CN108033540A - A kind of method that crystalline substance glue load nano zero-valence iron composite material removes heavy metal chromium - Google Patents
A kind of method that crystalline substance glue load nano zero-valence iron composite material removes heavy metal chromium Download PDFInfo
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- CN108033540A CN108033540A CN201711075573.0A CN201711075573A CN108033540A CN 108033540 A CN108033540 A CN 108033540A CN 201711075573 A CN201711075573 A CN 201711075573A CN 108033540 A CN108033540 A CN 108033540A
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- Prior art keywords
- composite material
- nano zero
- valence iron
- brilliant glue
- chromium
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/70—Treatment of water, waste water, or sewage by reduction
- C02F1/705—Reduction by metals
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
- C02F2101/22—Chromium or chromium compounds, e.g. chromates
Abstract
The invention discloses a kind of method that brilliant glue load nano zero-valence iron composite material removes heavy metal chromium.This method is to add brilliant glue load nano zero-valence iron composite material into chromium solution, is reacted.The brilliant glue load nano zero-valence iron composite material of the present invention had both maintained the super large pore structure of brilliant glue, the reactivity of nano zero valence iron is improved again, so that nano zero valence iron distribution of particles is on brilliant glue duct and surface, prevent intergranular reunion, it can effectively realize the efficient process of pollution of chromium in environment water, can be widely applied to environment field for the treatment of of water pollution.
Description
Technical field
The present invention relates to a kind of method that brilliant glue load nano zero-valence iron composite material removes heavy metal chromium.
Background technology
Heavy metal chromium derives from a wealth of sources, and such as plating, process hides, pharmacy, printing and dyeing industry discharge substantial amounts of chromate waste water and enter ring
Border, directly results in the serious pollution of water body.Data shows that leather industry processing 1t raw hides, to discharge containing chromium is the useless of 410mg/L
Water 50-60t；Content of 6-valence Cr ions higher in electroplating wastewater of chromium, when especially changing electroplate liquid, usually discharges a large amount of high concentrations and contains chromium
Waste water.Existence form mainly has Cr VI (Cr (VI)) and trivalent chromium (Cr (III)) to chromium in water, the two is with entirely different
Chemical feature and bio-toxicity, and can mutually convert under certain condition.Cr (III) is primarily present in reproducibility, weak acid
Property under the conditions of, in water easily with other materials formed complex compound and be stable in the presence of in deposit；Cr (VI) is in any pH value
Under in soluble state and being stabilized.The toxicity of wherein Cr (VI) is at least 100 times of Cr (III)；A small amount of contact can draw
Uncomfortable schneiderian membrane, ulcer or perforation of nasal septum are played, long-term, high-dose contacts the damage that can cause kidney, liver, or even induces cancer
Disease.Exceeded Cr VI in the environment will not natural degradation, will in the environment accumulate and damage to organism.It is in consideration of it, beautiful
Cr (VI) is determined as one of toxicant of 17 kinds of highly dangerous by Bureau for Environmental Protection of state (EPA).China is also by chromium and its chemical combination
Thing is planned to priority pollutants ranks, and Cr VI is the first pollutant in industrial wastewater discharge standard.China
The content of Cr (VI) must not exceed in clear stipulaties water body in standards for drinking water quality and water environment quality standard
0.05mg/L。
There is a variety of the minimizing technology of Cr (VI), the conventional method of domestic and international processing waste water containing chrome mainly has chemistry to sink in water body
Shallow lake method, absorption method, ion-exchange, UF membrane and biological treatment etc., these methods have obtained certain progress under study for action,
But still there are produced in processing procedure a large amount of chromium-bearing sludges, easily cause secondary pollution, cost is excessive, stability is bad etc. asks
Topic.
In recent years, nano zero valence iron (nZVI) is because of its special nanostructured, higher reactivity and stronger reduction
Ability and be widely used in Cr (VI) removal research in；The big Cr of toxicity (VI) can be reduced to toxicity by nano zero valence iron
Small Cr (III), then enables Cr (III) that precipitation reaction occurs and removes.Exactly because however, specific surface area big nZVI and
Surface energy, and its distinctive magnetism, cause nZVI easily to reunite and aoxidize, so as to generate larger particle, drop significantly
Low its reactivity and reducing power.
NZVI is loaded on some carriers (such as：Zeolite, montmorillonite, bentonite, activated carbon etc.) study on the modification one
Determine to improve the reunion situation of nZVI in degree, enhance its reactivity；But these modified materials are still in powder
Shape, applied to being not readily separated in wastewater treatment process, forms a large amount of sludge, and is easy to run off, and secondary pollution is most probably caused, to ring
Border and human health constitute a serious threat.In order to prevent the reunion of nano zero-valence iron particle, its reactivity, and energy are improved
Avoid the loss of nZVI particles and give up, it is necessary to select other new carrier materials to solve nano zero-valence iron particle in processing containing chromium
Problem present in water.
The content of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of easy to operate, reactivity height, without secondary
Pollution, light, small, the brilliant glue load nano zero-valence iron composite material of environmental sound, and this brilliant glue load is provided and is received
The method that rice zero-valent iron composite material removes heavy metal chromium.
The technical solution used in the present invention is：
A kind of method that crystalline substance glue load nano zero-valence iron composite material removes heavy metal chromium, is that brilliant glue is loaded nano zero-valence
Iron composite material is added into chromium solution, is reacted.
The pH value range of chromium solution is 2~12.
The concentration of Cr is 40mg/L~60mg/L in chromium solution.
The mass ratio of brilliant glue load nano zero-valence iron composite material and Cr in chromium solution is (1.8~7.5)：1.
In brilliant glue load nano zero-valence iron composite material, the load capacity of nano zero valence iron is the 3%~15% of brilliant colloid amount.
The preparation method of brilliant glue load nano zero-valence iron composite material comprises the following steps：
1) by ferrous salt solution and brilliant glue hybrid reaction, brilliant glue-Fe is obtained2+Material；
2) by brilliant glue-Fe2+After material clean, reacted with reducing agent solution, then through over cleaning, drying, obtains brilliant glue load
Nano zero-valence iron composite material.
Brilliant glue is sodium acrylate crystalline substance gel matrix.
In the preparation method step 1) of brilliant glue load nano zero-valence iron composite material, ferrous salt is ferrous sulfate.
In the preparation method step 1) of brilliant glue load nano zero-valence iron composite material, reducing agent is sodium borohydride.
Remove in heavy metal chromium method, the time of reaction is 2h~5h.
The beneficial effects of the invention are as follows：
The brilliant glue load nano zero-valence iron composite material of the present invention had not only maintained the super large pore structure of brilliant glue, but also improved and receive
The reactivity of rice Zero-valent Iron so that nano zero valence iron distribution of particles prevents intergranular reunion on brilliant glue duct and surface,
It can effectively realize the efficient process of pollution of chromium in environment water, can be widely applied to environment field for the treatment of of water pollution.
Specifically, method of the invention has the following advantages relative to the conventional process of chromium：
1st, use super-macroporous crystal gel matrix to prevent nano zero valence iron particle agglomeration for support modification nano zero valence iron, limit
Its indeterminate growth, forms particle size smaller, the zero-valent iron particle of reactivity higher, can efficiently remove the heavy metal in water body
Chromium, operating process are simple；
2nd, the scope of application of pH value is wide in range (4~12)；
3rd, brilliant glue load nano zero-valence iron composite material has solution ph certain regulating power (to maintain 8~10 models
Enclose), avoid the process that industry removes first acidifying reduction Re-boostering test precipitation during chromium；
4th, the composite material of freeze-drying can preserve the several months, still keep high reactivity；
5th, the composite material of freeze-drying is in small bulk, and swelling behavior is good, light, small, can be applied to ambient water dirt
The emergency processing of dye and permeable reactive barrier technology, easy to recycling.
Brief description of the drawings
Fig. 1 is comparison figure of the different materials to chromium removal effect；
Fig. 2 is the dynamics figure that different materials remove Cr VI and total chromium；
Fig. 3 be under different pH value composite material to the removal effect figure of Cr VI and total chromium；
Fig. 4 is the residual spirogram of trivalent chromium under different pH value；
Fig. 5 is the variation diagram of chromium solution system pH before and after reaction；
Fig. 6 is the dissolution spirogram of nano zero valence iron in different pH value chromium solution systems.
Embodiment
A kind of method that crystalline substance glue load nano zero-valence iron composite material removes heavy metal chromium, is that brilliant glue is loaded nano zero-valence
Iron composite material is added into chromium solution, is reacted.
Preferably, the pH value range of chromium solution is 2~12.
Preferably, the concentration of Cr is 40mg/L~60mg/L in chromium solution.
Preferably, the mass ratio of brilliant glue load nano zero-valence iron composite material and Cr in chromium solution is (1.8~7.5)：1.
Preferably, in brilliant glue load nano zero-valence iron composite material, the load capacity of nano zero valence iron is the 3% of brilliant colloid amount
~15%；It is further preferred that in brilliant glue load nano zero-valence iron composite material, the load capacity of nano zero valence iron is brilliant colloid amount
3.5%~13.3%.
The preparation method of brilliant glue load nano zero-valence iron composite material comprises the following steps：
1) by ferrous salt solution and brilliant glue hybrid reaction, brilliant glue-Fe is obtained2+Material；
2) by brilliant glue-Fe2+After material clean, reacted with reducing agent solution, then through over cleaning, drying, obtains brilliant glue load
Nano zero-valence iron composite material.
Preferably, brilliant glue is sodium acrylate crystalline substance gel matrix.
Preferably, in the preparation method step 1) of brilliant glue load nano zero-valence iron composite material, ferrous salt is ferrous sulfate.
Preferably, in the preparation method step 1) of brilliant glue load nano zero-valence iron composite material, reducing agent is sodium borohydride.
Sodium acrylate crystalline substance gel matrix and sodium acrylate crystalline substance glue load nano zero-valence iron composite material preparation method referring to
Preparation method disclosed in a kind of preparation methods of nano zero valence iron of CN105499604A.
Preferably, remove in heavy metal chromium method, the time of reaction is 2h~5h.
Present disclosure is described in further detail below by way of specific embodiment.
The preparation of brilliant glue load nano zero-valence iron composite material
Reference《A kind of preparation method of nano zero valence iron》(CN105499604A) method disclosed in prepares brilliant glue load
Nano zero-valence iron composite material.
Acrylic acid nano-crystal gel matrix (PSA) is prepared using low temperature gelation technology.
Weigh ferrous sulfate heptahydrate and prepare presoma Fe2+Ion concentration is respectively the solution of 20mM, 30mM, 40mM, 50mM
200mL, the 20 pieces of PSA prepared crystalline substances glue (mould of the brilliant glue of preparation is consistent, and the quality of every piece of brilliant glue is 0.0702g) are added
To above-mentioned Fe2+In solion, 150r/min constant-temperature tables reaction 24h is placed in so that Fe2+Ion and the Na in brilliant glue+Ion
Ion-exchange reactions fully occurs, PSA-Fe is prepared2+。
The PSA-Fe that will be prepared2+Brilliant glue material is cleaned with a large amount of deionized waters and is placed in there-necked flask, is then prepared
100mL sodium borohydride solutions, are added dropwise in there-necked flask under nitrogen atmosphere protection, are further continued for reacting after completion of dropwise addition
0.5h, a large amount of deionized deoxygenated water cleanings, freeze-drying obtain brilliant glue load nano zero-valence iron composite material (PSA-nZVI).
The brilliant glue load nano zero-valence iron composite material numbering being prepared be PSA-nZVI-20, PSA-nZVI-30,
PSA-nZVI-40, PSA-nZVI-50, correspond to presoma Fe respectively2+The concentration of ion is respectively 20mM, 30mM, 40mM, 50mM.
The measure of nano zero-valence iron content in composite material
It is specific as follows by the content of nano zero valence iron in chemical Determination by Stripping different loads amount composite material：
The HCl solution 50mL of 5M is pipetted in 100mL conical flasks (three groups of Duplicate Samples), by prepare one block of composite material
It is added in HCl, reacts 12h in 150r/min, 25 DEG C of constant-temperature table；After reaction, 0.45 μm of fiber filter was sampled
Film, atomic absorption detecting iron concentration after 50 times of dilution, finally calculates to obtain nano zero valence iron in every piece of dry brilliant glue according to formula (1)
Content.
In formula (1), c represents the concentration (mg/L) for the iron ion that Atomic absorption measures, and V represents the volume (50mL) of HCl, m
Represent the quality (0.0702g) of brilliant glue.
Table 1 is the content and thermal gravimetric analysis results of nano zero valence iron in composite material prepared by different precursor concentrations.From
In table 1 as can be seen that with the increase of precursor concentration, the content increase of nano zero valence iron, the results show in composite material
It is consistent with thermogravimetric residual quantity to learn leaching analysis result.
The content and thermal gravimetric analysis results of nano zero valence iron in composite material prepared by the different precursor concentrations of table 1
Note：In table 1, PSA cryogel, that is, acrylic acid nano-crystal glue, a represent the nZVI contents that chemical leaching obtains；B tables
Show the result that thermogravimetric obtains；C indicate without.
Test of the material to chromium removal effect in water body
Different materials are subjected to contrast test to chromium removal effect in water body, it is specific as follows：
The concentration of six parts of (every part of three groups of Duplicate Samples) 50mL is taken to be placed in for 50mg/L chromium solutions in 100mL conical flasks, respectively
Add 0.018g nZVI (equivalent to the content of nZVI in two pieces of PSA-nZVI-40), two pieces of PSA crystalline substances glue, two pieces of PSA-nZVI-
20th, two pieces of PSA-nZVI-30, two pieces of PSA-nZVI-40, two pieces of PSA-nZVI-50, are placed in 150r/min, 25 DEG C of constant temperature shakes
3h is reacted in bed；After reaction, 0.45 μm of fibrous filter membrane was sampled, Atomic absorption surveys total chromium concn after diluting certain multiple,
And total chromium removal rate is calculated with formula (2) and formula (3) respectively and removes capacity.
In formula (2) and formula (3), C0Represent the initial concentration (50mg/L) of chromium, CiRepresent total chromium concn of atomic absorption detecting
(mg/L)；In formula (3), V represents chromium solution volume (50mL), and m represents the content (g) of nano zero valence iron in every kind of material.
Attached drawing 1 is comparison figure of the different materials to chromium removal effect.As shown in Figure 1, composite material (PSA-nZVI-40) is right
The removal rate of chromium is better than nano zero valence iron (consistent with zeroth order iron content in PSA-nZVI-40) and PSA crystalline substance glue；As load capacity increases
Add, removal rate increases；When precursor concentration is 40mM, composite material is best to the removal effect of chromium, and up to 90%.Cause
This, does follow-up test using the composite material prepared under this concentration conditions.
The dynamics research that material removes chromium
Different materials remove chromium and carry out dynamics research, it is specific as follows：
The concentration of 11 parts of (every part of three groups of Duplicate Samples) 50mL is taken to be placed in for 50mg/L chromium solutions in 100mL conical flasks, respectively
0.018g nZVI, two blocks of PSA-nZVI-40 composite materials are added, is placed in 150r/min, 25 DEG C of constant-temperature table and reacts, point
Not in 10min, 20min, 30min, 60min, 90min, 120min, 180min, 240min, 360min, 720min, 1440min
0.45 μm of fibrous filter membrane was sampled, the total chromium concn of atomic absorption detecting after acidifying, spectrophotometric determination hexavalent chromium concentration.With standard
120min experimental datas before first _ order kinetics equation simulation reaction, shown in pseudo-first-order kinetics equation such as formula (4).
In formula (4), C0Represent the initial concentration (50mg/L) of chromium, CtRepresent the chromium concn (mg/L) of t moment, kobsIt is ln
(ct/c0)-t slope.
Attached drawing 2 is the dynamics figure that different materials remove Cr VI and total chromium.Composite material is to sexavalence as can be seen from Figure 2
The removal effect of chromium and total chromium is better than nano zero valence iron.Table 2 is to use pseudo-first-order kinetics equation fitting result.
2 pseudo-first-order kinetics equation fitting result of table
It was found from the pseudo-first-order dynamics fitting result listed from table 2, composite material is to receive except the observed rate constant of chromium
1.5 times of rice Zero-valent Iron, illustrate that the presence of brilliant gel matrix does not have an impact nano zero valence iron and the mass transport process of chromium reaction, and
Improve the reactivity of nano zero valence iron.
PH value removes composite material the influence of heavy metal chromium
The influence that pH value removes composite material heavy metal chromium is probed into, it is specific as follows：
The concentration for preparing 50mL is 50mg/L chromium solutions, and it is respectively 2,4,6,8,10,12 to adjust pH value, adds two pieces of PSA-
NZVI-40 composite materials, are placed in reacting 3h in 150r/min, 25 DEG C of constant-temperature table, sampled film after reaction, and survey
The pH value of system after fixed reaction, and become with the pH value of nano zero valence iron reaction system and turn to control.
Attached drawing 3 is that for composite material to the removal effect figure of Cr VI and total chromium, attached drawing 4 is under different pH value under different pH value
The residual spirogram of trivalent chromium.From figs. 3 and 4 it can be seen that in wide in range pH value range, composite material is to Cr VI and total chromium
Removal efficiency keep higher level；When pH value is 12, effect slightly reduces, and the trivalent chromium precipitation mainly formed is again
Caused by dissolving, cause remaining trivalent chromium concentration rise in solution.
Attached drawing 5 is the variation diagram of chromium solution system pH before and after reaction.Solution in composite system as can be seen from Figure 5
PH value maintain in metastable scope (8~10), and the pH value of nano zero valence iron system change it is then bigger, illustrate answer
Condensation material has the pH value of chromium solution system certain adjustment effect, maintains it and is conducive to the scope that trivalent chromium precipitates
It is interior, improve the removal effect of total chromium.
The stability of brilliant glue load nano zero valence iron in the reaction system
The stability of brilliant glue load nano zero valence iron in the reaction system is probed into, it is specific as follows：
The concentration for preparing 50mL is 50mg/L chromium solutions, and it is respectively 2,4,6,8,10,12 to adjust pH value, adds two pieces of PSA-
NZVI-40 composite materials, are placed in reacting 3h in 150r/min, 25 DEG C of constant-temperature table, sampled film, atom after reaction
Absorption measurement iron concentration.Attached drawing 6 is the dissolution spirogram of nano zero valence iron in different pH value chromium solution systems.Can be with from Fig. 6
Find out, when pH value range is 4~12, the iron ion of dissolution can be neglected in solution, far smaller than Drinking Water in China regulation
Iron concentration.So under field conditions (factors), brilliant glue load nano zero-valence iron composite material is relatively stable, reduces nanometer
The loss of Zero-valent Iron, avoids secondary pollution.
Experiment and research to sum up is understood：1st, the composite material counterweight being prepared when precursor concentration of the present invention is 40mM
The removal effect of crome metal is best；2nd, for compared to nano zero-valence iron particle, brilliant glue loads nano zero-valence iron composite material counterweight
Crome metal has high removal efficiency, and the super large pore structure of brilliant gel matrix causes composite material during the reaction without mass transfer
Resistance；3rd, in the case where pH value of solution changes greatly, brilliant glue load nano zero-valence iron composite material counterweight crome metal can also reach
Preferable removal effect；4th, brilliant glue load nano zero-valence iron composite material has certain adjustment effect to the pH of chromium solution, makes
It maintains in metastable scope (8~10), is conducive to trivalent chromium and forms precipitation, improves the removal effect of chromium；5th, brilliant glue
Load nano zero-valence iron composite material prevents nano zero valence iron to be lost in water body, reduces nano zero-valence iron particle and deposits in the application
Potential hazard, block composite material easy to recycle, efficiently and environmental protection.
Claims (10)
1. a kind of method that crystalline substance glue load nano zero-valence iron composite material removes heavy metal chromium, it is characterised in that：Brilliant glue is loaded
Nano zero-valence iron composite material is added into chromium solution, is reacted.
2. the method that a kind of brilliant glue load nano zero-valence iron composite material according to claim 1 removes heavy metal chromium, its
It is characterized in that：The pH value range of chromium solution is 2~12.
3. the method that a kind of brilliant glue load nano zero-valence iron composite material according to claim 2 removes heavy metal chromium, its
It is characterized in that：The concentration of Cr is 40mg/L~60mg/L in chromium solution.
4. the method that a kind of brilliant glue load nano zero-valence iron composite material according to claim 3 removes heavy metal chromium, its
It is characterized in that：The mass ratio of brilliant glue load nano zero-valence iron composite material and Cr in chromium solution is (1.8~7.5)：1.
5. the method that a kind of brilliant glue load nano zero-valence iron composite material according to claim 4 removes heavy metal chromium, its
It is characterized in that：In brilliant glue load nano zero-valence iron composite material, the load capacity of nano zero valence iron be brilliant colloid amount 3%~
15%.
6. the method that a kind of brilliant glue load nano zero-valence iron composite material according to claim 5 removes heavy metal chromium, its
It is characterized in that：The preparation method of brilliant glue load nano zero-valence iron composite material comprises the following steps：
1) by ferrous salt solution and brilliant glue hybrid reaction, brilliant glue-Fe is obtained2+Material；
2) by brilliant glue-Fe2+After material clean, reacted with reducing agent solution, then through over cleaning, drying, obtains brilliant glue load nanometer
Zero-valent iron composite material.
7. the method that a kind of brilliant glue load nano zero-valence iron composite material according to claim 6 removes heavy metal chromium, its
It is characterized in that：Brilliant glue is sodium acrylate crystalline substance gel matrix.
8. the method that a kind of brilliant glue load nano zero-valence iron composite material according to claim 6 removes heavy metal chromium, its
It is characterized in that：In step 1), ferrous salt is ferrous sulfate.
9. the method that a kind of brilliant glue load nano zero-valence iron composite material according to claim 6 removes heavy metal chromium, its
It is characterized in that：In step 1), reducing agent is sodium borohydride.
10. the method that a kind of brilliant glue load nano zero-valence iron composite material according to claim 1 removes heavy metal chromium, its
It is characterized in that：The time of reaction is 2h~5h.
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| CN108689473A (en) * | 2018-05-24 | 2018-10-23 | 中国科学院重庆绿色智能技术研究院 | A kind of preparation method and applications of Zero-valent Iron porcelain ball |
| CN113769721A (en) * | 2021-09-28 | 2021-12-10 | 上海大学 | Preparation method and application of novel lignin hydrogel loaded nZVI material |
| CN114984929A (en) * | 2022-06-06 | 2022-09-02 | 浙江工业大学 | Ethylenediamine resin zero-valent iron-loaded nanocomposite, preparation method thereof and application thereof in synchronous reduction and trapping of hexavalent chromium in water |
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| CN114984929A (en) * | 2022-06-06 | 2022-09-02 | 浙江工业大学 | Ethylenediamine resin zero-valent iron-loaded nanocomposite, preparation method thereof and application thereof in synchronous reduction and trapping of hexavalent chromium in water |
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