CN104759288A - Heterogeneous Cu-Mn-Ce Fenton-like catalyst, and preparation method and use thereof - Google Patents
Heterogeneous Cu-Mn-Ce Fenton-like catalyst, and preparation method and use thereof Download PDFInfo
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- CN104759288A CN104759288A CN201410002596.9A CN201410002596A CN104759288A CN 104759288 A CN104759288 A CN 104759288A CN 201410002596 A CN201410002596 A CN 201410002596A CN 104759288 A CN104759288 A CN 104759288A
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- 239000003054 catalyst Substances 0.000 title claims abstract description 52
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000011259 mixed solution Substances 0.000 claims abstract description 22
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims abstract description 20
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims abstract description 19
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 claims abstract description 19
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000002351 wastewater Substances 0.000 claims abstract description 13
- 239000000463 material Substances 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 7
- 238000001354 calcination Methods 0.000 claims abstract description 5
- 238000009826 distribution Methods 0.000 claims abstract description 3
- 238000001035 drying Methods 0.000 claims abstract description 3
- 238000001914 filtration Methods 0.000 claims abstract description 3
- 238000005406 washing Methods 0.000 claims abstract description 3
- 239000000975 dye Substances 0.000 claims description 15
- 239000011148 porous material Substances 0.000 claims description 9
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 9
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 claims description 6
- 229940043267 rhodamine b Drugs 0.000 claims description 6
- 230000035484 reaction time Effects 0.000 claims description 2
- 230000003197 catalytic effect Effects 0.000 abstract description 9
- 230000015556 catabolic process Effects 0.000 abstract description 3
- 238000006555 catalytic reaction Methods 0.000 abstract description 3
- 238000006731 degradation reaction Methods 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 2
- 238000007598 dipping method Methods 0.000 abstract 1
- 229910021426 porous silicon Inorganic materials 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 11
- -1 regulates pH to 3 Substances 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 239000006185 dispersion Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000007210 heterogeneous catalysis Methods 0.000 description 3
- 229910044991 metal oxide Inorganic materials 0.000 description 3
- 150000004706 metal oxides Chemical class 0.000 description 3
- 230000002378 acidificating effect Effects 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000002808 molecular sieve Substances 0.000 description 2
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 229920002521 macromolecule Polymers 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
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Abstract
The invention provides a preparation method and a use of a high-performance heterogeneous Cu-Mn-Ce Fenton-like catalyst. The preparation method of the catalyst comprises the following steps: 1, preparing a copper nitrate, cerium nitrate and manganese nitrate mixed solution; 2, repeatedly dipping a highly ordered meso-porous silicon oxide material in the mixed solution obtained in step 1, filtering, washing, and drying; and 3, calcining a material prepared in step 2 in a muffle furnace to obtain the heterogeneous Cu-Mn-Ce Fenton-like catalyst. A Fenton-like reaction system formed by the catalyst and hydrogen peroxide can realize efficient catalytic degradation of high-concentration dye wastewater at a low temperature under normal pressure, and has the advantages of simple making technology, low cost, large specific surface area, narrow aperture distribution, high catalysis activity and wide pH application range.
Description
Technical field
The invention belongs to catalyst preparing and application, relate to a kind of heterogeneous Cu-Mn-Ce type Fenton catalyst and its production and use.
Background technology
Waste water from dyestuff has caused serious problem of environmental pollution, brings great threat to the health of the mankind, although traditional homogeneous phase Fenton catalyst also has considerable catalytic activity for waste water from dyestuff, its pH scope of application is narrower.Therefore, preparation is a kind of efficiently, and the wide heterogeneous catalysis of the pH scope of application has very important practical meaning in engineering.In recent years, some are also in the news for the heterogeneous catalysis of waste water from dyestuff.Wherein, researcher finds bimetallic mixed oxide catalyst, as MOFe
2o
3(M:Fe, Co, Cu, Mn), has higher catalytic activity than Fe2O3 catalyst usually, and CuOFe
2o
3and CoOFe
2o
3also there is wider pH tolerance range (Applied Catalysis B:Environmental2006,66, (3-4), 258-264.), but this kind of metal oxide catalyst is without dispersion, cannot reach nanoscale, contact surface is less, limits its catalytic activity.Also have some researchers active component Cu to be dispersed in (Journal of hazardousmaterials2007,144, (3), 663-667) on ZSM-5 molecular sieve, but the duct of ZSM-5 molecular sieve belong to micropore, is difficult to be applicable to macromolecular substances.Some researchers are also had to select some mesoporous supports to disperse, its heterogeneous catalysis prepared also illustrates the catalytic activity higher than the catalyst without dispersion, but the active component of this kind of catalyst is easy to reunite owing to not adding dispersant, thus affect its catalytic activity (catalysis communications2006,7, (7), 478-483).From document and patent results, the existing usual catalytic activity of heterogeneous Fenton catalyst for waste water from dyestuff is not high, and active component dispersion is uneven, and easily reunites.Therefore, prepare good dispersion degree and there is one of high performance heterogeneous type Fenton catalyst study hotspot becoming waste water from dyestuff.
Summary of the invention
The object of the present invention is to provide a kind of heterogeneous Cu-Mn-Ce type Fenton catalyst and its production and use.
For achieving the above object, the present invention is by the following technical solutions:
A preparation method for heterogeneous Cu-Mn-Ce type Fenton catalyst, comprises following steps:
(1) copper nitrate, cerous nitrate and manganese nitrate mixed solution is configured;
(2) meso pore silicon oxide material of high-sequential be impregnated in repeatedly in the mixed solution of step (1) gained, filtration, washing, drying;
(3) then, the material that step (2) is obtained is placed in Muffle furnace and calcines, obtain heterogeneous Cu-Mn-Ce type Fenton catalyst (i.e. Cu-Mn-Ce/ mesopore silicon oxide, Cu-Mn-Ce/OMS).
In copper nitrate in described step (1), cerous nitrate, manganese nitrate mixed solution, the concentration of each material is 0.1 ~ 1mol/L.
In described step (2), the dosage of the meso pore silicon oxide material of high-sequential is 10 ~ 40g/L, and dip time is 4 ~ 8h.
The meso pore silicon oxide material of described high-sequential is MCM-41 or SBA-15.
Calcining heat in described step (3) is 300 ~ 500 DEG C, and calcination time is 6h.
The heterogeneous Cu-Mn-Ce type Fenton catalyst (i.e. Cu-Mn-Ce/OMS) that a kind of said method is obtained.
Described Cu-Mn-Ce type Fenton catalyst belongs to new construction high-performance porous catalyst, and its duct is two-dimentional hexagonal structure and uniform and ordered, and aperture is comparatively large, and distribution is generally at 2-10nm, and specific area is generally 200-600m
2/ g, pore volume scope is 0.2-0.6cm
3/ g.In addition, catalyst activity component disperses is even, and catalytic capability is stronger.
A purposes for above-mentioned heterogeneous Cu-Mn-Ce catalyst treatment waste water from dyestuff, comprises the following steps:
In waste water from dyestuff, add hydrogen peroxide and above-mentioned obtained heterogeneous Cu-Mn-Ce catalyst form embryonic stem-like cells system and react.In course of reaction, heterogeneous Cu-Mn-Ce catalyst hydrogen peroxide produces free radical cracking dye molecule.
Described dyestuff is one or more in rhodamine B or azogeramine etc., and dye strength is 1 ~ 2000mg/L.
The dosage of described heterogeneous Cu-Mn-Ce catalyst is 0.1 ~ 0.4g/L.
The dosage of described hydrogen peroxide is 0.2 ~ 0.8mol/L.
Described reaction temperature is 70 ~ 90 DEG C.
In described reaction, pH value is 3 ~ 7.
The described reaction time is 50-210min.
The present invention has following beneficial effect:
The invention provides a kind of methods for making and using same of heterogeneous Cu-Mn-Ce type Fenton catalyst.This catalyst manufacture craft is simple, and cost is lower, and duct uniform and ordered, pH is applied widely.The Fenton reaction system formed with hydrogen peroxide has higher catalytic activity to dye wastewater with high concentration (rhodamine B, azogeramine etc.) under the condition of low temperature, normal pressure, even if in neutral conditions, this catalyst still can keep higher degradation efficiency.
Accompanying drawing explanation
Fig. 1 is the TEM photo of catalyst in the embodiment of the present invention 1.This catalyst soakage time is 6h, calcines 6h and obtain at 300 DEG C.In figure, dash area is successfully the reactive metal oxides of load on mesopore silicon oxide.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is described further.
Embodiment 1
(1) mixed solution (copper nitrate, manganese nitrate and cerous nitrate concentration are respectively the mixed solution of 1mol/L) first, configuring the copper nitrate of 1mol/L, manganese nitrate and cerous nitrate is stand-by;
(2) secondly, 1g SBA-15 is impregnated into repeatedly (20g/L) in the mixed solution of the above-mentioned copper nitrate of 50mL, manganese nitrate and cerous nitrate and stirs 8h, then filter, dry;
(3) then, gained sample in step (2) is placed in Muffle furnace, and at 300 DEG C, calcine 6h can obtain heterogeneous Cu-Mn-Ce type Fenton catalyst, its TEM picture as shown in Figure 1.As seen from Figure 1, this catalyst is demonstrating large-scale ordered arrangement strip structure along [110] direction, and in figure, dash area is successfully the reactive metal oxides of load on mesopore silicon oxide.Its structural parameters are as shown in table 1;
(4) then, the high concentration rhodamine B solution to 1000mg/L adds the heterogeneous Cu-Mn-Ce type Fenton catalyst of 0.2g/L and 0.4mol/L hydrogen peroxide, regulates pH to 3, solution is heated to 70 DEG C simultaneously, allows this system react 210min.
Decolorizing effect is remarkable, and degradation efficiency reaches more than 99%, as shown in table 2.
Embodiment 2
(1) mixed solution stand-by (copper nitrate, manganese nitrate and cerous nitrate concentration are respectively the mixed solution of 0.1mol/L) of the copper nitrate of 0.1mol/L, manganese nitrate and cerous nitrate first, is configured;
(2) secondly, 0.5g MCM-41 is impregnated into repeatedly (10g/L) in the mixed solution of the above-mentioned copper nitrate of above-mentioned 50mL, manganese nitrate and cerous nitrate and stirs 4h, then filter, dry;
(3) then, gained sample in step (2) is placed in Muffle furnace, at 500 DEG C, calcines 6h can obtain heterogeneous Cu-Mn-Ce type Fenton catalyst;
(4) then, red 1 solution of the high-concentration acidic wastewater to 2000mg/L adds the heterogeneous Cu-Mn-Ce type Fenton catalyst of 0.1g/L and 0.2mol/L hydrogen peroxide, regulates pH to 3, solution is heated to 70 DEG C simultaneously, allows this system react 210min, the results are shown in Table 2.
Embodiment 3
(1) mixed solution (copper nitrate, manganese nitrate and cerous nitrate concentration are respectively the mixed solution of 0.5mol/L) first, configuring the copper nitrate of 0.5mol/L, manganese nitrate and cerous nitrate is stand-by;
(2) secondly, 2g MCM-41 is impregnated into repeatedly (40g/L) in the mixed solution of 50mL copper nitrate, manganese nitrate and cerous nitrate and stirs 6h, then filter, dry;
(3) then, gained sample in step (2) is placed in Muffle furnace, at 400 DEG C, calcines 6h can obtain heterogeneous Cu-Mn-Ce type Fenton catalyst;
(4) then, the high concentration rhodamine B solution to 1500mg/L adds the heterogeneous Cu-Mn-Ce type Fenton catalyst of 0.4g/L and 0.8mol/L hydrogen peroxide, regulates pH to 5, solution is heated to 80 DEG C simultaneously, allows this system react 210min, the results are shown in Table 2.
Embodiment 4
(1) mixed solution first, configuring the copper nitrate of 0.5mol/L, manganese nitrate and cerous nitrate is stand-by;
(2) secondly, 1g SBA-15 is impregnated into repeatedly (20g/L) in the mixed solution of 50mL copper nitrate, manganese nitrate and cerous nitrate and stirs 6h, then filter, dry;
(3) then, gained sample in step (2) is placed in Muffle furnace, at 300 DEG C, calcines 6h can obtain heterogeneous Cu-Mn-Ce type Fenton catalyst;
(4) then, the high concentration rhodamine B solution to 1mg/L adds the heterogeneous Cu-Mn-Ce type Fenton catalyst of 0.2g/L and 0.4mol/L hydrogen peroxide, regulates pH to 3, solution is heated to 90 DEG C simultaneously, allows this system react 50min, the results are shown in Table 2.
Embodiment 5
(1) mixed solution (copper nitrate, manganese nitrate and cerous nitrate concentration are respectively the mixed solution of 0.5mol/L) first, configuring the copper nitrate of 0.5mol/L, manganese nitrate and cerous nitrate is stand-by;
(2) secondly, 1g SBA-15 is impregnated into repeatedly (20g/L) in the mixed solution of 50mL copper nitrate, manganese nitrate and cerous nitrate and stirs 6h, then filter, dry;
(3) then, gained sample in step (2) is placed in Muffle furnace, at 300 DEG C, calcines 6h can obtain heterogeneous Cu-Mn-Ce type Fenton catalyst;
(4) then, red 1 solution of the high-concentration acidic wastewater to 2000mg/L adds the heterogeneous Cu-Mn-Ce type Fenton catalyst of 0.2g/L and 0.4mol/L hydrogen peroxide, regulates pH to 7, solution is heated to 70 DEG C simultaneously, allows this system react 210min, the results are shown in Table 2.
Table 1 is the structural parameters of heterogeneous Cu-Mn-Ce type Fenton catalyst in embodiment 1.
Table 1
Table 2 is decolorizing efficiencies of embryonic stem-like cells system in embodiment 1-5.
Table 2
| Embodiment | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 |
| Decolorizing efficiency | ＞99% | ＞65% | ＞85% | ＞99% | ＞65% |
Above-mentioned is can understand and apply the invention for ease of those skilled in the art to the description of embodiment.Person skilled in the art obviously easily can make various amendment to these embodiments, and General Principle described herein is applied in other embodiments and need not through performing creative labour.Therefore, the invention is not restricted to embodiment here, those skilled in the art, according to announcement of the present invention, do not depart from improvement that scope makes and amendment all should within protection scope of the present invention.
Claims (10)
1. a preparation method for heterogeneous Cu-Mn-Ce type Fenton catalyst, is characterized in that: comprise following steps:
(1) copper nitrate, cerous nitrate and manganese nitrate mixed solution is configured;
(2) meso pore silicon oxide material of high-sequential be impregnated in repeatedly in the mixed solution of step (1) gained, filtration, washing, drying;
(3) material that step (2) is obtained is placed in Muffle furnace to calcine, obtains heterogeneous Cu-Mn-Ce type Fenton catalyst.
2. preparation method according to claim 1, is characterized in that: in the copper nitrate in described step (1), cerous nitrate, manganese nitrate mixed solution, the concentration of each material is 0.1 ~ 1mol/L.
3. preparation method according to claim 1, is characterized in that: in described step (2), the dosage of the meso pore silicon oxide material of high-sequential is 10 ~ 40g/L, and dip time is 4 ~ 8h.
4. the preparation method according to claim 1 or 3, is characterized in that: the meso pore silicon oxide material of described high-sequential is MCM-41 or SBA-15.
5. preparation method according to claim 1, is characterized in that: the calcining heat in described step (3) is 300 ~ 500 DEG C, and calcination time is 6h.
6. the heterogeneous Cu-Mn-Ce type Fenton catalyst that in a claim 1-5, arbitrary described preparation method obtains.
7. heterogeneous Cu-Mn-Ce type Fenton catalyst according to claim 6, is characterized in that: the pore size distribution range of described heterogeneous Cu-Mn-Ce type Fenton catalyst is 2-10nm, and specific area is 200-600m
2/ g, pore volume is 0.2-0.6cm
3/ g.
8. a purposes for the heterogeneous Cu-Mn-Ce catalyst treatment waste water from dyestuff described in claim 6, is characterized in that: comprise the following steps: in waste water from dyestuff, add hydrogen peroxide and heterogeneous Cu-Mn-Ce catalyst form embryonic stem-like cells system and react.
9. purposes according to claim 8, is characterized in that: described dyestuff is one or more in rhodamine B or azogeramine, and dye strength is 1 ~ 2000mg/L.
10. purposes according to claim 8, is characterized in that: the dosage of described heterogeneous Cu-Mn-Ce catalyst is 0.1 ~ 0.4g/L;
Or the dosage of described hydrogen peroxide is 0.2 ~ 0.8mol/L;
Or described reaction temperature is 70 ~ 90 DEG C; In described reaction, pH value is 3 ~ 7; The described reaction time is 50-210min.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106630102A (en) * | 2017-01-17 | 2017-05-10 | 武汉纺织大学 | Application and method of degrading organic wastewater with Ce-OMS-2 catalyst |
| CN108273516A (en) * | 2017-10-12 | 2018-07-13 | 北京森泉伟业科技有限公司 | A kind of method that electrolytic manganese residues prepare effective catalyst and catalyzing hydrogen peroxide oxidative degradation methylene blue |
| CN109046373A (en) * | 2018-07-24 | 2018-12-21 | 成都信息工程大学 | Heterogeneous class Fenotn catalyst CeO capable of magnetic separating2The preparation method and application of/MZFS |
| CN111151289A (en) * | 2019-12-25 | 2020-05-15 | 浙江工商大学 | Manganese-based bimetallic oxide mesoporous material and preparation and application thereof |
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| CN101601998A (en) * | 2009-06-11 | 2009-12-16 | 浙江省环境保护科学设计研究院 | A kind of Preparation of catalysts method that is used for treating high-concentration organic wastewater through catalytic oxidation |
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Patent Citations (1)
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| CN101601998A (en) * | 2009-06-11 | 2009-12-16 | 浙江省环境保护科学设计研究院 | A kind of Preparation of catalysts method that is used for treating high-concentration organic wastewater through catalytic oxidation |
Non-Patent Citations (1)
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| FRANK L.Y. LAM ET AL: ""A high performance bimetallic catalyst for photo-Fenton oxidation of Orange II over a wide pH range"", 《CATALYSIS COMMUNICATIONS》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106630102A (en) * | 2017-01-17 | 2017-05-10 | 武汉纺织大学 | Application and method of degrading organic wastewater with Ce-OMS-2 catalyst |
| CN108273516A (en) * | 2017-10-12 | 2018-07-13 | 北京森泉伟业科技有限公司 | A kind of method that electrolytic manganese residues prepare effective catalyst and catalyzing hydrogen peroxide oxidative degradation methylene blue |
| CN108273516B (en) * | 2017-10-12 | 2020-10-27 | 北京森泉伟业科技有限公司 | Method for preparing efficient catalyst by electrolytic manganese slag and catalyzing hydrogen peroxide to oxidize and degrade methylene blue |
| CN109046373A (en) * | 2018-07-24 | 2018-12-21 | 成都信息工程大学 | Heterogeneous class Fenotn catalyst CeO capable of magnetic separating2The preparation method and application of/MZFS |
| CN109046373B (en) * | 2018-07-24 | 2021-02-05 | 成都信息工程大学 | Magnetically separable heterogeneous Fenton-like catalyst CeO2Preparation method and application of/MZFS |
| CN111151289A (en) * | 2019-12-25 | 2020-05-15 | 浙江工商大学 | Manganese-based bimetallic oxide mesoporous material and preparation and application thereof |
| CN111151289B (en) * | 2019-12-25 | 2022-12-06 | 浙江工商大学 | Manganese-based bimetallic oxide mesoporous material and preparation and application thereof |
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