7. according to claim 1,2,4,6 described in any item high stabilities consolidate the preparation method of arsenic mineral, which is characterized in that step
Suddenly the temperature of the control of catalytic oxidation system described in (1) is 30 DEG C~120 DEG C.
8. according to right want 1 described in high stability consolidate the preparation method of arsenic mineral, which is characterized in that the iron salt solutions are sulphur
At least one of sour ferrous solution, ferric chloride solution or iron nitrate solution.
9. the preparation method that high stability according to claim 1 consolidates arsenic mineral, which is characterized in that the ferrous salt solution
For at least one of ferrous sulfate solution, solution of ferrous chloride or ferrous nitrate solution.
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| CN106823234A (en) * | 2016-12-21 | 2017-06-13 | 中南大学 | A kind of method that hydro-thermal method prepares the solid arsenic mineral of high stability |
| CN106823233A (en) * | 2016-12-21 | 2017-06-13 | 中南大学 | A kind of method that fractional crystallisation method prepares the solid arsenic mineral of high stability |
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| CN108946819B (en) * | 2018-07-10 | 2020-11-10 | 中南大学 | Stabilization method of scorodite |
| CN108947420A (en) * | 2018-07-25 | 2018-12-07 | 郴州市金贵银业股份有限公司 | A kind of processing method of arsenic-containing waste residue |
| CN110255770B (en) * | 2019-07-03 | 2022-05-27 | 昆明理工大学 | Method for treating arsenic in nonferrous smelting waste acid by using jarosite slag and carbide slag |
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| CN105499250A (en) * | 2015-12-01 | 2016-04-20 | 昆明理工大学 | Stabilizing treatment method for sulfide arsenic-removed dregs |
| CN105753218B (en) * | 2016-04-13 | 2018-10-16 | 中国科学院过程工程研究所 | A method of removal trivalent arsenic |
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| CN106823234A (en) * | 2016-12-21 | 2017-06-13 | 中南大学 | A kind of method that hydro-thermal method prepares the solid arsenic mineral of high stability |
| CN106823233A (en) * | 2016-12-21 | 2017-06-13 | 中南大学 | A kind of method that fractional crystallisation method prepares the solid arsenic mineral of high stability |
| CN106823233B (en) * | 2016-12-21 | 2019-08-13 | 中南大学 | A method of distribution crystallisation preparation high stability consolidates arsenic mineral |
| CN106823234B (en) * | 2016-12-21 | 2019-08-27 | 中南大学 | A kind of method that hydro-thermal method preparation high stability consolidates arsenic mineral |
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