CN106075800A - A kind of ferric arsenate/goethitum material utilizing arsenic containing solution preparation to have nucleocapsid structure realizes the method for solid arsenic - Google Patents
A kind of ferric arsenate/goethitum material utilizing arsenic containing solution preparation to have nucleocapsid structure realizes the method for solid arsenic Download PDFInfo
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- CN106075800A CN106075800A CN201610388443.1A CN201610388443A CN106075800A CN 106075800 A CN106075800 A CN 106075800A CN 201610388443 A CN201610388443 A CN 201610388443A CN 106075800 A CN106075800 A CN 106075800A
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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
- 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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- A62D2101/43—Inorganic substances containing heavy metals, in the bonded or free state
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Abstract
The invention discloses a kind of method that ferric arsenate/goethitum material utilizing arsenic containing solution preparation to have nucleocapsid structure realizes solid arsenic;After the pH regulator of arsenic containing solution to acidity, described arsenic containing solution add ferrous salt and is passed through oxygen-containing gas, stirring reaction in a heated condition, obtain precipitated ferric arsenate;Described precipitated ferric arsenate is immersed in alkaline solution reaction, must have the ferric arsenate/goethitum material of nucleocapsid structure, the method can be by the arsenic in arsenic containing solution by simple, the technique of low cost, make the particularly preferred ferric arsenate/goethitum material with nucleocapsid structure of stability, it is achieved being permanently fixed of arsenic.
Description
Technical field
The invention particularly relates to a kind of preparation method containing arsenic Core-shell structure material;Particularly to utilizing containing arsenic waste solution or
Arsenic leaching solution preparation has the method that the ferric arsenate/goethitum material of nucleocapsid structure realizes solid arsenic, belongs to field of environmental improvement,
Background technology
Arsenic is a kind of toxic element, in the earth's crust mainly with the indissoluble arsenates such as the calcium of low toxicity, ferrum, manganese, aluminum and Realgar,
Orpimentum (Auripigmentum), the form stable of mispickel sulfides are present in rock stratum and soil.The mankind during mineral resource development and utilization, arsenic
Natural stability form destroyed and discharged the water solublity arsenic of high poison, the height especially produced in nonferrous metallurgical process
Concentration arsenic-containing waste water, has become as one of main path of release high poison arsenic.In recent years, at China Hunan, Guangxi, Guizhou, cloud
The nonferrous smelting industry City Regions such as south there occurs a lot of regional arseniasis event, and arsenic pollutes and has become as society's extensive concern
Tender subject.To this kind of high arsenic Metallurgical Waste Water, the processing method of document report has chemical precipitation method, ion exchange, absorption
Method, extraction and biochemical process [etc., but the most only chemical precipitation method can be applied at industrial scale.Chemical precipitation
The ultimate principle of method is that the high poison arsenic of solution state is changed into the indissoluble arsenate of low toxicity, and by security landfill return to big oneself
In Ran.It is good that chemical precipitation method requires that indissoluble arsenate precipitation possesses high, the solid arsenic safety of arsenic removal efficiency, and cost is the lowest more
Good.According to China's national standard, in terms of arsenic removal efficiency, require that the remaining arsenic concentration in arsenic removal rear solution is reduced to 50 μ g/L,
Gu arsenic safety is then evaluated by toxicity leaching experiment (TCLP), it is desirable to leachate arsenic concentration is less than 5mg/L.
At present, only Tricalcium arsenate and ferric arsenate two class indissoluble arsenate can preferably meet above-mentioned requirements.Tricalcium arsenate and
Ferric arsenate is basic simlarity on arsenic removal process, adds the molysite deposition such as Calx or iron sulfate by certain C a/As ratio or Fe/As ratio
Agent, adds Tricalcium arsenate and the precipitated ferric arsenate that i.e. can get indissoluble after nertralizer adjusts pH value.For high the giving up containing arsenic of acid concentration
Water, uses Calx to make nertralizer, utilizes the solid arsenic of the Tricalcium arsenate generated, and is the conventional method of current enterprise, but the water after arsenic removal
CaSO in solution4Content is higher, and subsequent treatment bothers very much.The generally integrated operation cost of Tricalcium arsenate arsenic removal is lower than ferric arsenate,
But ferric arsenate has clear superiority in terms of the high efficiency of arsenic removal, the safety of solid arsenic.The dissolubility in water of ferric arsenate
(AB type refractory tungsten alloys, solubility product 10-21~10-24Left and right, dissolubility about 10-11mol.L-1) than Tricalcium arsenate (A2B3Type indissoluble electricity
Xie Zhi, solubility product 10-18~10-21, dissolubility about 10-5mol.L-1) little about 1,000,000 times, simultaneously in arsenic acid calcium salt and air
Form calcium carbonate and water solublity arsenic acid after carbon dioxide exposure, cause " the anti-molten phenomenon " of arsenic to there is security hidden trouble.By
There is Cost Obstacles in the popularization and application in ferric arsenate, domestic smelter would rather select the Tricalcium arsenate with potential safety hazard to remove mostly
Arsenic.And the arsenic removal cost of ferric arsenate is greatly reduced the level suitable with Tricalcium arsenate, need the consumption of molysite deposition agent
Fall amount cuts down more than half, namely need from technique by Fe/As than from about 4 be down to 2 within.
Summary of the invention
There is the defects such as high, the arsenic fixation effect difference of solid arsenic cost for existing As retention, it is an object of the invention to be to carry
For a kind of method of low cost, the most admittedly arsenic, the method can be by the arsenic in arsenic containing solution by simple, the technique of low cost, system
Become the particularly preferred ferric arsenate/goethitum material with nucleocapsid structure of stability, it is achieved being permanently fixed of arsenic.
In order to realize above-mentioned technical purpose, the invention provides a kind of arsenic utilizing arsenic containing solution preparation to have nucleocapsid structure
Acid ferrum/goethitum material realizes the method for solid arsenic, after the pH regulator of arsenic containing solution to acidity, adds in described arsenic containing solution
Ferrous salt and be passed through oxygen-containing gas, stirs reaction in a heated condition, obtains precipitated ferric arsenate;Described precipitated ferric arsenate is immersed in
Alkaline solution reacts, to obtain final product.
Technical scheme it is critical only that and arsenic changes into the preferable ferric arsenate of stability, further at ferric arsenate
The goethitum layer that Surface Creation is fine and close, protects ferric arsenate, defines a kind of special Core-shell structure material, can be the most real
Now it is permanently fixed containing the arsenic in arsenic waste solution or arsenic leaching solution, prevents the arsenic dissolution after fixing from causing secondary pollution.
Preferably scheme, arsenic containing solution is the arsenic-containing waste water that metallurgical industry produces, or arsenic-containing smoke dust and/or slag containing arsenic
Leachate.Generally it is adapted to the various smelting waste liquid containing arsenic, or the high arsenic cigarette produced in the smelting process such as lead, zinc, antimony, copper, stannum
The arsenic leaching solution of the metallurgical wastes such as the high arsenic content anode slurry produced in the electrolytic processes such as dirt and lead bullion, silver, copper.
Preferably scheme, in arsenic-containing water solution, arsenic content is 5~50 grams per liters.
More preferably scheme, arsenic containing solution pH regulator to 1~3.Regulation pH uses sulfuric acid solution and/or sodium hydroxide molten
Liquid.
Preferably scheme, ferrous salt addition in arsenic containing solution is 1.2~5 times of arsenic mol in arsenic containing solution.
More preferably scheme, ferrous salt is at least one in ferrous sulfate, ferrous chloride, ferrous nitrate.
Preferably scheme, the flow velocity of oxygen-containing gas is 0.1~5 liter/per minute;Described oxygen-containing gas is oxygen and/or sky
Gas.
More preferably scheme, adds ferrous salt in described arsenic containing solution and is passed through oxygen-containing gas, being again heated to 70~95
DEG C, stirring reaction 6~12 hours.
Preferably scheme, the pH of alkaline solution is 10~14.
More preferably scheme, described precipitated ferric arsenate be immersed in alkaline solution reaction time be 1~24 hour.
Hinge structure, the Advantageous Effects that technical scheme is brought:
Technical scheme first with containing arsenic waste solution as raw material, prepare a kind of there is nucleocapsid structure ferric arsenate/
Goethitum material, it is achieved being permanently fixed of arsenic.Arsenic, with ferrous salt as raw material, is changed into difficulty by acidic oxidation by this technical scheme
Being dissolved in the precipitated ferric arsenate of water, precipitated ferric arsenate reacts further in alkaline solution, forms one layer of densification on ferric arsenate surface
Goethitum layer, ferric arsenate is carried out second protection, substantially increases the stability of ferric arsenate/goethitum material.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, result shows that in leachate, arsenic concentration is less than in " hazardous waste judging standard leaching characteristic identification GB 5085.3-2007 "
5 mg/litre of defined, meet the standard of safety arsenic compound admittedly.
Technical scheme realizes the fixing of arsenic by two-step method, and reaction condition is gentle, and step is simple;And use
Gu arsenic raw material is ferrous salt, air or oxygen etc., cheap, beneficially popularization and application;The arsenic with nucleocapsid structure of preparation
By toxicity characteristic leaching procedure, acid ferrum/goethitum material illustrates that it is safe and reliable, can solve current smelting as arsenic material the most admittedly
The arsenic pollution problem of gold enterprise.
Accompanying drawing explanation
[Fig. 1] is particular flow sheet of the present invention;
[Fig. 2] is the X-ray powder diffraction figure of the solid arsenic material of nucleocapsid structure in the embodiment of the present invention 1;
[Fig. 3] is the solid arsenic scanning of materials Electronic Speculum figure of nucleocapsid structure in the embodiment of the present invention 1.
Detailed description of the invention
Following example are intended to present invention rather than the further restriction to scope are described.
Raw material arsenic-containing water solution of the present invention takes from the high-arsenic dust leachate of Hunan copper smelting plant institute output,
Leachate preparation method is made according to patent " a kind of high arsenic metallurgical waste gradient arsenic removing method " (patent No. 201110379510)
Standby.Determine the content of arsenic in solution by ICP, and regulate the concentration of arsenic in solution by evaporation or dilute.
Toxicity leaching experiment (TCLP), according to " solid waste Leaching leaching method horizontal vibration method HJ 557-
2010 " regulation, joins in distilled water by prepared ferric arsenate/goethitum Core-shell structure material, and solid-to-liquid ratio is 1 to 10,
Level is shaken 8 hours, after standing 16 hours, filters and collect leachate, uses plasma direct-reading spectrometer (ICP) to test leaching
Go out the concentration of arsenic in liquid.
Embodiment 1
Prepare the arsenic containing solution of 1 liter of 30 grams per liter according to the method described above, use concentrated sulphuric acid regulation pH value of solution to 1.According to ferrum arsenic
Mol ratio 1.5 weighs the green vitriol of 166.83 grams, joins in solution and keeps solution stirring.It is passed through in solution
Oxygen, flow velocity is 0.5 liter/min.Solution is heated to 90 degrees Celsius, is kept stirring for and leads to oxygen and react 7 hours.Treat that solution is cold
Filtering the most afterwards, precipitate with deionized water is washed, and is dried, obtains shallow green powder solid.And use plasma direct-reading spectrometer
(ICP) test the arsenic content in solution after reaction, be 99.6% by being calculated heavy arsenic rate.By obtained pressed powder
Being soaked in the sodium hydroxide solution that pH is 11 12 hours, filter, wash, be dried, obtain khaki powder, this is target product
Thing.Product finally having carried out X-ray powder diffraction test with field emission scanning electron microscope, Fig. 2 is the X of the solid arsenic material of nucleocapsid structure
Ray powder diffraction pattern, as can be seen from the figure prepared material is the complex of two hydration ferric arsenates and goethitum really;Fig. 3
For the solid arsenic scanning of materials Electronic Speculum figure of nucleocapsid structure, the kernel of material and shell, show our material as we can clearly see from the figure
Material is Core-shell structure material really.
Embodiment 2
Prepare the arsenic containing solution of 1 liter of 10 grams per liter according to the method described above, use concentrated sulphuric acid regulation pH value of solution to 1.According to ferrum arsenic
Mol ratio 2 weighs the green vitriol of 74.15 grams, joins in solution and keeps solution stirring.Oxygen it is passed through in solution
Gas, flow velocity is 2 liters/min.Solution is heated to 80 degrees Celsius, is kept stirring for and leads to oxygen and react 9 hours.After solution cools down
Filtering, precipitate with deionized water is washed, and is dried, obtains shallow green powder solid.And use plasma direct-reading spectrometer (ICP) to survey
After having tried to react, the arsenic content in solution, is 99.4% by being calculated heavy arsenic rate.Obtained pressed powder is soaked in
PH be 13 sodium hydroxide solution in 6 hours, filter, wash, be dried, obtain pale red powder, this is target product.
Embodiment 3
Prepare the arsenic containing solution of 1 liter of 50 grams per liter according to the method described above, use concentrated sulphuric acid regulation pH value of solution to 2.According to ferrum arsenic
Mol ratio 3 weighs the Iron dichloride tetrahydrate of 397.62 grams, joins in solution and keeps solution stirring.Sky it is passed through in solution
Gas, flow velocity is 5 liters/min.Solution is heated to 70 degrees Celsius, is kept stirring for and leads to oxygen and react 12 hours.Treat that solution cools down
Rear filtration, precipitate with deionized water is washed, and is dried, obtains shallow green powder solid.And use plasma direct-reading spectrometer (ICP)
Test the arsenic content in solution after reaction, be 99.5% by being calculated heavy arsenic rate.Obtained pressed powder is soaked
In the sodium hydroxide solution that pH is 14 2 hours, filtering, wash, be dried, obtain red powder, this is target product.
Above product all enters according to the regulation of " solid waste Leaching leaching method horizontal vibration method HJ 557-2010 "
Row toxicity characteristic leaching procedure, in result leachate, arsenic concentration is below 5 mg/litre, is safe solid waste, is safe solid arsenic
Material.
Claims (10)
1. ferric arsenate/goethitum the material utilizing arsenic containing solution preparation to have nucleocapsid structure realizes a method for solid arsenic, and it is special
Levy and be: after the pH regulator of arsenic containing solution to acidity, described arsenic containing solution adds ferrous salt and is passed through oxygen-containing gas,
Under heating condition, stirring reaction, obtains precipitated ferric arsenate;Described precipitated ferric arsenate is immersed in alkaline solution reaction, to obtain final product.
Ferric arsenate/goethitum the material utilizing arsenic containing solution preparation to have nucleocapsid structure the most according to claim 1 realizes
Gu the method for arsenic, it is characterised in that: described arsenic containing solution be metallurgical industry produce arsenic-containing waste water, or arsenic-containing smoke dust and/or
The arsenic leaching solution of slag.
Ferric arsenate/goethitum the material utilizing arsenic containing solution preparation to have nucleocapsid structure the most according to claim 1 and 2 is real
The method now consolidating arsenic, it is characterised in that: in described arsenic-containing water solution, arsenic content is 5~50 grams per liters.
Ferric arsenate/goethitum the material utilizing arsenic containing solution preparation to have nucleocapsid structure the most according to claim 1 realizes
Gu the method for arsenic, it is characterised in that: described arsenic containing solution pH regulator to 1~3.
Ferric arsenate/goethitum the material utilizing arsenic containing solution preparation to have nucleocapsid structure the most according to claim 1 realizes
Gu the method for arsenic, it is characterised in that: described ferrous salt addition in arsenic containing solution is arsenic mol in arsenic containing solution
1.2~5 times.
Arsenic containing solution preparation is utilized to have ferric arsenate/goethitum material of nucleocapsid structure in fact the most according to claim 1 or 5
The method now consolidating arsenic, it is characterised in that: described ferrous salt is at least one in ferrous sulfate, ferrous chloride, ferrous nitrate.
Ferric arsenate/goethitum the material utilizing arsenic containing solution preparation to have nucleocapsid structure the most according to claim 1 realizes
Gu the method for arsenic, it is characterised in that: the flow velocity of described oxygen-containing gas is 0.1~5 liter/per minute;Described oxygen-containing gas is oxygen
Gas and/or air.
8. according to the arsenic containing solution solid arsenic preparation that utilizes described in claim 1,2,4,5 or 7, there is the ferric arsenate/pin of nucleocapsid structure
Iron mine material realizes the method for solid arsenic, it is characterised in that: in described arsenic containing solution, add ferrous salt and be passed through oxygen-containing gas, then
It is heated to 70~95 DEG C, stirring reaction 6~12 hours.
Ferric arsenate/goethitum the material utilizing arsenic containing solution preparation to have nucleocapsid structure the most according to claim 1 realizes
Gu the method for arsenic, it is characterised in that: the pH of alkaline solution is 10~14.
Ferric arsenate/goethitum the material utilizing arsenic containing solution preparation to have nucleocapsid structure the most according to claim 1 realizes
Gu the method for arsenic, it is characterised in that: described precipitated ferric arsenate be immersed in alkaline solution reaction time be 1~24 hour.
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CN106834712A (en) * | 2016-12-21 | 2017-06-13 | 中南大学 | A kind of arsenic-containing smoke dust dearsenification and the method for the solid arsenic mineral of fractional crystallisation method synthesis |
CN106868320A (en) * | 2016-12-21 | 2017-06-20 | 中南大学 | A kind of preparation method of the solid arsenic mineral of high stability |
CN109626547A (en) * | 2018-12-26 | 2019-04-16 | 中南大学 | A method of using ferrous ion catalysis oxidation high concentration trivalent arsenic |
CN109761285A (en) * | 2019-03-14 | 2019-05-17 | 中南大学 | A kind of preparation method of the alkaline-resisting solid arsenic material of ferric arsenate@ferrous sulfide |
CN109847256A (en) * | 2019-04-17 | 2019-06-07 | 中南大学 | A kind of ferric arsenate@polymer consolidates the Arsenic fixation method of arsenic material and its preparation and arsenic containing solution |
CN114561558A (en) * | 2022-02-23 | 2022-05-31 | 中南大学 | Method for recovering antimony and solid arsenic from arsenic-containing crystal |
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CN106834712A (en) * | 2016-12-21 | 2017-06-13 | 中南大学 | A kind of arsenic-containing smoke dust dearsenification and the method for the solid arsenic mineral of fractional crystallisation method synthesis |
CN106868320A (en) * | 2016-12-21 | 2017-06-20 | 中南大学 | A kind of preparation method of the solid arsenic mineral of high stability |
CN109626547A (en) * | 2018-12-26 | 2019-04-16 | 中南大学 | A method of using ferrous ion catalysis oxidation high concentration trivalent arsenic |
CN109761285A (en) * | 2019-03-14 | 2019-05-17 | 中南大学 | A kind of preparation method of the alkaline-resisting solid arsenic material of ferric arsenate@ferrous sulfide |
CN109761285B (en) * | 2019-03-14 | 2019-12-24 | 中南大学 | Preparation method of ferric arsenate @ ferrous sulfide alkali-resistant arsenic-fixing material |
CN109847256A (en) * | 2019-04-17 | 2019-06-07 | 中南大学 | A kind of ferric arsenate@polymer consolidates the Arsenic fixation method of arsenic material and its preparation and arsenic containing solution |
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 |
CN114561558A (en) * | 2022-02-23 | 2022-05-31 | 中南大学 | Method for recovering antimony and solid arsenic from arsenic-containing crystal |
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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