CN108946819A - The stabilization method of scorodite - Google Patents
The stabilization method of scorodite Download PDFInfo
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- CN108946819A CN108946819A CN201810751143.4A CN201810751143A CN108946819A CN 108946819 A CN108946819 A CN 108946819A CN 201810751143 A CN201810751143 A CN 201810751143A CN 108946819 A CN108946819 A CN 108946819A
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- scorodite
- stabilization method
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D39/00—Filtering material for liquid or gaseous fluids
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Abstract
The invention discloses a kind of stabilization methods of scorodite, comprising the following steps: 1) mixes scorodite powder with acidic ferrous salt solution and heat, and be continually fed into oxidizing gas, obtain slurry；2) slurry is filtered, washed, dried, obtain the scorodite coated by hydrated ferric oxide.Scorodite stabilization method proposed by the present invention, by the way that scorodite is added into acid ferrous iron solution, oxidizing gas is continually fed into solution again hydrolyzes ferrous ions, and one layer of hydrated ferric oxide clad is deposited in scorodite particle surface, product stability with higher after being wrapped by can stablize stockpiling under acid, alkalinity, oxidisability and reductive condition.Simple process of the invention, easy to operate, the product strainability after cladding is good, and toxicity leaching concentration is very low, and the stable region pH is wide, can stablize stockpiling under alkalinity and reductive condition.
Description
Technical field
The present invention relates to the processing methods of scorodite, more particularly to a kind of stabilization method of scorodite.
Background technique
Molysite consolidates arsenic method and is divided into coprecipitation and scorodite method.So-called coprecipitation be will contain trivalent ferrous solution with containing arsenic it is molten
Liquid mixing is made iron be hydrolyzed to ferrihydrite, is fixed arsenic using adsorption effect of the ferrihydrite to arsenic by adjusting pH value；Furthermore also often
Generation water outlet arsenic iron ore is reacted with iron by arsenic and the mixture of ferric arsenate achievees the purpose that solid arsenic.This method biggest advantage is
The solid arsenic product stability arrived is high.But it inevitably the disadvantage is that molysite consumption is larger, general initial iron arsenic molar ratio is wanted
Greater than 3, and the obtained quantity of slag is larger.In addition, the solid arsenic slag cannot stable stockpiling under alkaline condition.In stockpiling process for a long time
In, the deep part in stockyard, since reproducibility atmosphere is often presented in anoxic, the pentavalent in solid arsenic slag that is co-precipitated at this time
Arsenic can be reduced to the biggish trivalent arsenic compound of solubility, to further can be discharged into environment.
Although scorodite is one of the most stable of compound being presently considered to, maximum defect is cannot be in alkali
Property and reductive condition under stablize stockpiling.According to previously reported, when pH is 2~6, the leaching concentration of As is lower than in scorodite
1mg/L.But under alkaline condition of the pH greater than 7 or under reductive condition, scorodite will discharge a large amount of arsenic, leach dense
Degree is up to 10~1000mg/L.In order to solve this problem, scientists are once attempted to coat smelly green onion using sodium metasilicate and aluminum phosphate
Stone, but effect is not obvious.Because of the anion SiO of clad4 3-And PO4 3-With the AsO in scorodite4 3-It will do it ion
Exchange, so that the release of arsenic is promoted, and after scorodite is wrapped by upper layer of gel, strainability will be substantially reduced,
It is more difficult during processing to be separated from solution.
Summary of the invention
In order to solve the technical issues of above-mentioned scorodite cannot stablize stockpiling under alkalinity and reductive condition, the present invention is mentioned
A kind of stabilization method of scorodite out.
Technical problem of the invention is resolved by technical solution below:
A kind of stabilization method of scorodite, comprising the following steps:
1) scorodite powder is mixed with acidic ferrous salt solution and is heated, and be continually fed into oxidizing gas, obtained
Slurry；
2) slurry is filtered, washed, dried, obtain the scorodite coated by hydrated ferric oxide.
Preferably, in step 1), the ferrous salt in the acidic ferrous salt solution include ferrous sulfate, frerrous chloride and
One of ferrous nitrate is a variety of.
Preferably, in step 1), the liquid-solid ratio of the acidic ferrous salt solution and the scorodite powder is 10~
100:1.
Preferably, in step 1), the pH value of the acidic ferrous salt solution is 0.5~2.0.
Preferably, in step 1), the concentration of the acidic ferrous salt solution is 0.1~1.0mol/L.
Preferably, in step 1), the oxidizing gas includes oxygen, air or oxygen-enriched air.
Preferably, in step 1), the rate that is passed through of the oxidizing gas is 1~20L/min.
Preferably, in step 1), the heating temperature is 50~100 DEG C.
Preferably, it is 250~500rpm that rate is kept stirring in the reaction process in step 1).
Preferably, in step 1), the reaction time be 5~for 24 hours.
It preferably, further include preparing acid ferrous salt solution before step 1).
In a preferred embodiment, a kind of stabilization method of scorodite is proposed, comprising the following steps:
1) scorodite powder is mixed with acidic ferrous salt solution and is heated, and be continually fed into oxidizing gas, obtained
Slurry.In the present embodiment, the ferrous salt in the acidic ferrous salt solution includes ferrous sulfate, frerrous chloride and ferrous nitrate
One of or it is a variety of；The pH value of the acidic ferrous salt solution is 0.5~2.0；The concentration of the acidic ferrous salt solution is
0.1~1.0mol/L；The oxidizing gas includes oxygen, air or oxygen-enriched air；The oxidizing gas is passed through rate
For 1~20L/min；The heating temperature is 50~100 DEG C；It is 250~500rpm that rate is kept stirring in reaction process；Reaction
Time be 5~for 24 hours.
2) slurry is filtered, washed, dried, obtain the scorodite coated by hydrated ferric oxide.
The beneficial effect of the present invention compared with the prior art includes: that scorodite stabilization method proposed by the present invention is to pass through
Scorodite is added into acid ferrous iron solution, then being continually fed into oxidizing gas into solution hydrolyzes ferrous ions, and
One layer of hydrated ferric oxide clad is deposited in scorodite particle surface, and product stability with higher after being wrapped by can be
Stablize stockpiling under acid, alkalinity, oxidisability and reductive condition.The hydration oxygen deposited using this method in scorodite particle surface
Changing iron is in crystalline state, and pattern is sheet, therefore obtained product has preferable strainability, and the product be conducive to is from molten
It is separated by filtration out in liquid.In addition, product leaches the raising of stability mainly using the physical isolation of clad, play to leaching
The suction-operated of " invasion " ion in solution and the arsenic of leaching and clad are hydrated ferric oxide and then change smelly green onion out
The dissolution equilibrium of stone inhibits the further leaching of arsenic.
Simple process of the invention, easy to operate, the product strainability after cladding is good, and toxicity leaching concentration is very low,
The stable region pH is wide, can stablize stockpiling under alkalinity and reductive condition.
Detailed description of the invention
Fig. 1 is the SEM figure of scorodite powder in the embodiment of the present invention 1.
Fig. 2 is the SEM figure of cladding product prepared by the embodiment of the present invention 1.
Fig. 3 is the STEM figure of cladding product prepared by the embodiment of the present invention 1.
Fig. 4 is the result figure of each element distribution of cladding product prepared by the embodiment of the present invention 1.
Specific embodiment
In order to make the foregoing objectives, features and advantages of the present invention clearer and more comprehensible, with reference to the accompanying drawing to the present invention
Specific embodiment be described in detail.Many details are explained in the following description in order to fully understand this hair
It is bright.But the invention can be embodied in many other ways as described herein, those skilled in the art can be not
Similar improvement is done in the case where violating intension of the present invention, therefore the present invention is not limited to the specific embodiments disclosed below.
It should be noted that the scorodite product coated by hydrated ferric oxide in the embodiment of the present invention is also referred to as coated and is produced
Object.
Embodiment 1
The present embodiment proposes a kind of stabilization method of scorodite, comprising the following steps:
The cladding of scorodite:
1) by Fe (II)-As (V)-O2-H2The scorodite powder 20g synthesized in O system is mixed with acidic ferrous salt solution
It is even to be heated, and it is continually fed into oxygen, reaction 5h obtains slurry.In the present embodiment, wherein the acidic ferrous salt solution
Liquid-solid ratio with the scorodite powder is 50:1；The volume of acidic ferrous salt solution is 1L, concentration 0.2mol/L, pH is
1.5；The rate that is passed through of the oxidizing gas is 1~20L/min；The heating temperature is 50~100 DEG C.
2) slurry is filtered, washed, dried, obtain the scorodite product coated by hydrated ferric oxide.
Further, in conjunction with the figure of scorodite powder different amplification in Fig. 1, it can be seen that scorodite powder is small
Particulate material made of grain stacks；It can be seen that in conjunction with the figure for coating product different amplification in Fig. 2 by hydrated ferric oxide
The scorodite surface of cladding is covered by laminated structure, illustrates that scorodite is coated by hydrated ferric oxide；In conjunction with transmission electron microscope picture
3, the model FEI-Titan G of transmission electron microscope260-300, from figure (a) therein to figure (c) it can be seen that scorodite is hydrated
Iron oxide cladding；In conjunction with Fig. 4, the result figure that (f) is the line scanning each element distribution of figure (e) in the direction of the arrow is schemed, it can from figure
To further illustrate that scorodite is coated by hydrated ferric oxide.
Toxicity leaches detection:
(1) toxicity leaching is carried out according to GB5085.3-2007 (solid waste judging standard-leaching characteristic identification), arsenic
Leaching concentration is less than 0.01mg/L, can safety and stability stockpiling much smaller than the limit value of the standard.
(2) consolidating mass ratio according to liquid is 20:1, is 9.3 by above-mentioned made 1g cladding powder product and 20mLpH value
NaOH solution mixing, is leached 10 days under the conditions of 25 DEG C, and the leaching concentration for measuring wherein arsenic is less than 0.01mg/L.
Embodiment 2
The scorodite product coated by hydrated ferric oxide is prepared according to the method for embodiment 1, wherein the concentration of ferrous sulfate
For 0.1mol/L, remaining condition is constant.
Toxicity leaches detection:
(1) toxicity leaching is carried out according to GB5085.3-2007 (solid waste judging standard-leaching characteristic identification), arsenic
Leaching concentration is less than 0.01mg/L, can safety and stability stockpiling much smaller than the limit value of the standard.
(2) consolidating mass ratio according to liquid is 20:1, is 9.3 by above-mentioned made 1g cladding powder product and 20mLpH value
NaOH solution mixing, is leached 10 days under the conditions of 25 DEG C, and the leaching concentration for measuring wherein arsenic is less than 0.01mg/L.
Embodiment 3
The scorodite product coated by hydrated ferric oxide is prepared according to the method for embodiment 1, wherein the concentration of ferrous sulfate
For 1.0mol/L, remaining condition is constant.
Toxicity leaches detection:
(1) toxicity leaching is carried out according to GB5085.3-2007 (solid waste judging standard-leaching characteristic identification), arsenic
Leaching concentration is less than 0.01mg/L, can safety and stability stockpiling much smaller than the limit value of the standard.
(2) consolidating mass ratio according to liquid is 20:1, is 8.6 by above-mentioned made 1g cladding powder product and 20mLpH value
NaOH solution mixing, is leached 10 days under the conditions of 25 DEG C, and the leaching concentration for measuring wherein arsenic is less than 0.01mg/L.
Embodiment 4
The scorodite product coated by hydrated ferric oxide is prepared according to the method for embodiment 1, wherein the concentration of ferrous sulfate
For 1.0mol/L, remaining condition is constant.
Toxicity leaches detection:
(1) toxicity leaching is carried out according to GB5085.3-2007 (solid waste judging standard-leaching characteristic identification), arsenic
Leaching concentration is less than 0.01mg/L, can safety and stability stockpiling much smaller than the limit value of the standard.
(2) consolidating mass ratio according to liquid is 20:1, is 9.3 by above-mentioned made 1g cladding powder product and 20mLpH value
NaOH solution mixing, is leached 10 days under the conditions of 25 DEG C, and the leaching concentration for measuring wherein arsenic is less than 0.01mg/L.
Embodiment 4
Prepare the scorodite product coated by hydrated ferric oxide according to the method for embodiment 1, wherein scorodite and solution
It is 10 that liquid, which consolidates mass ratio, remaining condition is constant.
Toxicity leaches detection:
(1) toxicity leaching is carried out according to GB5085.3-2007 (solid waste judging standard-leaching characteristic identification), arsenic
Leaching concentration is less than 0.01mg/L, can safety and stability stockpiling much smaller than the limit value of the standard.
(2) consolidating mass ratio according to liquid is 20:1, is 9.3 by above-mentioned made 1g cladding powder product and 20mLpH value
NaOH solution mixing, is leached 10 days under the conditions of 25 DEG C, and the leaching concentration for measuring wherein arsenic is less than 0.01mg/L.
Embodiment 6
Prepare the scorodite product coated by hydrated ferric oxide according to the method for embodiment 1, wherein scorodite and solution
It is 100 that liquid, which consolidates mass ratio, remaining condition is constant, obtains cladding product.
Toxicity leaches detection:
(1) toxicity leaching is carried out according to GB5085.3-2007 (solid waste judging standard-leaching characteristic identification), arsenic
Leaching concentration is less than 0.01mg/L, can safety and stability stockpiling much smaller than the limit value of the standard.
(2) consolidating mass ratio according to liquid is 20:1, is 9.3 by above-mentioned made 1g cladding powder product and 20mLpH value
NaOH solution mixing, is leached 10 days under the conditions of 25 DEG C, and the leaching concentration for measuring wherein arsenic is less than 0.01mg/L.
Embodiment 7
The scorodite product coated by hydrated ferric oxide is prepared according to the method for embodiment 1, and wherein oxygen-supply speed is 10L/
Min, remaining condition are constant.
Toxicity leaches detection:
(1) toxicity leaching is carried out according to GB5085.3-2007 (solid waste judging standard-leaching characteristic identification), arsenic
Leaching concentration is less than 0.01mg/L, can safety and stability stockpiling much smaller than the limit value of the standard.
(2) consolidating mass ratio according to liquid is 20:1, is 9.3 by above-mentioned made 1g cladding powder product and 20mLpH value
NaOH solution mixing, is leached 10 days under the conditions of 25 DEG C, and the leaching concentration for measuring wherein arsenic is less than 0.01mg/L.
Embodiment 8
The scorodite product coated by hydrated ferric oxide is prepared according to the method for embodiment 1, and wherein oxygen-supply speed is 20L/
Min, remaining condition are constant.
Toxicity leaches detection:
(1) toxicity leaching is carried out according to GB5085.3-2007 (solid waste judging standard-leaching characteristic identification), arsenic
Leaching concentration is less than 0.01mg/L, can safety and stability stockpiling much smaller than the limit value of the standard.
(2) consolidating mass ratio according to liquid is 20:1, is 9.3 by above-mentioned made 1g cladding powder product and 20mLpH value
NaOH solution mixing, is leached 10 days under the conditions of 25 DEG C, and the leaching concentration for measuring wherein arsenic is less than 0.01mg/L.
Embodiment 9
Prepare according to the method for embodiment 1 by hydrated ferric oxide coat scorodite product, wherein the reaction time be for 24 hours,
Remaining condition is constant.
Toxicity leaches detection:
(1) toxicity leaching is carried out according to GB5085.3-2007 (solid waste judging standard-leaching characteristic identification), arsenic
Leaching concentration is less than 0.01mg/L, can safety and stability stockpiling much smaller than the limit value of the standard.
(2) consolidating mass ratio according to liquid is 20:1, is 9.3 by above-mentioned made 1g cladding powder product and 20mLpH value
NaOH solution mixing, is leached 10 days under the conditions of 25 DEG C, and the leaching concentration for measuring wherein arsenic is less than 0.01mg/L.
Embodiment 10
Prepare according to the method for embodiment 1 by hydrated ferric oxide coat scorodite product, wherein the reaction time be for 24 hours,
Remaining condition is constant.
Toxicity leaches detection:
(1) toxicity leaching is carried out according to GB5085.3-2007 (solid waste judging standard-leaching characteristic identification), arsenic
Leaching concentration is less than 0.01mg/L, can safety and stability stockpiling much smaller than the limit value of the standard.
(2) consolidating mass ratio according to liquid is 20:1, is 9.3 by above-mentioned made 1g cladding powder product and 20mLpH value
NaOH solution mixing, is leached 10 days under the conditions of 25 DEG C, and the leaching concentration for measuring wherein arsenic is less than 0.01mg/L.
Embodiment 11
The scorodite product coated by hydrated ferric oxide is prepared according to the method for embodiment 1, the use of frerrous chloride is source of iron,
With hydrochloric acid tune pH value, remaining condition is constant.
Toxicity leaches detection:
(1) toxicity leaching is carried out according to GB5085.3-2007 (solid waste judging standard-leaching characteristic identification), arsenic
Leaching concentration is less than 0.01mg/L, can safety and stability stockpiling much smaller than the limit value of the standard.
(2) consolidating mass ratio according to liquid is 20:1, is 9.3 by above-mentioned made 1g cladding powder product and 20mLpH value
NaOH solution mixing, is leached 10 days under the conditions of 25 DEG C, and the leaching concentration for measuring wherein arsenic is less than 0.01mg/L.
Embodiment 12
The scorodite product coated by hydrated ferric oxide is prepared according to the method for embodiment 1, the use of ferrous nitrate is source of iron,
With nitric acid tune pH value, remaining condition is constant.
Toxicity leaches detection:
(1) toxicity leaching is carried out according to GB5085.3-2007 (solid waste judging standard-leaching characteristic identification), arsenic
Leaching concentration is less than 0.01mg/L, can safety and stability stockpiling much smaller than the limit value of the standard.
(2) consolidating mass ratio according to liquid is 20:1, is 9.3 by above-mentioned made 1g cladding powder product and 20mLpH value
NaOH solution mixing, is leached 10 days under the conditions of 25 DEG C, and the leaching concentration for measuring wherein arsenic is less than 0.01mg/L.
Embodiment 13
It is proposed that a kind of stabilization method of scorodite is same as Example 1 in the present embodiment.
Toxicity leaches detection:
Consolidating mass ratio according to liquid is 20:1, the NaOH for being 8.3 by above-mentioned made 1g cladding powder product and 20mLpH value
Solution mixing, is leached 10 days under the conditions of 25 DEG C, and the leaching concentration for measuring wherein arsenic is less than 0.01mg/L.
Embodiment 14
It is proposed that a kind of stabilization method of scorodite is same as Example 1 in the present embodiment.
Toxicity leaches detection:
Consolidating mass ratio according to liquid is 20:1, is 8.6 by above-mentioned made 1g cladding powder product and 20mLpH value
NaH2PO4The mixing of-NaOH buffer solution, is leached 10 days under the conditions of 25 DEG C, and the leaching concentration for measuring wherein arsenic is 1.8mg/L.
Embodiment 15
It is proposed that a kind of stabilization method of scorodite is same as Example 1 in the present embodiment.
Toxicity leaches detection:
Consolidating mass ratio according to liquid is 20:1, is 7.6 by above-mentioned made 1g cladding powder product and 20mLpH value, oxidation is also
Former potential (Eh) is the Na of -100~0mV2The mixing of S solution, is leached 10 days under the conditions of 25 DEG C, measures the leaching concentration of wherein arsenic
For 0.3mg/L.
Embodiment 16
It is proposed that a kind of stabilization method of scorodite is same as Example 1 in the present embodiment.
Toxicity leaches detection:
Consolidating mass ratio according to liquid is 20:1, is 8.1 by above-mentioned made 1g cladding powder product and 20mLpH value, oxidation is also
The Na2S solution that former potential (Eh) is -100~0mV mixes, and leaches 10 days under the conditions of 25 DEG C, measures the leaching concentration of wherein arsenic
For 0.9mg/L.
In conclusion the invention has the advantages that
(1) present invention process is simple, easy to operate, and used ferrous salt and oxygen are common material in metallurgical industry
Material, reaction condition is mild, low for equipment requirements.
(2) product of hydrated ferric oxide cladding scorodite prepared by the present invention, the big strainability of particle are good.
(3) product of hydrated ferric oxide prepared by the present invention cladding scorodite leaches that stability is high, pH be 2~7 it is weak
Under acid condition, the leaching concentration for coating arsenic in product is less than 0.01mg/L；In the case where pH is 7~11 alkaline condition, arsenic
Leaching concentration is less than 2mg/L；In addition, coating arsenic in product under the conditions of molten alkaline reduction (pH 8~10, Eh-100~0mV)
Leaching concentration be less than 1mg/L, lower than GB5085.3-2007 hazardous waste identify national Specification limit value (5mg/L).It can
Safety stockpiling.It solves scorodite and is difficult to stablize under alkalinity and reductive condition and store up this problem.
Unless otherwise defined, all technical and scientific terms used herein and the skill for belonging to technical field of the invention
The normally understood meaning of art personnel is identical, is intended merely to achieve the purpose that describe specific embodiment, it is not intended that in limiting this hair
It is bright.Each technical characteristic of embodiment described above can be combined arbitrarily, for simplicity of description, not in above-described embodiment
The all possible combination of each technical characteristic be all described, if however, there is no contradiction in the combination of these technical features,
It all should be considered as described in this specification.
The above content is a further detailed description of the present invention in conjunction with specific preferred embodiments, and it cannot be said that
Specific implementation of the invention is only limited to these instructions.For those skilled in the art to which the present invention belongs, it is not taking off
Under the premise of from present inventive concept, several equivalent substitute or obvious modifications can also be made, and performance or use is identical, all answered
When being considered as belonging to protection scope of the present invention.
Claims (10)
1. a kind of stabilization method of scorodite, which comprises the following steps:
1) scorodite powder is mixed with acidic ferrous salt solution and is heated, and be continually fed into oxidizing gas, obtain slurry；
2) slurry is filtered, washed, dried, obtain the scorodite coated by hydrated ferric oxide.
2. the method as described in claim 1, which is characterized in that the ferrous iron in step 1), in the acidic ferrous salt solution
Salt includes one of ferrous sulfate, frerrous chloride and ferrous nitrate or a variety of.
3. stabilization method as described in claim 1, which is characterized in that in step 1), the acidic ferrous salt solution with
The liquid-solid ratio of the scorodite powder is 10~100:1.
4. stabilization method according to claim 1-3, which is characterized in that described acid sub- in step 1)
The pH value of iron salt solutions is 0.5~2.0.
5. stabilization method according to claim 1-3, which is characterized in that described acid sub- in step 1)
The concentration of iron salt solutions is 0.1~1.0mol/L.
6. stabilization method according to claim 1, which is characterized in that in step 1), the oxidizing gas includes
Oxygen, air or oxygen-enriched air.
7. stabilization method according to claim 1, which is characterized in that in step 1), the oxidizing gas leads to
Entering rate is 1~20L/min.
8. stabilization method according to claim 1, which is characterized in that in step 1), the heating temperature be 50~
100℃。
9. stabilization method according to claim 1, which is characterized in that be kept stirring in the reaction process in step 1)
Rate is 250~500rpm.
10. stabilization method according to claim 1, which is characterized in that in step 1), the reaction time be 5~
24h。
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| CN108640157A (en) * | 2018-06-04 | 2018-10-12 | 云南云铜锌业股份有限公司 | A kind of heavy arsenic method of arsenic containing solution |
| CN113526563A (en) * | 2021-09-14 | 2021-10-22 | 赛恩斯环保股份有限公司 | Long-term stabilization treatment method for arsenic in arsenic-containing waste liquid |
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| 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 |
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| CN102421708A (en) * | 2009-05-13 | 2012-04-18 | 同和金属矿业有限公司 | Scorodite-type iron-arsenic compound particles, production method, and arsenic-containing solid |
| CN106830091A (en) * | 2016-12-21 | 2017-06-13 | 中南大学 | A kind of precipitation from arsenic containing solution obtains the method for leaching stability scorodite high |
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