CN110508233A - A kind of solidification and stabilization material and preparation method thereof for administering arsenic pollution - Google Patents
A kind of solidification and stabilization material and preparation method thereof for administering arsenic pollution Download PDFInfo
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- CN110508233A CN110508233A CN201910462753.7A CN201910462753A CN110508233A CN 110508233 A CN110508233 A CN 110508233A CN 201910462753 A CN201910462753 A CN 201910462753A CN 110508233 A CN110508233 A CN 110508233A
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- limonite
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
- B01J20/28057—Surface area, e.g. B.E.T specific surface area
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B09—DISPOSAL OF SOLID WASTE; RECLAMATION OF CONTAMINATED SOIL
- B09C—RECLAMATION OF CONTAMINATED SOIL
- B09C1/00—Reclamation of contaminated soil
- B09C1/08—Reclamation of contaminated soil chemically
Abstract
A kind of solidification and stabilization material and preparation method thereof for administering arsenic pollution, material include the mechanical activation limonite for being about 0.2 μm through the average grain diameter that mechanical activation obtains.Preparation method includes the following steps: step 1, and a certain amount of natural limonite is smashed or rough lapping is the biggish powdered limonite of granularity；Powdered limonite is sieved by step 2, obtains fine powder limonite；Fine powder limonite is placed in ball mill and carries out mechanical activation by step 3, and dehydrated alcohol is added as decentralized medium in mechanical activation process；Obtain the mechanical activation limonite that the average grain diameter is about 0.2 μm.
Description
Technical field
The present invention relates to a kind of solidification and stabilization materials and preparation method thereof for administering arsenic pollution, belong to soil remediation
Technical field.
Background technique
Arsenic (As) is a kind of toxic nonmetalloid, is often applied to the production of pesticide and alloy etc..Its with it is carcinogenic,
Teratogenesis, mutagenic effect, and be widely present in soil and groundwater, it is most common at present, most tight to public health harm
One of the pollutant of weight.It is announced according to World Health Organization official, global ten thousand populations at least more than 5000 are faced with region As
The threat of poisoning, such as Bangladesh, China, the U.S., India, Chile, Japan, Argentina, Canada, including China
Asian countries As threaten it is the most serious.
The increase of soil As concentration will affect the normal function of the ecosystem, and cause to plant, animal and human health
Greatly threaten.In addition, the As in polluted soil enters surrounding body the effects of can also eluting by runoff, infiltration, rainwater
(surface water and groundwater), to further threaten to human health.Currently, common heavy metal pollution of soil repairs skill
Art includes engineering soil moved in improve the original, phytoremediation, chemical leaching, electro reclamation, solidification and stabilization etc..Wherein, chemical stabilization is turned to solid
Change one kind of stabilization technology, there are the advantages such as at low cost, quick, small to soil fail, thus by domestic and international soil weight
The extensive concern in metallic pollution reparation field.The key of the technical application is selection economy, efficient stabilization material.
Currently, it is various for the adsorbent material of As in soil pollution and water pollution, and be mostly synthetic material, price is high
Expensive, practicability is not high, is not easy to realize large-scale production and application.
Summary of the invention
To make up deficiency existing for above-mentioned field, the present invention provides a kind of for administering the solidification and stabilization material of arsenic pollution
And preparation method thereof, this is used to administer the solidification and stabilization material of arsenic pollution using natural minerals as raw material, and cheap, this is used for
The preparation method for administering the solidification and stabilization material of arsenic pollution is simple, it is easy to accomplish large-scale production and application.
The invention is realized by the following technical scheme:
It is a kind of for administering the solidification and stabilization material of arsenic pollution, the average grain diameter including obtaining through mechanical activation is about
0.2 μm of mechanical activation limonite.Preferably, the mechanical activation limonite that the average grain diameter is about 0.2 μm, partial size are less than
1 μm of mechanical activation limonite accounts for the 95% of its gross mass in quality.Preferably, the mechanical activation limonite is in quality
On account for the 2%-10% of the soil quality containing As.
It is a kind of for administering the preparation method of the solidification and stabilization material of arsenic pollution, which comprises the steps of:
Step 1: a certain amount of natural limonite is smashed or rough lapping is the biggish powdered limonite of granularity；
Step 2: powdered limonite is sieved, and obtains fine powder limonite；
Step 3: fine powder limonite is placed in ball mill and carries out mechanical activation, and nothing is added in mechanical activation process
Water-ethanol is as decentralized medium；Obtain the mechanical activation limonite that the average grain diameter is about 0.2 μm.
Preferably, in step 3, the fine powder limonite mechanical activation 3-24 hours in the ball mill.
Preferably, the solid-to-liquid ratio of the fine powder limonite and the dehydrated alcohol is 5:4 (g:mL) in step 3.
Preferably, the ball material mass ratio of the ball mill is 10:1 in step 3.
Preferably, the ball mill is planetary ball mill, and ball grinding cylinder and abrading-ball are agate material in step 3
Matter, the abrading-ball are bead.
Preferably, in step 3, the revolution revolving speed 320r/min of the ball mill, rotation revolving speed 640r/min.
Preferably, the powdered limonite is crossed 200 meshes in step 2.
Preferably, in step 3, fine powder limonite mechanical activation 3h, 6h or 12h in the ball mill.
Advantage is the present invention compared with the existing technology:
1, present invention obtains a kind of for administering the solidification and stabilization material of arsenic pollution, including mechanical activation limonite,
It is 0.2-1 μm that mechanical activation limonite carries out the partial size after mechanical activation in the ball mill, reachable to the adsorption capacity of As (V)
8.26-8.34mg·g-1, to the adsorption capacity of As (III) up to 8.73-9.14mgg-1；
2, a kind of solidification and stabilization material for administering arsenic pollution of the present invention and preparation method thereof is with natural brown
Iron ore material is raw material, raw material contain it is abundant, it is cheap, it is readily available, and its finished product is compared to synthetic material, manufacture letter
It is single, it is easy to accomplish large-scale production.
3, of the present invention a kind of for administering the solidification and stabilization material of arsenic pollution, specific surface area is obviously mentioned
There are more amorphous phases in height, reduces crystallizable mineral degree, but mineral species do not change, and with natural brown iron
Mine is compared, and is obviously got a promotion to the absorption property of As.
4, mechanical activation limonite prepared by the present invention has apparent stabilization effect to As in As contaminated soil, stablizes
Change efficiency up to 78% or more, and the physicochemical properties such as soil pH value is influenced small.
5, a kind of preparation method for administering the solidification and stabilization material of arsenic pollution of the present invention is fairly simple, no
In the presence of complicated raw material and harsh synthesis condition, raw material is easy to get, and mechanical activation process is simple, without heating, withdrawing deposit, consumes
When it is short, but significantly improve limonite to the adsorption capacity of As.
Detailed description of the invention
Fig. 1 is transmission electron microscope (TEM) figure of mechanical activation limonite；
Fig. 2 is that fine powder limonite changes from the X difraction spectrum (XRD) of the mechanical activation limonite of different mechanical activation times
Figure；
Fig. 3 is the mechanical activation limonite (H2) after the fine powder limonite (H1) without mechanical activation and mechanical activation 12h
FTIR spectrogram；
Fig. 4 is the mechanical activation limonite (H2) after the fine powder limonite (H1) without mechanical activation and mechanical activation 12h
To the influence diagram of soil available As content.
Specific embodiment
Embodiment 1
It is a kind of for administering the solidification and stabilization material of arsenic pollution, the average grain diameter including obtaining through mechanical activation is about
0.2 μm of mechanical activation limonite.Specifically, when the average grain diameter of the mechanical activation limonite is 0.2 μm or so, wherein grain
It accounts for the 95% of its total amount (quality meter) to mechanical activation limonite particle of the diameter less than 1 μm, and wherein the content of Fe element is
63.8%, the phase constituent of object containing goethite, grain graininess is uniform, crystallinity is low, at this point, reaching best to the adsorption capacity of As.Its is right
The adsorption capacity of As (V) is up to 8.26-8.34mgg-1, to the adsorption capacity of As (III) up to 8.73-9.14mgg-1。
Embodiment 2
It is a kind of for administering the preparation method of the solidification and stabilization material of arsenic pollution, include the following steps:
Step 1: choosing iron content in the natural limonite of 60-70%, is smashed and rough lapping is the biggish powder of granularity
Last shape limonite；
Step 2: powdered limonite is sieved, and obtains fine powder limonite；
Step 3: fine powder limonite is placed in meter river in Henan Province YXQM-2L type planetary ball mill and carries out mechanical activation, ball milling
Cylinder and abrading-ball choose agate material, and abrading-ball chooses bead, and ratio of grinding media to material is set as 10:1, and the revolution revolving speed of ball mill is set as 320r/
Min, rotation revolving speed are set as 640r/min；
And dehydrated alcohol being added in mechanical activation process as decentralized medium, fine powder limonite and dehydrated alcohol are consolidated
Liquor ratio is 5:4 (g:mL)；Fine powder limonite is subjected to mechanical activation 3-24h in the ball mill, obtaining the average grain diameter is about
0.2 μm of mechanical activation limonite.
From transmission electron microscope (TEM) figure of mechanical activation limonite shown in FIG. 1 as can be seen that in the brown iron of the mechanical activation
The minimum grain size of mine can be reduced to 100nm hereinafter, material is in aggregating state simultaneously, and granular size is uneven.And mechanical activation is brown
The average grain diameter of iron ore is lower, and specific surface area is bigger, can be obviously improved the adsorption capacity to As.
X difraction spectrum (XRD) phenogram of mechanical activation limonite as shown in Figure 2, analysis is it is found that with machine in for 24 hours
Tool activates the lengthening that limonite carries out the mechanical activation time, goethite characteristic peak weakened, and diffraction maximum increases, crystallizable mineral degree
It reduces, changes to weak crystalloid, and do not occur new span, there are certain coherent conditions between particle.
Embodiment 3
It is a kind of for administering the preparation method of the solidification and stabilization material of arsenic pollution, include the following steps:
Step 1: choosing iron content in the natural limonite of 60-70%, is smashed and rough lapping is the biggish powder of granularity
Last shape limonite；
Step 2: powdered limonite is crossed into 200 meshes, obtains fine powder limonite；
Step 3: fine powder limonite is placed in meter river in Henan Province YXQM-2L type planetary ball mill and carries out mechanical activation, ball milling
Cylinder and abrading-ball choose agate material, and abrading-ball chooses bead, and ratio of grinding media to material is set as 10:1, and the revolution revolving speed of ball mill is set as 320r/
Min, rotation revolving speed are set as 640r/min；
And dehydrated alcohol is added in mechanical activation process as decentralized medium, the fine powder limonite and the anhydrous second
The solid-to-liquid ratio of alcohol is 5:4 (g:mL)；By fine powder limonite mechanical activation 12h in the ball mill, obtaining the average grain diameter is
0.214 μm of mechanical activation limonite.At this point, with the growth of mechanical activation time, due to the brown iron of agglomeration mechanical activation
The average grain diameter of mine increases.
It is specific:
As shown in table 1, after mechanical activation 12h, the partial size of natural fine powder limonite is reduced to mechanical work by 16.848 μm
0.214 μm for changing limonite, specific surface area is by 10.257m2/ g is increased to 56.744m2/g.Mechanical activation limonite specific surface area
It is significantly improved, adsorption capacity also enhances with the raising of specific surface area.Fine powder limonite and mechanical activation as shown in Figure 3
The FTIR comparison chart of limonite it is found that mechanical activation limonite compared with the fine powder limonite without mechanical activation, due to machinery
The variation of chemical composition is not caused in activation process, so the position of absorption band has almost no change.To with fine powder limonite,
After mechanical activation 12h, in 895cm-1The hydroxyl O-H flexural vibrations peak at place enhances, in 3698cm-1It is flexible that hydroxyl O-H occurs in place
Vibration absorption peak, 3101cm-1Locate the enhancing of goethite characteristic peak, so after carrying out mechanical activation, mechanical activation limonite material table
Significantly increase in the site O-H in face.
The mechanical activation limonite of 1 mechanical activation 12h of table is compared with the fine powder limonite fundamental characteristics without mechanical activation
Table
Note: H1: the fine powder limonite without mechanical activation；H2: mechanical activation 12h mechanical activation limonite.Institute below
The H1 and H2 shown is identical as content shown in this table.
Respectively using the pure Na of chemistry3AsO4·12H2O and NaAsO2It is configured to various concentration As (V) and As (III) solution.
Mechanical activation limonite (H2) after taking the fine powder limonite (H1) without mechanical activation and mechanical activation 12h respectively
0.20g, be added thereto concentration gradient be 0,5,10,20,40,60,80, As (III) the solution 25mL of 100mg/L (material
Solid-to-liquid ratio is 8g/L), adjusting solution system pH is 7.0, back-ground electolyte 0.01mol/LNaNO3, in 25 DEG C, 200r/min
Under the conditions of sustained oscillation 20h, centrifugal filtration takes the concentration difference of supernatant measurement material absorption front and back As solution, and retains reaction
Material afterwards, to determine that material changes the adsorption capacity of As (III).And 3 repetitions are set and are tested.Material is not added in setting simultaneously
Blank control.Isothermal adsorption analysis is carried out to experimental configuration.The results are shown in Table 3 for analysis.Absorption etc. of the material to As (III)
Warm line such as table 2.As shown in Table 2, mechanical activation limonite is without mechanical activation to the adsorption capacity of As up to 8.73mg/g
4.18 times of fine powder limonite, and it is higher than natural iron-bearing mineral conventional at present.
Suction of the mechanical activation limonite of fine powder limonite and mechanical activation 12h of the table 2 without mechanical activation to As (III)
Attached isotherm data
Note: H1: the fine powder limonite without mechanical activation；H2: mechanical activation 12h mechanical activation limonite.
Mechanical activation limonite (H2) after taking the fine powder limonite (H1) without mechanical activation and mechanical activation 12h respectively
0.20g, be added thereto concentration gradient be 0,5,10,20,40,60,80, (material is consolidated by As (V) the solution 25mL of 100mg/L
Liquor ratio is 8g/L), adjusting solution system pH is 7.0, back-ground electolyte 0.01mol/LNaNO3, in 25 DEG C, 200r/min item
Persistent oscillation 20h under part, after reaction terminating.Adsorption isotherm such as table 3 of the material to As (V).As shown in Table 3, after mechanical activation
Natural limonite to the adsorption capacity of As (V) up to 8.34mg/g, be 2.79 times of the fine powder limonite without mechanical activation,
And it is higher than natural iron-bearing mineral conventional at present.
Absorption of the mechanical activation limonite of fine powder limonite and mechanical activation 12h of the table 3 without mechanical activation to As (V)
Isotherm data
Note: H1: the fine powder limonite without mechanical activation；H2: mechanical activation 12h mechanical activation limonite.
Embodiment 4
Respectively by the mechanical activation limonite (H2) after the fine powder limonite (H1) without mechanical activation and mechanical activation 12h
It is added in As contaminated soil according to a certain percentage, blank control: containing NaHCO in As contaminated soil3Extract the ratio of state As
For 1.07 ± 0.05mg/kg.Take 2 respectively, 5, the mechanical activation limonite after 10g mechanical activation 12h be added to 100g As it is dirty
It contaminates in soil, after being sufficiently mixed, under the conditions of adjusting soil moisture content reaches field capacity, seals triangle with hydrophobic permeable membrane
Bottle, continuous culture reach stable to adsorption effect.The NaHCO of As contaminated soil after stabilisation3Extract state As content (available state As
Content) variation is as shown in Figure 4.As shown in Figure 4, the natural limonite after mechanical activation is aobvious to the stabilization effect of soil arsenic pollution
Enhancing is write, and when mechanical activation limonite addition quality is 5~10% of the soil quality containing As, NaHCO can be made3Extract state
Arsenic concentration drops to 0.31 ± 0.020mg/kg~0.23 ± 0.07mg/kg by 1.07 ± 0.05mg/kg, stabilizes efficiency and reaches
71.18%~78.45%, it is 1.7~2.2 times of the natural limonite of non-mechanical activation, and be substantially better than at present that remaining is natural
Iron-bearing mineral.
It should be pointed out that specific embodiment described above can make those skilled in the art that this hair be more fully understood
It is bright, but do not limit the invention in any way.Therefore, although this specification referring to drawings and examples to present invention has been
Detailed description, it will be understood by those skilled in the art, however, that still can modify or equivalently replace the present invention,
In short, all do not depart from the technical solution and its change of the spirit and scope of the present invention, should all cover in protection of the invention
In range.
Claims (11)
1. a kind of for administering the solidification and stabilization material of arsenic pollution, which is characterized in that be averaged including what is obtained through mechanical activation
The mechanical activation limonite that partial size is about 0.2 μm.
2. according to claim 1 a kind of for administering the solidification and stabilization material of arsenic pollution, which is characterized in that described flat
The mechanical activation limonite that equal partial size is about 0.2 μm, mechanical activation limonite of the partial size less than 1 μm account for its total matter in quality
The 95% of amount.
3. according to claim 1 a kind of for administering the solidification and stabilization material of arsenic pollution, which is characterized in that the machine
Tool activation limonite accounts for the 2%-10% of the soil quality containing As in quality.
4. a kind of for administering the preparation method of the solidification and stabilization material of arsenic pollution, which comprises the steps of:
Step 1: a certain amount of natural limonite is smashed or rough lapping is the biggish powdered limonite of granularity；
Step 2: powdered limonite is sieved, and obtains fine powder limonite；
Step 3: fine powder limonite being placed in ball mill and carries out mechanical activation, and anhydrous second is added in mechanical activation process
Alcohol is as decentralized medium；Obtain the mechanical activation limonite that the average grain diameter is about 0.2 μm.
5. according to claim 4 a kind of for administering the preparation method of the solidification and stabilization material of arsenic pollution, feature
It is, in step 3, the fine powder limonite mechanical activation 3-24 hours in the ball mill.
6. it is according to claim 4 or 5 a kind of for administering the preparation method of the solidification and stabilization material of arsenic pollution, it is special
Sign is, in step 3, the solid-to-liquid ratio of the fine powder limonite and the dehydrated alcohol is 5:4 (g:mL).
7. according to claim 4 a kind of for administering the preparation method of the solidification and stabilization material of arsenic pollution, feature
It is, in step 3, the ball material mass ratio of the ball mill is 10:1.
8. according to claim 4 a kind of for administering the preparation method of the solidification and stabilization material of arsenic pollution, feature
It is, in step 3, the ball mill is planetary ball mill, and ball grinding cylinder and abrading-ball are agate material, and the abrading-ball is
Bead.
9. according to claim 4 a kind of for administering the preparation method of the solidification and stabilization material of arsenic pollution, feature
It is, in step 3, the revolution revolving speed 320r/min of the ball mill, rotation revolving speed 640r/min.
10. according to claim 4 a kind of for administering the preparation method of the solidification and stabilization material of arsenic pollution, feature
It is, in step 2, the powdered limonite is crossed into 200 meshes.
11. it is according to claim 4 a kind of for administering the preparation method of the solidification and stabilization material of soil arsenic pollution,
It is characterized in that, in step 3, fine powder limonite mechanical activation 3h, 6h or 12h in the ball mill.
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