CN102172511A - Preparation method of MnO2/Fe3O4 compound adsorbent - Google Patents
Preparation method of MnO2/Fe3O4 compound adsorbent Download PDFInfo
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- CN102172511A CN102172511A CN 201110082321 CN201110082321A CN102172511A CN 102172511 A CN102172511 A CN 102172511A CN 201110082321 CN201110082321 CN 201110082321 CN 201110082321 A CN201110082321 A CN 201110082321A CN 102172511 A CN102172511 A CN 102172511A
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- China
- Prior art keywords
- compound adsorbent
- preparation
- mno
- mno2
- solution
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- 239000003463 adsorbent Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 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
- 150000001875 compounds Chemical class 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 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
- 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
- 239000012286 potassium permanganate Substances 0.000 abstract 2
- 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
- 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 17
- 239000002245 particle Substances 0.000 description 4
- 238000001179 sorption measurement Methods 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 238000012795 verification Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000010521 absorption reaction 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
- 239000002594 sorbent Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
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- Water Treatment By Sorption (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention relates to a preparation method of a compound adsorbent, in particular to a preparation method of an MnO2/Fe3O4 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, then putting the solution into an anaerobic operating floor, then adding NaOH, stirring the solution rapidly to mix the matters uniformly with a glass rod after bluish green flocculates appear, then pouring the solution to a beaker filled with KMnO4, stirring the solution until KMnO4 is completely dissolved, 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 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.
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
2Apparent density lower, in water, form easily shortcoming such as ultra-fine grain, 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
4The preparation method of compound adsorbent.
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 KMn
O4 fully till the dissolving, quiet heavy 1～2h, and 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.
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
2Formal row 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.
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 electron-microscope scanning figure of compound adsorbent, Fig. 4 are 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.
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
2Formal row 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.
Adopt following verification experimental verification to the effect of heavy metal adsorption: 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 (4)
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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110082321 CN102172511B (en) | 2011-04-01 | 2011-04-01 | Preparation method of MnO2/Fe3O4 compound adsorbent |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110082321 CN102172511B (en) | 2011-04-01 | 2011-04-01 | Preparation method of MnO2/Fe3O4 compound adsorbent |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102172511A true CN102172511A (en) | 2011-09-07 |
| CN102172511B CN102172511B (en) | 2013-03-06 |
Family
ID=44515867
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201110082321 Expired - Fee Related CN102172511B (en) | 2011-04-01 | 2011-04-01 | Preparation method of MnO2/Fe3O4 compound adsorbent |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102172510A (en) * | 2011-04-01 | 2011-09-07 | 哈尔滨工业大学 | Preparation method of MnO2/Fe3O4 compound adsorbent and method for removing lead in water with compound adsorbent |
| 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 |
| 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 |
-
2011
- 2011-04-01 CN CN 201110082321 patent/CN102172511B/en not_active Expired - Fee Related
Non-Patent Citations (2)
| Title |
|---|
| 《Journal of Hazardous Materials》 20090309 Gaosheng Zhang et al Adsorption behavior and mechanism of arsenate at Fe-Mn binary oxide/water interface 第820页至第825页 1-4 第168卷, * |
| 《Water Research》 20070323 Gaosheng Zhang et al Preparation and evaluation of a novel Fe-Mn binary oxide adsorbent for effective arsenite removal 第1921-1928页 1-4 第41卷, * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102172510A (en) * | 2011-04-01 | 2011-09-07 | 哈尔滨工业大学 | Preparation method of MnO2/Fe3O4 compound adsorbent and method for removing lead in water with compound adsorbent |
| CN102172510B (en) * | 2011-04-01 | 2013-03-13 | 哈尔滨工业大学 | Preparation method of MnO2/Fe3O4 compound adsorbent and method for removing lead in water with compound adsorbent |
| 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 |
| 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 |
| CN102188949B (en) * | 2011-04-12 | 2013-01-16 | 哈尔滨工业大学 | Method for removing arsenic (III) in water by utilizing composite MnO2/Fe3O4 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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| Publication number | Publication date |
|---|---|
| CN102172511B (en) | 2013-03-06 |
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