CN101318132A - Method for preparing supported nano-iron oxide/tripolite compound catalyst - Google Patents
Method for preparing supported nano-iron oxide/tripolite compound catalyst Download PDFInfo
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- CN101318132A CN101318132A CNA2007100284836A CN200710028483A CN101318132A CN 101318132 A CN101318132 A CN 101318132A CN A2007100284836 A CNA2007100284836 A CN A2007100284836A CN 200710028483 A CN200710028483 A CN 200710028483A CN 101318132 A CN101318132 A CN 101318132A
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Abstract
The invention provides a preparation method for a supported nano iron oxide/diatomite complex catalyst, which comprises the following steps: taking soluble ferric salt as the raw material, dissolving and dispersing the ferric salt in the water, adding alkali liquor to regulate the pH value to be 6-9, washing the obtained deposition, adding water and diatomite, allowing the weight percentage of the iron content in the ferric salt and the added diatomite to be 1.0 percent to 20 percent, uniformly stirring, roasting the solution at high temperature of 300-500 DEG C for 3-5 hours and obtaining the supported nano iron oxide /diatomite complex catalyst. The method has the advantages of low cost and simple steps and the obtained supported nano iron oxide/diatomite complex catalyst has the advantages of stability, small grain size, better settling ability and recycling.
Description
Technical field
The present invention relates to a kind of is matrix with diatomite, ferriferous oxide is prepared the preparation method of load supported nano-iron oxide/tripolite compound catalyst thereon.
Background technology
Supported nano-iron oxide/tripolite compound catalyst, be to be matrix with diatomite, ferriferous oxide is prepared load supported nano-iron oxide thereon, have characteristics such as surface area is big, surface-active functional group is more, mainly be to carry out reduction reaction or as catalyst, it has the oxidative degradation function to organic contact scar thing in the environment in chemical reaction.As a kind of environmental improvement material, have broad application prospects.
With respect to the ferriferous oxide that exists naturally, artificial synthetic ferriferous oxide mainly is a crystal habit, and (ZPC) is higher for zero point charge, but same, and surface area is big, surface-active functional group changeability more, electric charge is strong.These ferriferous oxides all have important effect to the absorption of nutrient in the soil and polluter, migration etc.
At present, the preparation nano-iron oxide can be synthesized by sluggish precipitation, sol-gel process, alkoxide hydrolysis, forced hydrolysis method, gas-phase decomposition method, microemulsion method etc.If the ferriferous oxide that is synthesized is carried out roasting under different temperatures and time condition, the crystal habit of sample, granular size, surface ion chemical state, catalytic performance etc. all there is bigger influence.
Summary of the invention
The objective of the invention is to propose a kind of supported nano-iron oxide/tripolite compound catalyst preparation method, it utilizes comparatively cheap diatomite of price and soluble ferric iron salt to be raw material, make full use of diatomaceous adsorption capacity, be prepared into supported nano-iron oxide/tripolite compound catalyst, to reduce the use cost of ferriferous oxide, improve catalytic effect, effect of settling and the range of application of iron oxidation catalyst as catalyst.
The method for preparing supported nano-iron oxide/tripolite compound catalyst proposed by the invention is as follows: be raw material with the soluble ferric iron salt, described molysite is dissolved dispersion in water, adding alkali lye adjusting pH is 6-9, obtain precipitation and after washing, add entry and diatomite, to add diatomaceous mass percent be 1.0%～20% to iron-holder with institute in the molysite, stir, promptly got supported nano-iron oxide/tripolite compound catalyst in 3～5 hours 300-500 ℃ of following high-temperature roasting.
The present invention is a weakly alkaline solution in order to the alkali lye of regulating soluble ferric iron salt dispersion liquid pH value, is good with ammoniacal liquor especially, can make the deposit seed that generates tiny, even and have residual alkali lye also can in heating process, remove in the system.The present invention need not with acid, and heating-up temperature and time are the key factors of preparation, the supported nano-iron oxide that can obtain than high stable in 3～5 hours at 300-500 ℃ of roasting temperature.
Described soluble ferric iron salt can be selected ferrous sulfate, ferric sulfate, ferric trichloride or ferrous chloride for use.
As seen the prepared supported nano-iron oxide/tripolite compound catalyst of the inventive method is done the test of X-ray powder diffraction and electron-microscope scanning, compared to independent diatomite diffraction curve, tangible ferriferous oxide peak (Fig. 1) is arranged on the diffraction curve of supported nano-iron oxide; In the diatomite substrate of porous, be adsorbed with a large amount of ferriferous oxides, and its particle diameter shows to have generated supported nano-iron oxide/tripolite compound catalyst (Fig. 2) all about 100nm.
Show also that through experiment this supported nano-iron oxide/tripolite compound catalyst can discharge iron ion (as shown in Figure 3) continually and steadily as source of iron in acid solution.
Do the test that source of iron is utilized Fenton's reaction degradation of organic substances repefral with this supported nano-iron oxide/tripolite compound catalyst, organic matter repefral concentration 20mg/l before the degraded, as seen the organic matter repefral concentration 2.5mg/l (as shown in Figure 4) after 120 minutes that degrades utilizes this supported nano-iron oxide to do the catalyst labile organic compound.
Useful technique effect provided by the present invention is: this method cost of material is cheap, and step is simple, and the gained supported nano-iron oxide/tripolite compound catalyst is stable, granularity is little, but settleability reuse is preferably arranged.
Description of drawings
Fig. 1 is the X-ray powder diffraction figure of supported nano-iron oxide/tripolite compound catalyst;
Fig. 2 is the sem photograph of supported nano-iron oxide/tripolite compound catalyst;
Fig. 3 is supported nano-iron oxide/tripolite compound catalyst iron ion stripping curve in acid solution;
Fig. 4 is a supported nano-iron oxide/tripolite compound catalyst degradation of organic substances degradation curve.
The specific embodiment
Embodiment one
The method for preparing supported nano-iron oxide/tripolite compound catalyst is as follows:
With ferrous sulfate (FeSO
4) be raw material, ferrous sulfate 0.75 is restrained stirring and dissolving in 200ml water, splashing into ammoniacal liquor is 6-7 to pH, suction filtration, precipitation is washed 6 times with distilled water, and is scattered in the 200ml water, adds 5g diatomite, after treating complete mixing,, get yellow powder in 400 ℃ of heating 4 hours.Wherein the content of ferriferous oxide is at 5%～8% (mass fraction).
Embodiment two
The method for preparing supported nano-iron oxide/tripolite compound catalyst is as follows:
With ferrous chloride (FeCl
2) be raw material, ferrous chloride 1.3 is restrained stirring and dissolving in 200ml water, splashing into ammoniacal liquor is 6-7 to pH, suction filtration, precipitation is washed 6 times with distilled water, and is scattered in the 200ml water, adds 5g diatomite, after treating complete mixing,, get buff powder in 500 ℃ of heating 3 hours.Wherein the content of ferriferous oxide is at 10%～15% (mass fraction).
Embodiment three
The method for preparing supported nano-iron oxide/tripolite compound catalyst is as follows:
With ferrous sulfate (Fe
2(SO
4)
3) be raw material, ferric sulfate 2 is restrained stirring and dissolving in 200ml water, splashing into ammoniacal liquor is 6-7 to pH, suction filtration, precipitation is with distilled water washing 6 times, and is scattered in the 200ml water, adds 5g diatomite, treat complete mixing after, in 400 ℃ of heating 3.5 hours, the yellowish-brown powder.Wherein the content of ferriferous oxide is at 15%～25% (mass fraction).
Embodiment four
The method for preparing supported nano-iron oxide/tripolite compound catalyst is as follows:
With ferric trichloride (FeCl
3) be raw material, ferric trichloride 2.9 is restrained stirring and dissolving in 400ml water, splashing into ammoniacal liquor is 6-7 to pH, suction filtration, precipitation is with distilled water washing 6 times, and is scattered in the 200ml water, adds 5g diatomite, treat complete mixing after, in 300 ℃ of heating 5 hours, brown powder.Wherein the content of ferriferous oxide is at 30%～35% (mass fraction).
Claims (4)
1. the preparation method of a supported nano-iron oxide/tripolite compound catalyst, it is characterized in that with the soluble ferric iron salt being raw material, described molysite is dissolved dispersion in water, adding alkali lye adjusting pH is 6-9, obtain precipitation and after washing, add entry and diatomite, to add diatomaceous mass percent be 1.0%～20% to iron-holder with institute in the molysite, stirs, and promptly got supported nano-iron oxide in 3～5 hours 300-500 ℃ of following high-temperature roasting.
2. the preparation method of supported nano-iron oxide/tripolite compound catalyst according to claim 1, the alkali lye that it is characterized in that regulating iron salt dispersion pH value is weakly alkaline solution.
3. the preparation method of supported nano-iron oxide/tripolite compound catalyst according to claim 2, the alkali lye that it is characterized in that regulating iron salt dispersion pH value is ammoniacal liquor.
4. the preparation method of supported nano-iron oxide/tripolite compound catalyst according to claim 1 is characterized in that described soluble ferric iron salt is ferrous sulfate, ferric sulfate, ferric trichloride or ferrous chloride.
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| CN2007100284836A CN101318132B (en) | 2007-06-08 | 2007-06-08 | Method for preparing supported nano-iron oxide/tripolite compound catalyst |
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| CN2007100284836A CN101318132B (en) | 2007-06-08 | 2007-06-08 | Method for preparing supported nano-iron oxide/tripolite compound catalyst |
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| CN101318132A true CN101318132A (en) | 2008-12-10 |
| CN101318132B CN101318132B (en) | 2010-09-01 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107983350A (en) * | 2017-11-03 | 2018-05-04 | 广东省资源综合利用研究所 | A kind of preparation method of heterogeneous Fenton catalyst |
| CN109395733A (en) * | 2018-12-04 | 2019-03-01 | 东北大学 | Fe2O3The preparation and the application in VOCs degradation for loading diatom soil ball catalysis material |
| CN110615518A (en) * | 2019-05-07 | 2019-12-27 | 中冶华天工程技术有限公司 | Fenton reaction ferrous iron slow release granule |
| CN111871413A (en) * | 2020-01-09 | 2020-11-03 | 长春工业大学 | Preparation and application of photocatalyst for degrading organic pollutants in water under alkaline condition |
Family Cites Families (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE2536488C2 (en) * | 1975-08-16 | 1977-08-25 | Ruhrchemie Ag | PROCESS FOR THE PRODUCTION OF UNSATATULATED HYDROCARBONS |
| CN1281495C (en) * | 2004-01-19 | 2006-10-25 | 复旦大学 | Method for preparing Fe-ZSM-5 zeolite microsphere using kieselguhr as raw material |
| CN100366342C (en) * | 2004-12-17 | 2008-02-06 | 南化集团研究院 | Catalyst for depriving nitrogen oxide under low temperature through reduction and preparation method |
| CN1970149A (en) * | 2006-12-07 | 2007-05-30 | 天津大学 | Bergmeal particle loaded nano TiO2 preparation method |
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2007
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107983350A (en) * | 2017-11-03 | 2018-05-04 | 广东省资源综合利用研究所 | A kind of preparation method of heterogeneous Fenton catalyst |
| CN109395733A (en) * | 2018-12-04 | 2019-03-01 | 东北大学 | Fe2O3The preparation and the application in VOCs degradation for loading diatom soil ball catalysis material |
| CN110615518A (en) * | 2019-05-07 | 2019-12-27 | 中冶华天工程技术有限公司 | Fenton reaction ferrous iron slow release granule |
| CN110615518B (en) * | 2019-05-07 | 2022-05-24 | 中冶华天工程技术有限公司 | Fenton reaction ferrous iron slow release granule |
| CN111871413A (en) * | 2020-01-09 | 2020-11-03 | 长春工业大学 | Preparation and application of photocatalyst for degrading organic pollutants in water under alkaline condition |
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| CN101318132B (en) | 2010-09-01 |
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