CN102172510A - Preparation method of MnO2/Fe3O4 compound adsorbent and method for removing lead in water with compound adsorbent - Google Patents
Preparation method of MnO2/Fe3O4 compound adsorbent and method for removing lead in water with compound adsorbent Download PDFInfo
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- CN102172510A CN102172510A CN 201110082285 CN201110082285A CN102172510A CN 102172510 A CN102172510 A CN 102172510A CN 201110082285 CN201110082285 CN 201110082285 CN 201110082285 A CN201110082285 A CN 201110082285A CN 102172510 A CN102172510 A CN 102172510A
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- compound adsorbent
- mno
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- water
- adsorbent
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Links
- 239000003463 adsorbent Substances 0.000 title claims abstract description 61
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 150000001875 compounds Chemical class 0.000 title claims abstract description 28
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 18
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 title abstract description 16
- -1 Fe3O4 compound Chemical class 0.000 title abstract 3
- SZVJSHCCFOBDDC-UHFFFAOYSA-N iron(II,III) oxide Inorganic materials O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 title abstract 3
- 238000001179 sorption measurement Methods 0.000 claims abstract description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 12
- 239000008367 deionised water Substances 0.000 claims abstract description 6
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 238000001914 filtration Methods 0.000 claims abstract description 5
- 239000011521 glass Substances 0.000 claims abstract description 5
- 239000000843 powder Substances 0.000 claims abstract description 5
- 239000006228 supernatant Substances 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 5
- 239000010865 sewage Substances 0.000 claims abstract description 4
- 238000001035 drying Methods 0.000 claims abstract description 3
- 239000013049 sediment Substances 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 5
- 238000005189 flocculation Methods 0.000 claims description 4
- 230000016615 flocculation Effects 0.000 claims description 4
- 239000006210 lotion Substances 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 4
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 5
- 238000000926 separation method Methods 0.000 abstract description 3
- 239000002244 precipitate Substances 0.000 abstract 3
- 238000000227 grinding Methods 0.000 abstract 1
- SURQXAFEQWPFPV-UHFFFAOYSA-L iron(2+) sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Fe+2].[O-]S([O-])(=O)=O SURQXAFEQWPFPV-UHFFFAOYSA-L 0.000 abstract 1
- 239000012286 potassium permanganate Substances 0.000 abstract 1
- 230000001376 precipitating effect Effects 0.000 abstract 1
- 230000003068 static effect Effects 0.000 abstract 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 26
- 238000010521 absorption reaction Methods 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 229910052742 iron Inorganic materials 0.000 description 2
- 238000012795 verification Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000000975 co-precipitation Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000002594 sorbent Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
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Abstract
The invention relates to a preparation method of a compound adsorbent and a method for removing lead in water with the compound adsorbent, in particular to a preparation method of an MnO2/Fe3O4 compound adsorbent and a method for removing lead in water with the compound adsorbent. The invention aims to solve the technical problem that MnO2 is not easy to separate, so the application of MnO2 to water treatment is limited. The preparation method comprises the following steps: dissolving FeSO4.7H2O into deionized water at room temperature, putting the solution into an anaerobic operating floor, adding NaOH, stirring the solution rapidly to mix the matters uniformly with a glass rod after bluish green flocculates appear, pouring the solution to a beaker filled with KMnO4, stirring the solution, carrying out static precipitating, removing the supernatant through filtration, repeatedly washing the precipitate, then drying the precipitate and grinding the precipitate into powder to obtain the MnO2/Fe3O4 compound adsorbent. The method for removing lead in water comprises the following steps: controlling the pH value of the sewage containing Pb (II) to be above 5 and then adding the compound adsorbent to carry out turbulence contact adsorption. The compound adsorbent for adsorbing the heavy metal can be separated from water by a magnet and the separation method is simple and easy to operate.
Description
Technical field
The present invention relates to a kind of preparation method of compound adsorbent and remove method plumbous in the water.
Background technology
Suction-operated is owing to its efficient adsorption to low-concentration heavy metal, and high economic benefit and strong operability receive much concern always.Compare MnO with metal oxides such as Fe, Al, Mn, Zn
2The strongest with heavy metal ion affinity.But MnO
2+ apparent density is lower, form shortcoming such as ultra-fine grain in water easily, and is not easily separated, limited the application in water treatment.
Summary of the invention
The present invention will solve MnO
2Not easily separated, limit the technical problem that it is used in water treatment; And provide MnO
2/ Fe
3O
4Plumbous method in the preparation method of compound adsorbent and the removal water thereof.
MnO
2/ Fe
3O
4The preparation method of compound adsorbent carries out in the steps below: at room temperature with 0.45molFeSO
47H
2O is dissolved in the 200mL ionized water, with being placed in the anaerobic operation platform, adds then 1.2molNaOH, occurs stirring and evenly mixing rapidly with glass bar after the blue-green flocculation, pours into then 0.1molKMnO is housed
4In the beaker, be stirred to KMnO
4Till dissolving fully, quiet heavy 1~2h, the filtering supernatant washes sediment until washing lotion becomes neutrality repeatedly with deionized water, sediment is put in the vacuum drying chamber then and dries 5~7h under 40~60 ℃ of conditions, is ground into powder, and obtains MnO
2/ Fe
3O
4Compound adsorbent.
MnO
2/ Fe
3O
4Compound adsorbent is removed method plumbous in the water and finished in the steps below: the pH value that will contain the sewage of Pb (II) is controlled more than 5, adds then the MnO of said method preparation
2/ Fe
3O
4Compound adsorbent carried out turbulent Contact-sorption more than 24 hours; Namely finished plumbous removal.
The present invention by coprecipitation with MnO
2Load to and obtain MnO on the tri-iron tetroxide
2/ Fe
3O
4Compound adsorbent, MnO in the compound adsorbent of the present invention's preparation
2It is comparatively even to distribute, and particle diameter is distributed in 1~100 μ m and does not wait, and manganese dioxide is with amorphous MnO
2Form exists.Adopt magnet just the compound adsorbent of absorption heavy metal to be separated to come from water, simple, the operation easily of separation method.Pb in the water (II) initial concentration is 100mg/L, adds present embodiment MnO
2/ Fe
3O
4Compound adsorbent, described compound adsorbent consumption is 0.4g/L, the adsorbance of described adsorbent is about 118.06mg/g.
Description of drawings
Fig. 1 is MnO
2/ Fe
3O
4Compound adsorbent mixes the design sketch in water; Fig. 2 is the design sketch with quiet heavy 2min behind the magnet adsorption; Fig. 3 is the MnO of the specific embodiment five preparations
2/ Fe
3O
4The Electronic Speculum tracing of compound adsorbent, Fig. 4 is the MnO of the specific embodiment five preparations
2/ Fe
3O
4The XRD diffraction spectrogram of compound adsorbent, Fig. 5 are the MnO of the specific embodiment five preparations
2/ Fe
3O
4The X-ray diffraction spectrogram of compound adsorbent; Fig. 6 is the specific embodiment six MnO
2/ Fe
3O
425 ° of adsorption isotherm line charts of compound adsorbent are among the figure
Represent different lead concentration solution samplings (from 10mg/l-300mg/l),
Expression Langmuir adsorption curve ,-expression Freundlich adsorption curve; Fig. 7 is the specific embodiment six MnO
2/ Fe
3O
4Compound adsorbent 2 curve of adsorption kinetics figure, the point that looses among the figure is 50mg/l lead solution different time absorption sample point; Fig. 8 is the curve of adsorption kinetics figure of the specific embodiment six different temperatures, and ■ represents 303K (30 ℃) among the figure, ▲ expression 313K (40 ℃),
Expression 323K (50 ℃) sample point.
The specific embodiment
Technical solution of the present invention is not limited to the following cited specific embodiment, also comprises any combination between each specific embodiment.
The specific embodiment one: MnO in the present embodiment
2/ Fe
3O
4The preparation method of compound adsorbent carries out in the steps below: at room temperature with 0.45molFeSO
47H
2O is dissolved in the 200mL ionized water, with being placed in the anaerobic operation platform, adds then 1.2mol NaOH, occurs stirring and evenly mixing rapidly with glass bar after the blue-green flocculation, pours into then 0.1molKMnO is housed
4In the beaker, be stirred to KMnO
4Till dissolving fully, quiet heavy 1~2h, the filtering supernatant washes sediment until washing lotion becomes neutrality repeatedly with deionized water, sediment is put in the vacuum drying chamber then and dries 5~7h under 40~60 ℃ of conditions, is ground into powder, and obtains MnO
2/ Fe
3O
4Compound adsorbent.
MnO in the compound adsorbent of present embodiment method preparation
2It is comparatively even to distribute, and particle diameter is distributed in 1~100 μ m and does not wait, and manganese dioxide is with amorphous MnO
2Form exists.
The specific embodiment two: what present embodiment and the specific embodiment one were different is: the described quiet heavy time is 1h.Other step is identical with the specific embodiment one with parameter.
The specific embodiment three: what present embodiment was different with the specific embodiment one or two is: described bake out temperature is 50 ℃.Other step is identical with the specific embodiment one or two with parameter.
The specific embodiment four: what present embodiment and the specific embodiment three were different is: described drying time is 6h.Other is identical with the specific embodiment three.
The specific embodiment five: present embodiment MnO
2/ Fe
3O
4The preparation method of compound adsorbent carries out in the steps below: at room temperature with 0.45molFeSO
47H
2O is dissolved in the 200mL ionized water, with being placed in the anaerobic operation platform, add then 1.2mol NaOH, occur stirring and evenly mixing rapidly (dissolved oxygen in all solution is fully reacted completely) with glass bar after the blue-green flocculation, pour into then 0.1molKMnO is housed
4In the beaker, be stirred to KMnO
4Till dissolving fully, quiet heavy 1h, filtering supernatant, sediment is washed until washing lotion becomes neutrality repeatedly with deionized water, then sediment is put in the vacuum drying chamber (prevent Surface Contact air from heating oxidized) and under 50 ℃ of conditions, dries 6h, be ground into powder, obtain MnO
2/ Fe
3O
4Compound adsorbent (Fig. 5).
MnO in the compound adsorbent of present embodiment method preparation
2Distribute comparatively evenly (Fig. 3), particle diameter is distributed in 1~100 μ m and does not wait (Fig. 4), and manganese dioxide is with amorphous MnO
2Form exists.
MnO with the present embodiment preparation
2/ Fe
3O
4Compound adsorbent mixes in the 100ml deionized water (sees Fig. 1), magnet is attached on bottle wall, original muddy adsorbent mixing material is gradually limpid, sorbent particles is rapidly close to magnet, effect illustrates that the compound adsorbent of present embodiment preparation has very superior performance aspect mud-water separation behind the quiet heavy 2min shown in Fig. 2.
The specific embodiment six: MnO
2/ Fe
3O
4Compound adsorbent is removed method plumbous in the water and finished in the steps below: the pH value that will contain the sewage of Pb (II) is controlled more than 5, adds then the MnO of the specific embodiment one described method preparation
2/ Fe
3O
4Compound adsorbent carried out turbulent Contact-sorption more than 24 hours; Namely finished plumbous removal.
Absorption Pb (II) the results are shown in Figure 6-8.
Fig. 6 is 25 ° of adsorption isotherms of adsorbent, illustrate when the concentration of adsorbent in solution is 0.4g/l, when pb (II) concentration is that 100mg/l can reach best removal effect, the mass ratio of adsorbent and pb (II) is 4: 1 o'clock by that analogy, and adsorbent reaches maximal absorptive capacity substantially and is about 118.06mg/g.
Fig. 7 is a curve of adsorption kinetics, and when adsorption time reaches 24 hours, adsorbance can not change substantially, and adsorbent is saturated to reach absorption, and 24 hours is optimum reacting time.
The high more adsorption effect of the former coolant-temperature gage of Fig. 8 is good more, and adsorption time is can reach maximal absorptive capacity in 24 hours.
The specific embodiment seven: what present embodiment and the specific embodiment six were different is: press MnO
2/ Fe
3O
4Compound adsorbent and pb (II) are that 4: 1 mass ratio adds MnO
2/ Fe
3O
4Compound adsorbent.Other step is identical with the specific embodiment six with parameter.
The effect that adopts following verification experimental verification that heavy metal pb (II) is adsorbed: pb in the water (II) initial concentration is 100mg/L, adds present embodiment MnO
2/ Fe
3O
4Compound adsorbent, described compound adsorbent consumption is 0.4g/L, the adsorbance of described adsorbent is about 118.06mg/g.
Claims (6)
1.MnO
2/ Fe
3O
4The preparation method of compound adsorbent is characterized in that MnO
2/ Fe
3O
4The preparation method of compound adsorbent carries out in the steps below: at room temperature with 0.45molFeSO
47H
2O is dissolved in the 200mL ionized water, with being placed in the anaerobic operation platform, adds then 1.2mol NaOH, occurs stirring and evenly mixing rapidly with glass bar after the blue-green flocculation, pours into then 0.1molKMnO is housed
4In the beaker, be stirred to KMnO
4Till dissolving fully, quiet heavy 1~2h, the filtering supernatant washes sediment until washing lotion becomes neutrality repeatedly with deionized water, sediment is put in the vacuum drying chamber then and dries 5~7h under 40~60 ℃ of conditions, is ground into powder, and obtains MnO
2/ Fe
3O
4Compound adsorbent.
2. MnO according to claim 1
2/ Fe
3O
4The preparation method of compound adsorbent is characterized in that the described quiet heavy time is 1h.
3. MnO according to claim 1 and 2
2/ Fe
3O
4The preparation method of compound adsorbent is characterized in that described bake out temperature is 50 ℃.
4. MnO according to claim 1 and 2
2/ Fe
3O
4The preparation method of compound adsorbent is characterized in that described drying time is 6h.
5. utilize the MnO of the described method preparation of claim 1
2/ Fe
3O
4Compound adsorbent is removed method plumbous in the water, it is characterized in that MnO
2/ Fe
3O
4Compound adsorbent is removed method plumbous in the water and finished in the steps below: the pH value that will contain the sewage of Pb (II) is controlled more than 5, adds then the MnO of the described method preparation of claim 1
2/ Fe
3O
4Compound adsorbent carried out turbulent Contact-sorption more than 24 hours; Namely finished plumbous removal.
6. according to the described MnO of claim 5
2/ Fe
3O
4Compound adsorbent is removed method plumbous in the water, it is characterized in that by MnO
2/ Fe
3O
4Compound adsorbent and pb (II) are that 4: 1 mass ratio adds MnO
2/ Fe
3O
4Compound adsorbent.
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Cited By (13)
Publication number | Priority date | Publication date | Assignee | Title |
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CN102188949A (en) * | 2011-04-12 | 2011-09-21 | 哈尔滨工业大学 | Method for preparing MnO2/Fe3O4 composite adsorbent and method for removing arsenic (III) in water by utilizing composite adsorbent |
CN102188948A (en) * | 2011-04-12 | 2011-09-21 | 哈尔滨工业大学 | Method for preparing MnO2/Fe3O4 composite adsorbent and method for removing arsenic (As) from water by using MnO2/Fe3O4 composite adsorbent |
CN103785345A (en) * | 2014-03-04 | 2014-05-14 | 武汉大学 | Supported manganese dioxide adsorbent and method for treating aniline waste water through same |
CN104209082A (en) * | 2014-10-10 | 2014-12-17 | 哈尔滨工业大学 | Method for preparing Fe3O4-MnO2 adsorbing agent and removing cadmium (II) in water by using Fe3O4-MnO2 adsorbing agent |
CN104353407A (en) * | 2014-11-19 | 2015-02-18 | 中南大学 | Fe-Mn system adsorbent and preparation and application method of Fe-Mn system adsorbent |
CN105688793A (en) * | 2016-01-25 | 2016-06-22 | 华东交通大学 | Preparation method of MnO2-based magnetic nano Fe3O4 heavy metal adsorbing material |
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CN105854785A (en) * | 2016-04-21 | 2016-08-17 | 南京大学 | Method for adsorption-removing lead pollution in water body by utilizing magnetic loading manganese dioxide composite material |
CN106365240A (en) * | 2016-10-13 | 2017-02-01 | 上海大学 | Method for removing heavy metals in waste water by recycling magnetic composite adsorption materials (MnO2-Fe3O4) |
CN107151678A (en) * | 2017-01-26 | 2017-09-12 | 大连理工大学 | The magnetic iron and manganese oxides of aerobic microbiological synthesis and its application |
CN108014745A (en) * | 2017-12-23 | 2018-05-11 | 福州大学 | The preparation method and applications of nano-magnetic iron-based-Mn oxide |
CN108128927A (en) * | 2017-12-28 | 2018-06-08 | 吉林建筑大学 | A kind of method for removing lead ion in water removal using sulphite reinforcing manganese sand |
CN108178369A (en) * | 2017-12-28 | 2018-06-19 | 深圳职业技术学院 | A kind of method for removing lead ion in water removal using single persulfate reinforcing manganese sand |
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CN102188948B (en) * | 2011-04-12 | 2013-01-16 | 哈尔滨工业大学 | Method for removing arsenic (As) from water by using MnO2/Fe3O4 composite adsorbent |
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CN106365240A (en) * | 2016-10-13 | 2017-02-01 | 上海大学 | Method for removing heavy metals in waste water by recycling magnetic composite adsorption materials (MnO2-Fe3O4) |
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CN108014745B (en) * | 2017-12-23 | 2020-05-08 | 福州大学 | Preparation method and application of nano magnetic iron-manganese oxide |
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