CN102745792B - Arsenic-removing material of nano ferrimanganic composite oxide and preparation method thereof - Google Patents
Arsenic-removing material of nano ferrimanganic composite oxide and preparation method thereof Download PDFInfo
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- CN102745792B CN102745792B CN 201210237752 CN201210237752A CN102745792B CN 102745792 B CN102745792 B CN 102745792B CN 201210237752 CN201210237752 CN 201210237752 CN 201210237752 A CN201210237752 A CN 201210237752A CN 102745792 B CN102745792 B CN 102745792B
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Abstract
The invention relates to an arsenic-removing material of nano ferrimanganic composite oxide, which is the nano ferrimanganic composite oxide, wherein the atom ratio of iron to manganese to oxygen is 4:3:(8-10); the valence of the manganese is <+4> and the valence of the iron is <+3>; a BET specific surface area of the arsenic-removing material is 225-282 m<2>/g; and the average grain diameter is 10-20 nm. The nano ferrimanganic composite oxide prepared by the method disclosed by the invention has a larger specific surface area and a good adsorption capability; the removing speed of arsenic ina water body is fast and the effect is good; not only can the arsenic be adsorbed and the trivalence arsenic with the great toxin is converted into the pentavalence arsenic with the small toxin, but also the arsenic can be removed and the detoxication function is realized; and the nano ferrimanganic composite oxide can be used for a static adsorption manner and also can be filled into a filling column to remove the arsenic in a dynamic adsorption manner.
Description
Technical field
The invention belongs to water treatment field, be specifically related to arsenic removal material of a kind of nanometer ferro manganese composite oxides and preparation method thereof.
Background technology
Now, the situation that arsenic content surpasses the human security standard for drinking in the water body under the state of nature extensively exists.China is subjected to one of the most serious country of arsenic contamination in the world.Arsenic is one of index of very important polluted drinking water, arsenic limit value in the drinking water standard of the up-to-date promulgation of China is 10 μ g/L, if according to tap water arsenic content hygienic standard, China has the tap water of tens million of populations to surpass this standard (China's endemic arsenic poisoning basic research work progress " the sick magazine of learning of place of china " Fu Songbo, Chen Zhi, 2006).If the water of human long-term drinking arsenic content overproof can cause arseniasis, and then cause multiple health problem, for example skin color changes, sole and skin of palm of hand meeting hardening, suffer from skin carcinoma, bladder cancer, lung cancer and ephrosis easily, and the vascular lesion of pin and leg, diabetes, hypertension and endocrine regulation disease, serious meeting causes death.
Dearsenicating method has chemical process, physical method, biological method etc. in the water body.Wherein, absorption method is with low cost, and is simple and easy to do, is the most common, effective means.The sorbing material of arsenic removal has burning mineral, hydrous oxides etc. such as wilkinite, diatomite, coconut husk, aluminum oxide, ferric oxide, and wherein ferriferous oxide has strong adsorptive power to arsenic and extensive concern the most.Arsenic is present in the nature underground water with trivalent and pentavalent state, and arsenious toxicity is more than 60 times of toxicity of pentavalent arsenic.
In the present sorbing material, mostly pentavalent arsenic there is removal effect preferably, but relatively poor to arsenious removal ability.Therefore the oxidation trivalent arsenic is pentavalent arsenic in the arsenic removal process, and the method for absorption arsenic removal can play the toxicity that reduces arsenic synchronously, can also improve the removal efficient of arsenic.Ferro manganese composite oxides is a kind of suitable material, and tetravalence manganese wherein can be oxidized to pentavalent arsenic with trivalent arsenic, and ferric iron has stronger removal ability to arsenic.[the people such as Qu Jiuhui of method before this, Preparation and evaluation of a novel Fe-Mn binary oxide adsorbent for effective arsenite removal, Water Research, 2007:41 (9)] in utilize permanganate and ferrous salt generation redox reaction, coprecipitation method has prepared micron-sized iron and manganese oxides, but oxidation takes place in ferrous salt easily in reaction process, operational condition is wayward, and the resultant productive rate is lower.
Summary of the invention
Technical problem to be solved by this invention is at above-mentioned deficiency of the prior art, and arsenic removal material of a kind of nanometer ferro manganese composite oxides and preparation method thereof is provided, and its arsenic removal material is fast, effective to the removal speed of arsenic in the water body.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is as follows:
A kind of arsenic removal material of nanometer ferro manganese composite oxides, it is the nanometer ferro manganese composite oxides, the atomic ratio of institute's iron content, manganese and oxygen is 4:3:(8 ~ 10), wherein manganese is+4 valencys, iron is+3 valencys.The BET specific surface area of described arsenic removal material is 225 ~ 282
m
2/ g, median size is 10 ~ 20 nm.
A kind of preparation method of arsenic removal material of nanometer ferro manganese composite oxides, it comprises the steps:
(1) mol ratio according to molysite and permanganate is 4:3, under vigorous stirring the iron salt solutions atomizing is sprayed into permanganate solution for drop, and constantly the pH value of regulation system is 8-10 and keeps stable simultaneously;
(2) treat iron salt solutions spray into finish after, place then and be heated to 90-100 ℃ on the electric furnace, remain on this temperature and continue heating 1 ~ 2 hour, prevent bumping with the glass stick stirring in the heat-processed, left standstill aging 6-12 hour, the gained solid reaction product is extremely neutral with deionized water wash, pulverize after the drying and sieve, in 300-500 ℃ of calcining 6-12 hour, can prepare the arsenic removal material of nanometer ferro manganese composite oxides again.
Press such scheme, described iron salt solutions concentration is less than 0.20mol/L.
Press such scheme, described permanganate concentration is less than 0.15mol/L.
Press such scheme, the alkaline conditioner of described regulation system pH is sodium hydroxide or the potassium hydroxide solution of 1-3 mol/L.
Press such scheme, described molysite is iron(ic) chloride.
Press such scheme, described permanganate is potassium permanganate or sodium permanganate.
Press such scheme, described drying temperature is 105-120 ℃, and be 5-10 hour time of drying.
Press such scheme, described vigorous stirring refers to that mixing speed is 150-200 rev/min.
The present invention joins in the permanganate reaction soln with spray pattern for behind the drop by ferric chloride Solution is atomized, the molysite drop of atomizing is fully contacted with reaction soln, the while vigorous stirring, increase the disturbance of reactive system, make the reaction of iron salt solutions and permanganate solution form the tiny solid reaction product of particle, and thermal degradation forms ferro manganese composite oxides, manganese wherein is+4 valencys, iron is+3 valencys, and then through calcination processing, reaction solid product particle is reduced, form the arsenic removal material of nanometer ferro manganese composite oxides.
Compared with prior art, the invention has the beneficial effects as follows:
1, nanometer ferro manganese composite oxides arsenic removal material of the present invention has bigger specific surface area and good adsorption performance, removal speed to arsenic in the water body is fast, effective, can not only arsenic-adsorbing, can also be oxidized to the less pentavalent arsenic of toxicity by the trivalent arsenic that toxicity is big, have oxidation detoxifcation and adsorption dual function, pollutents such as trivalent arsenic and pentavalent arsenic are had good removal effect; 2, the arsenic removal material for preparing of the present invention both can be used for the Static Adsorption mode, the packed column dynamic adsorption mode of also can packing into, and the arsenic removal operational condition is simple, reacts completely, and preparation process simple controllable, with low cost can be mass-produced, and is easy to utilize; 3, after the present invention utilizes the spraying trivalent iron salt and the abundant hybrid reaction of permanganate that enter, the colloid that generates is heated again and make, this method has been avoided in the past the rotten situation of ferrous salt in the reaction process, makes simultaneously and reacts more abundant; 4, calcination process of the present invention is conducive to the ferro manganese composite oxides size and further reduces, and specific surface area increases.
Description of drawings
Fig. 1 is that the EDAX of the arsenic removal material of the embodiment of the invention 1 described nanometer ferro manganese composite oxides can spectrogram.
Fig. 2 is the BET test pattern of the arsenic removal material of the embodiment of the invention 1 described nanometer ferro manganese composite oxides,
Fig. 3 is the transmission electron microscope TEM figure of the arsenic removal material of the embodiment of the invention 1 described nanometer ferro manganese composite oxides.
Fig. 4 is that the arsenic removal material of the embodiment of the invention 1 described nanometer ferro manganese composite oxides is to the effect of removing arsenic figure of trivalent arsenic and pentavalent arsenic.
Fig. 5 is that the EDAX of the arsenic removal material of the embodiment of the invention 2 described nanometer ferro manganese composite oxides can spectrogram.
Fig. 6 is the BET test pattern of the arsenic removal material of the embodiment of the invention 2 described nanometer ferro manganese composite oxides,
Fig. 7 is the transmission electron microscope TEM figure of the arsenic removal material of the embodiment of the invention 2 described nanometer ferro manganese composite oxides.
Embodiment
Embodiment 1
A kind of arsenic removal material of nanometer ferro manganese composite oxides, it is the nanometer ferro manganese composite oxides, and the atomic ratio of institute's iron content, manganese and oxygen is 4:3:10, and wherein manganese is+4 valencys, and iron is+3 valencys, the BET specific surface area of described arsenic removal material is 282 m
2/ g, median size is 20 nm.
The arsenic removal material of above-mentioned nanometer ferro manganese composite oxides, its preparation method comprises the steps:
(1) takes by weighing 9.48 gram KMnO
4With 21.62 gram FeCl
36H
2O is dissolved in respectively in the 500ml deionized water, and above-mentioned ferric chloride Solution atomizing is sprayed in the KMnO4 solution for drop, and the sodium hydroxide regulation system pH value that adopts 1 mol/L is 8 and makes it keep stable;
(2) treat FeCl
36H
2After O solution sprays into and finishes, above-mentioned solution is heated to 90 ℃ on electric furnace, continues heating 2 hours in this temperature, have chlorine to produce in the heat-processed, constantly stir with glass stick and prevent bumping; Left standstill then aging 12 hours, the gained solid reaction product is extremely neutral with deionized water wash, and 105 ℃ of dryings were calcined 12 hours in 300 ℃ after 10 hours again, namely obtained the arsenic removal material of nanometer ferro manganese composite oxides.
The reaction principle of this arsenic removal material is: under heating condition, permanganate decomposes oxygen and the chlorion generation redox reaction that produces, manganese in the MnO4 is reduced to the Mn(IV), generated chlorine simultaneously, under the pH of reaction system condition, Fe(III) colloid that generates decomposes in heat-processed.Finally obtained the nanometer ferro manganese composite oxides of uniform component.
As shown in Figure 1: the arsenic removal material of this nanometer ferro manganese composite oxides is composite oxides, and the atomic ratio of iron, manganese and oxygen is 4:3:10.
As shown in Figure 2, the BET specific surface area of the arsenic removal material of this nanometer ferro manganese composite oxides is 282 m
2/ g.
As shown in Figure 3, the arsenic removal material uniform particles of this nanometer ferro manganese composite oxides, median size are 10 ~ 20nm.
The effect of the arsenic removal material of above-mentioned nanometer ferro manganese composite oxides is:
Usage quantity with 1g/L in the water body that initial arsenic concentration is 2 mg/L, pH 7.0 adds this arsenic removal material, 200 rev/mins of concussions of shaking table, and arsenious concentration is calculated the trivalent arsenic clearance over time in the detection architecture, the results are shown in Figure 4.As shown in Figure 4: after 5 minutes, this arsenic removal material can reach 84.1% and 72.4% to the clearance of trivalent arsenic in the water body and pentavalent arsenic, after 15 minutes, this material can reach 92.4% and 84.6% to the clearance of trivalent arsenic in the water body and pentavalent arsenic, after 1 hour, this material can reach to the clearance of trivalent arsenic in the water body and pentavalent arsenic that the clearance to trivalent arsenic and pentavalent arsenic can reach 99.9% and 99.2% after 96.3% and 91.8%, 3 hour.
Embodiment 2
A kind of arsenic removal material of nanometer ferro manganese composite oxides, it is the nanometer ferro manganese composite oxides, and the atomic ratio of institute's iron content, manganese and oxygen is 4:3:8, and wherein manganese is+4 valencys, and iron is+3 valencys, the BET specific surface area of described arsenic removal material is 225 m
2/ g, median size is 10 nm.
The arsenic removal material of above-mentioned nanometer ferro manganese composite oxides, its preparation method comprises the steps:
(1) takes by weighing 11.76 gram NaMnO
43H
2O and 21.62 gram FeCl
36H
2O is dissolved in respectively in the 500ml deionized water, and the ferric chloride Solution atomizing is sprayed into NaMnO for drop
4In the solution, the potassium hydroxide regulation system pH value that adopts 3mol/L is 10 and makes it keep stable;
(2) treat FeCl
36H
2After O solution sprays into and finishes, above-mentioned solution is heated to 95 ℃ on electric furnace, continues heating 1 hour in this temperature, prevent bumping with the glass stick stirring in the heat-processed; Left standstill then aging 6 hours, the gained solid reaction product is washed till neutrality with deionized water, 120 ℃ of dryings were calcined 6 hours in 500 ℃ after 5 hours again, namely obtained the arsenic removal material of nanometer ferro manganese composite oxides.Reaction principle and example 1 are similar, do not repeat them here.
As shown in Figure 5: the arsenic removal material of this nanometer ferro manganese composite oxides is composite oxides, and the atomic ratio of iron, manganese and oxygen is 4:3:8.As shown in Figure 6, the BET specific surface area of the arsenic removal material of this nanometer ferro manganese composite oxides is 240 m
2/ g.
As shown in Figure 7, the arsenic removal material uniform particles of this nanometer ferro manganese composite oxides, particle diameter is about 10 ~ 20nm.
Usage quantity with 0.5 g/L in the water body that initial arsenic concentration is 2 mg/L, pH 7.0 adds this arsenic removal material, and arsenious concentration is over time in the detection architecture, calculate the trivalent arsenic clearance, after 3 hours, this material can reach 98.5% and 96.2% to the clearance of trivalent arsenic in the water body and pentavalent arsenic.
Claims (8)
1. the arsenic removal material of a nanometer ferro manganese composite oxides, it is characterized in that it is the nanometer ferro manganese composite oxides, the atomic ratio of institute's iron content, manganese and oxygen is 4:3:(8 ~ 10), wherein manganese is+4 valencys, iron is+3 valencys, and the preparation process of described nanometer ferro manganese composite oxides is as follows:
(1) mol ratio according to iron(ic) chloride and permanganate is 4:3, under agitation the ferric chloride Solution atomizing is sprayed into permanganate solution for drop, and constantly the pH value of regulation system is 8-10 and keeps stable simultaneously;
(2) after ferrous solution to be chlorinated sprays into and finishes, place then to be heated to 90-100 ℃ on the electric furnace, remain on this temperature and continue heating 1 ~ 2 hour, prevent bumping with the glass stick stirring in the heat-processed, left standstill aging 6-12 hour;
(3) the gained solid reaction product is extremely neutral with deionized water wash, pulverize after the drying and sieve, again in 300-500 ℃ of calcining 6-12 hour, can prepare the arsenic removal material of nanometer ferro manganese composite oxides.
2. the arsenic removal material of a kind of nanometer ferro manganese composite oxides according to claim 1, the BET specific surface area that it is characterized in that described arsenic removal material is 225 ~ 282 m
2/ g, median size is 10 ~ 20 nm.
3. a method for preparing the arsenic removal material of the described nanometer ferro manganese composite oxides of claim 1 is characterized in that it comprises the steps:
(1) mol ratio according to iron(ic) chloride and permanganate is 4:3, under agitation the ferric chloride Solution atomizing is sprayed into permanganate solution for drop, and constantly the pH value of regulation system is 8-10 and keeps stable simultaneously;
(2) after ferrous solution to be chlorinated sprays into and finishes, place then and be heated to 90-100 ℃ on the electric furnace, remain on this temperature and continue heating 1 ~ 2 hour, prevent bumping with the glass stick stirring in the heat-processed, left standstill aging 6-12 hour, the gained solid reaction product is extremely neutral with deionized water wash, pulverize after the drying and sieve, in 300-500 ℃ of calcining 6-12 hour, can prepare the arsenic removal material of nanometer ferro manganese composite oxides again.
4. the preparation method of the arsenic removal material of a kind of nanometer ferro manganese composite oxides according to claim 3 is characterized in that described ferric chloride Solution concentration is less than 0.20mol/L.
5. the preparation method of the arsenic removal material of a kind of nanometer ferro manganese composite oxides according to claim 3 is characterized in that described permanganate concentration is less than 0.15mol/L.
6. the preparation method of the arsenic removal material of a kind of nanometer ferro manganese composite oxides according to claim 3 is characterized in that described permanganate is potassium permanganate or sodium permanganate.
7. the preparation method of the arsenic removal material of a kind of nanometer ferro manganese composite oxides according to claim 3, the alkaline conditioner that it is characterized in that described regulation system pH is sodium hydroxide or the potassium hydroxide solution of 1-3 mol/L.
8. the preparation method of the arsenic removal material of a kind of nanometer ferro manganese composite oxides according to claim 3 is characterized in that described drying temperature is 105-120 ℃, and be 5-10 hour time of drying.
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| CN110975794A (en) * | 2019-11-22 | 2020-04-10 | 昆明理工大学 | Iron-manganese composite oxide/Fe3O4Preparation method and application of core-shell material |
| CN111534307B (en) * | 2020-05-25 | 2021-07-13 | 浙江中地净土科技有限公司 | Double-layer covering soil remediation agent for heavy metal contaminated soil and preparation method |
| CN111908653B (en) * | 2020-07-13 | 2022-09-23 | 矿冶科技集团有限公司 | Slow-release arsenic and antimony removal medicament, preparation method thereof and method for deeply treating heavy metal wastewater by adopting slow-release arsenic and antimony removal medicament |
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Application publication date: 20121024 Assignee: Hubei agricultural Chang rang soil remediation Polytron Technologies Inc Assignor: China University of Geosciences (Wuhan) Contract record no.: 2017420000004 Denomination of invention: Arsenic-removing material of nano ferrimanganic composite oxide and preparation method thereof Granted publication date: 20130918 License type: Exclusive License Record date: 20170317 |
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