CN106075800B - A method of using arsenic containing solution preparation there is ferric arsenate/goethite material of core-shell structure to realize solid arsenic - Google Patents
A method of using arsenic containing solution preparation there is ferric arsenate/goethite material of core-shell structure to realize solid arsenic Download PDFInfo
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- CN106075800B CN106075800B CN201610388443.1A CN201610388443A CN106075800B CN 106075800 B CN106075800 B CN 106075800B CN 201610388443 A CN201610388443 A CN 201610388443A CN 106075800 B CN106075800 B CN 106075800B
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- A62D3/00—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances
- A62D3/30—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances by reacting with chemical agents
- A62D3/33—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances by reacting with chemical agents by chemical fixing the harmful substance, e.g. by chelation or complexation
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- A—HUMAN NECESSITIES
- A62—LIFE-SAVING; FIRE-FIGHTING
- A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
- A62D2101/00—Harmful chemical substances made harmless, or less harmful, by effecting chemical change
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Abstract
The invention discloses a kind of methods that using arsenic containing solution preparation there is ferric arsenate/goethite material of core-shell structure to realize solid arsenic；After the pH of arsenic containing solution is adjusted to acidity, ferrous salt is added in the arsenic containing solution and is passed through oxygen-containing gas, is stirred to react in a heated condition, obtains precipitated ferric arsenate；The precipitated ferric arsenate, which is immersed in alkaline solution, to react, up to ferric arsenate/goethite material with core-shell structure, arsenic in arsenic containing solution can be passed through the technique of simple low cost by this method, the particularly preferred ferric arsenate with the core-shell structure/goethite material of stability is made, realizes being permanently fixed for arsenic.
Description
Technical field
The invention particularly relates to a kind of preparation methods of Core-shell structure material containing arsenic；In particular to using arsenious waste solution or
The method that there is ferric arsenate/goethite material of core-shell structure to realize solid arsenic for arsenic leaching solution preparation, belongs to field of environmental improvement,
Background technique
Arsenic is a kind of toxic element, in the earth's crust mainly with the indissolubles arsenate such as calcium, iron, manganese, aluminium of low toxicity and realgar,
Orpiment, the form stable of mispickel sulfides are present in rock stratum and soil.The mankind are during mineral resource development and utilization, arsenic
Natural stability form destroyed and released the water-soluble arsenic of high poison, the height especially generated in nonferrous metallurgical process
Concentration arsenic-containing waste water has become one of the main path of release high poison arsenic.In recent years, in China Hunan, Guangxi, Guizhou, cloud
A lot of regional arsenic poisoning events have occurred in the nonferrous smeltings industry dense region such as south, and arsenic pollution has become social extensive concern
Tender subject.To this kind of high arsenic Metallurgical Waste Water, processing method reported in the literature has chemical precipitation method, ion-exchange, absorption
Method, extraction and biochemical method [etc., but only chemical precipitation method can be applied at industrial scale at present.Chemical precipitation
The basic principle of method is the indissoluble arsenate that the high poison arsenic of solution state is changed into low toxicity, and by security landfill back to greatly certainly
In so.Chemical precipitation method require indissoluble arsenate precipitating to have arsenic removal is high-efficient, solid arsenic safety is good, and cost it is more low more
It is good.According to China's national standard, the remaining arsenic concentration in arsenic removal rear solution is required to be reduced to 50 μ g/L in terms of arsenic removal efficiency,
Gu arsenic safety is then evaluated by toxicity leaching experiment (TCLP), it is desirable that leachate arsenic concentration is less than 5mg/L.
Currently, only calcium arsenate and two class indissoluble arsenate of ferric arsenate can better meet above-mentioned requirements.Calcium arsenate and
Ferric arsenate is substantially similar on arsenic removal process, and the molysite depositions such as lime or ferric sulfate are added by certain C a/As ratio or Fe/As ratio
The calcium arsenate and precipitated ferric arsenate of indissoluble can be obtained after neutralizer adjustment pH value is added in agent.It is high for acid concentration useless containing arsenic
Water makees neutralizer using lime, consolidates arsenic using the calcium arsenate of generation, is the common method of current enterprise, but the water after arsenic removal
CaSO in solution4Content is higher, and subsequent processing is very troublesome.The integrated operation cost of usual calcium arsenate arsenic removal is lower than ferric arsenate,
However ferric arsenate the high efficiency of arsenic removal, solid arsenic safety in terms of have a clear superiority.The solubility in water of ferric arsenate
(AB type refractory tungsten alloys, solubility product 10-21~10-24Left and right, solubility about 10-11mol.L-1) than calcium arsenate (A2B3Type indissoluble electricity
Xie Zhi, solubility product 10-18~10-21, solubility about 10-5mol.L-1) about 1,000,000 times small, while in arsenic acid calcium salt and air
Formation calcium carbonate and water-soluble arsenic acid after carbon dioxide exposure, lead to " the anti-molten phenomenon " of arsenic and there are security hidden troubles.By
In ferric arsenate popularization and application there are Cost Obstacles, domestic smelter would rather select the calcium arsenate with security risk to remove mostly
Arsenic.And by the arsenic removal cost of ferric arsenate be greatly reduced with the comparable level of calcium arsenate, need the consumption of molysite deposition agent
Drop amount cuts down more than half, that is, needs to be down to Fe/As ratio within 2 from 4 or so from technique.
Summary of the invention
There is solid the defects of arsenic is at high cost, arsenic fixation effect is poor for existing As retention, the purpose of the present invention is be to mention
For a kind of method of inexpensive, efficient arsenic admittedly, this method can be made by the arsenic in arsenic containing solution by the technique of simple low cost
At the particularly preferred ferric arsenate with the core-shell structure/goethite material of stability, being permanently fixed for arsenic is realized.
In order to achieve the above technical purposes, the present invention provides a kind of arsenic using arsenic containing solution preparation with core-shell structure
The method that sour iron/goethite material realizes solid arsenic, after the pH of arsenic containing solution is adjusted to acidity, is added in the arsenic containing solution
Ferrous salt and it is passed through oxygen-containing gas, is stirred to react in a heated condition, obtains precipitated ferric arsenate；The precipitated ferric arsenate is immersed in
In alkaline solution react to get.
Technical solution of the present invention key is for arsenic to be converted to the preferable ferric arsenate of stability, further in ferric arsenate
The goethite layer of Surface Creation densification, protects ferric arsenate, forms a kind of special Core-shell structure material, can be effectively real
Arsenic in existing arsenious waste solution or arsenic leaching solution is permanently fixed, and prevents the arsenic dissolution after fixing from causing secondary pollution.
Preferred scheme, arsenic containing solution are that the arsenic-containing waste water that metallurgical industry generates or arsenic-containing smoke dust and/or slag contain arsenic
Leachate.Generally it is adapted to the high arsenic cigarette generated in the smelting processes such as the various smelting waste liquids containing arsenic or lead, zinc, antimony, copper, tin
The arsenic leaching solution of the metallurgical wastes such as the high arsenic content anode slurry generated in the electrolytic processes such as dirt and lead bullion, silver, copper.
Preferred scheme, arsenic content is 5~50 grams per liters in arsenic-containing water solution.
More preferably scheme, arsenic containing solution pH are adjusted to 1~3.It is molten using sulfuric acid solution and/or sodium hydroxide to adjust pH
Liquid.
Preferred scheme, additional amount of the ferrous salt in arsenic containing solution are 1.2~5 times of arsenic mol in arsenic containing solution.
More preferably scheme, ferrous salt are at least one of ferrous sulfate, frerrous chloride, ferrous nitrate.
Preferred scheme, the flow velocity of oxygen-containing gas is 0.1~5 liter/per minute；The oxygen-containing gas is oxygen and/or sky
Gas.
Ferrous salt is added in the arsenic containing solution and is passed through oxygen-containing gas, is again heated to 70~95 for more preferably scheme
DEG C, it is stirred to react 6~12 hours.
Preferred scheme, the pH of alkaline solution are 10~14.
More preferably scheme, it is 1~24 hour that the precipitated ferric arsenate, which is immersed in time for reacting in alkaline solution,.
Compared with the prior art, technical solution of the present invention bring advantageous effects:
Technical solution of the present invention for the first time using arsenious waste solution as raw material, prepare a kind of ferric arsenate with core-shell structure/
Goethite material realizes being permanently fixed for arsenic.Arsenic is converted to difficulty using ferrous salt as raw material, by acidic oxidation by the technical solution
It is dissolved in the precipitated ferric arsenate of water, precipitated ferric arsenate further reacts in alkaline solution, forms one layer of densification in arsenic acid iron surface
Goethite layer, to ferric arsenate carry out second protection, substantially increase ferric arsenate/goethite material stability.Pass through toxicity
Leaching experiment (TCLP) is carried out according to the regulation of " solid waste Leaching leaching method horizontal vibration method HJ 557-2010 "
Test, the results showed that arsenic concentration is lower than in " hazardous waste judging standard leaching characteristic identification GB 5085.3-2007 " in leachate
5 mg/litres of defined meet the standard that safety consolidates arsenic compound.
Technical solution of the present invention realizes the fixation of arsenic by two-step method, and reaction condition is mild, and step is simple；And use
Gu arsenic raw material is ferrous salt, air or oxygen etc., cheap, be conducive to promote and apply；The arsenic with core-shell structure of preparation
Sour iron/goethite material illustrates that it is safe and reliable by toxicity characteristic leaching procedure, can be used as preferably arsenic material admittedly, solves current smelting
The arsenic pollution problem of golden enterprise.
Detailed description of the invention
[Fig. 1] is specific flow chart of the present invention；
[Fig. 2] is the X-ray powder diffraction figure that core-shell structure consolidates arsenic material in the embodiment of the present invention 1；
[Fig. 3] is that core-shell structure consolidates arsenic scanning of materials electron microscope in the embodiment of the present invention 1.
Specific embodiment
Following embodiment is intended to illustrate summary of the invention, rather than further limits to the scope of the present invention.
Raw material arsenic-containing water solution of the present invention is derived from the high-arsenic dust leachate of Hunan copper smelting plant institute output,
Liquid and preparation method thereof is leached to make according to patent " a kind of high arsenic metallurgical waste gradient arsenic removing method " (patent No. 201110379510)
It is standby.The content of arsenic in solution is determined by ICP, and the concentration of arsenic in solution is adjusted by evaporating or being diluted with water.
Toxicity leaching experiment (TCLP), according to " solid waste Leaching leaching method horizontal vibration method HJ 557-
Prepared ferric arsenate/goethite Core-shell structure material is added in distilled water by regulation 2010 ", and solid-to-liquid ratio is 1 to 10,
Level concussion 8 hours, after standing 16 hours, is filtered and is collected leachate, leaching is tested using plasma direct-reading spectrometer (ICP)
Out in liquid arsenic concentration.
Embodiment 1
The arsenic containing solution for preparing 1 liter of 30 grams per liter according to the method described above adjusts pH value of solution to 1 using the concentrated sulfuric acid.According to iron arsenic
Molar ratio 1.5 weighs 166.83 grams of green vitriol, is added in solution and solution is kept to stir.It is passed through into solution
Oxygen, flow velocity are 0.5 liter/min.Solution is heated to 90 degrees Celsius, is kept stirring and reacts 7 hours with logical oxygen.It is cold to solution
But it filtering afterwards, precipitating is washed with deionized, and it is dry, obtain shallow green powder solid.And use plasma direct-reading spectrometer
(ICP) arsenic content after reacting in solution is tested, it is 99.6% that heavy arsenic rate, which is obtained by calculation,.By obtained solid powder
It is soaked in the sodium hydroxide solution that pH is 11 12 hours, is filtered, washed, dries, obtain khaki powder, this is target production
Object.X-ray powder diffraction finally has been carried out to product and field emission scanning electron microscope is tested, Fig. 2 is the X that core-shell structure consolidates arsenic material
Ray powder diffraction pattern, as can be seen from the figure material prepared is the compound of two hydration ferric arsenates and goethite really；Fig. 3
Consolidate arsenic scanning of materials electron microscope for core-shell structure, the kernel and shell of material, show our material as we can clearly see from the figure
Material is Core-shell structure material really.
Embodiment 2
The arsenic containing solution for preparing 1 liter of 10 grams per liter according to the method described above adjusts pH value of solution to 1 using the concentrated sulfuric acid.According to iron arsenic
Molar ratio 2 weighs 74.15 grams of green vitriol, is added in solution and solution is kept to stir.Oxygen is passed through into solution
Gas, flow velocity are 2 liters/min.Solution is heated to 80 degrees Celsius, is kept stirring and reacts 9 hours with logical oxygen.After solution is cooling
Filtering, precipitating are washed with deionized, dry, obtain shallow green powder solid.And it is surveyed using plasma direct-reading spectrometer (ICP)
The arsenic content after reacting in solution is tried, it is 99.4% that heavy arsenic rate, which is obtained by calculation,.Obtained solid powder is soaked in
6 hours in the sodium hydroxide solution that pH is 13, it is filtered, washed, dries, obtain pale red powder, this is target product.
Embodiment 3
The arsenic containing solution for preparing 1 liter of 50 grams per liter according to the method described above adjusts pH value of solution to 2 using the concentrated sulfuric acid.According to iron arsenic
Molar ratio 3 weighs 397.62 grams of Iron dichloride tetrahydrate, is added in solution and solution is kept to stir.Sky is passed through into solution
Gas, flow velocity are 5 liters/min.Solution is heated to 70 degrees Celsius, is kept stirring and reacts 12 hours with logical oxygen.It is cooling to solution
After filter, precipitating is washed with deionized, dry, obtains shallow green powder solid.And use plasma direct-reading spectrometer (ICP)
The arsenic content after reacting in solution is tested, it is 99.5% that heavy arsenic rate, which is obtained by calculation,.Obtained solid powder is impregnated
2 hours in the sodium hydroxide solution that pH is 14, it is filtered, washed, dries, obtain red powder, this is target product.
The above product according to " solid waste Leaching leaching method horizontal vibration method HJ 557-2010 " regulation into
Row toxicity characteristic leaching procedure, as a result arsenic concentration is below 5 mg/litres in leachate, is safe solid waste, is safe solid arsenic
Material.
Claims (8)
1. a kind of method that using arsenic containing solution preparation there is ferric arsenate/goethite material of core-shell structure to realize solid arsenic, special
Sign is: after the pH of arsenic containing solution is adjusted to acidity, ferrous salt is added in the arsenic containing solution and is passed through oxygen-containing gas,
It is stirred to react under heating condition, obtains precipitated ferric arsenate；The precipitated ferric arsenate be immersed in alkaline solution react to get；
Additional amount of the ferrous salt in arsenic containing solution is 1.2~5 times of arsenic mol in arsenic containing solution；
The pH of alkaline solution is 10~14.
2. according to claim 1 using arsenic containing solution preparation there is ferric arsenate/goethite material of core-shell structure to realize
Gu the method for arsenic, it is characterised in that: the arsenic containing solution be metallurgical industry generate arsenic-containing waste water or arsenic-containing smoke dust and/or
The arsenic leaching solution of slag.
3. according to claim 1 or 2 have ferric arsenate/goethite material of core-shell structure real using arsenic containing solution preparation
Now consolidate the method for arsenic, it is characterised in that: arsenic content is 5~50 grams per liters in the arsenic-containing water solution.
4. according to claim 1 using arsenic containing solution preparation there is ferric arsenate/goethite material of core-shell structure to realize
Gu the method for arsenic, it is characterised in that: the arsenic containing solution pH is adjusted to 1~3.
5. according to claim 1 using arsenic containing solution preparation there is ferric arsenate/goethite material of core-shell structure to realize
Gu the method for arsenic, it is characterised in that: the ferrous salt is at least one of ferrous sulfate, frerrous chloride, ferrous nitrate.
6. according to claim 1 using arsenic containing solution preparation there is ferric arsenate/goethite material of core-shell structure to realize
Gu the method for arsenic, it is characterised in that: the flow velocity of the oxygen-containing gas be 0.1~5 liter/per minute；The oxygen-containing gas is oxygen
Gas and/or air.
7. according to claim 1, consolidating ferric arsenate/needle iron that arsenic preparation has core-shell structure using arsenic containing solution described in 2,4 or 6
The method that pit wood material realizes solid arsenic, it is characterised in that: ferrous salt is added in the arsenic containing solution and is passed through oxygen-containing gas, then plus
Heat is stirred to react 6~12 hours to 70~95 DEG C.
8. according to claim 1 using arsenic containing solution preparation there is ferric arsenate/goethite material of core-shell structure to realize
Gu the method for arsenic, it is characterised in that: it is 1~24 hour that the precipitated ferric arsenate, which is immersed in time for reacting in alkaline solution,.
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| CN106834712B (en) * | 2016-12-21 | 2018-12-11 | 中南大学 | A kind of method that arsenic-containing smoke dust dearsenification and distribution crystallisation synthesize solid arsenic mineral |
| CN106868320B (en) * | 2016-12-21 | 2019-01-08 | 中南大学 | A kind of high stability consolidates the preparation method of arsenic mineral |
| CN109626547A (en) * | 2018-12-26 | 2019-04-16 | 中南大学 | A method of using ferrous ion catalysis oxidation high concentration trivalent arsenic |
| CN109761285B (en) * | 2019-03-14 | 2019-12-24 | 中南大学 | Preparation method of ferric arsenate @ ferrous sulfide alkali-resistant arsenic-fixing material |
| CN109847256B (en) * | 2019-04-17 | 2021-04-09 | 湖南知远环保科技有限公司 | Ferric arsenate @ polymer arsenic fixation material, preparation method thereof and arsenic fixation method of arsenic-containing solution |
| CN114561558B (en) * | 2022-02-23 | 2023-08-29 | 中南大学 | Method for recycling antimony and fixing arsenic from arsenic-containing crystal |
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