CN103230796A - Preparation method of attapulgite supported ferroferric oxide - Google Patents
Preparation method of attapulgite supported ferroferric oxide Download PDFInfo
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- CN103230796A CN103230796A CN2013101476275A CN201310147627A CN103230796A CN 103230796 A CN103230796 A CN 103230796A CN 2013101476275 A CN2013101476275 A CN 2013101476275A CN 201310147627 A CN201310147627 A CN 201310147627A CN 103230796 A CN103230796 A CN 103230796A
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Abstract
The invention relates to a preparation method of attapulgite supported ferroferric oxide, which is used for increasing the specific surface area of a Fe3O4 catalyst and improving the adsorption capacity of the catalyst surface to obtain better catalytic performance. The method takes attapulgite as a carrier and FeSO4.7H2O as an iron source, and comprises the following steps of: putting the attapulgite and FeSO4.7H2O at a mass ratio of (1:15)-(5:1) into a three-neck flask, adding a certain amount of water, and stirring for certain time under nitrogen protection at 40-80 DEG C; dropwise adding hydrogen peroxide with certain concentration according to a molar ratio of H2O2 to Fe<2+> of 1:3; adding a NaOH solution until pH is 10-13; transferring to a closed polytetrafluoroethylene reaction kettle; and settling for 8-16 hours at 120-200 DEG C. According to the method provided by the invention, the synthesized supported Fe3O4 has the advantages of simple method, low cost and large specific surface area, can form a Fenton's reagent with hydrogen peroxide, can effectively catalyze, oxidize and degrade organic wastewater to prevent secondary pollution, and is favorable for recovering and circularly utilizing the catalyst.
Description
Technical field:
The present invention relates to a kind of support type Fe
3O
4The preparation method, relate in particular to a kind of preparation method of attapulgite load tri-iron tetroxide.
Background technology:
Attapulgite (Attapulgite ATP) has another name called palygorskite or Palygorskite, be a kind of layer of chain structure contain Shuifu County's zeopan clay mineral, have unique dispersion, high temperature resistant, anti-good colloidal nature such as saline and alkaline and higher adsorption bleaching ability.Because inner porous road, specific area is big, is generally 146～210 m
2/ g, maximum can reach 500 m
2More than/the g, most cation, hydrone and a certain size polarity organic molecule all can directly be adsorbed in the duct.Because the structural property of attapulgite determines that it is a kind of very good catalyst carrier.
Traditional Fe
2+The Fenton reagent that ion and hydrogen peroxide are formed can produce a large amount of hydroxyl radical free radicals, though it is good to be used for the treatment effect of organic wastewater, but causes secondary pollution to water.Fe
3O
4As a kind of heterogeneous catalysis, can form the class Fenton reagent with hydrogen peroxide, not only have good catalytic performance, and because Fe
3O
4Exist magnetic to be easier to from aqueous systems, separate, prevent the secondary pollution of water body.Because Fe
3O
4Less (35.25 m of specific area
2/ g), and less with the hydrogen peroxide touch opportunity in water body, the situation of the invalid decomposition of part hydrogen peroxide can take place.
Summary of the invention:
The object of the present invention is to provide a kind of preparation method of attapulgite load tri-iron tetroxide, problem to be solved is to improve Fe
3O
4The specific area of catalyst, the adsorption capacity of raising catalyst surface has made it better catalytic performance.
A kind of preparation method of attapulgite load tri-iron tetroxide is characterized in that, carrier is attapulgite, FeSO
47H
2O is source of iron, attapulgite and Fe
3O
4Mass ratio is 1:3～5:1, and the key step of its preparation method comprises: (1) is with attapulgite powder and FeSO
47H
2O is hybridly prepared into the aqueous solution, makes attapulgite fully adsorb Fe
2+(2) H in molar ratio
2O
2: Fe
2+=1:3 is added dropwise to the hydrogen peroxide of mass concentration 10%～30%, and temperature is 40～80 ℃; (3) dripping NaOH solution and carry out sedimentation, is 10～13 until the pH of reaction system, in 120～200 ℃ of following sedimentation 8～16h.
This preparation method's concrete steps are:
(1) 200 mesh sieves are crossed in the Concave-convex clay rod ore deposit after fragmentation, grinding, it is standby to obtain the canescence powder;
(2) use FeSO
47H
2The amount of O is calculated Fe
3O
4Theoretical yield;
(3) in the 100mL there-necked flask, feed N
2Behind the air, add the attapulgite powder that 2g gets ready in the eliminating bottle, add the FeSO of certain mass
47H
2O, the quality of attapulgite and the Fe that gets as calculated
3O
4The ratio of theoretical yield is between 1:3～5:1;
(4) add 20mL distilled water, in 40～80 ℃ of water-baths, add thermal agitation 20min, make attapulgite fully adsorb Fe
2+
(5) according to mol ratio H
2O
2: Fe
2+=1:3 drips hydrogen peroxide in there-necked flask, hydrogen peroxide is added dropwise to complete the back and continues reaction 10min;
(6) dripping NaOH solution in there-necked flask, is 10～13 until the pH of reaction system, continues reaction 10min;
(7) system in the there-necked flask all is transferred in the polytetrafluoroethylene (PTFE) reactor, reacts 8～16 h down in 120～200 ℃;
(8) carry out filtering and washing until neutrality after reaction is finished, after 40～60 ℃ of following dryings, pulverize.
The present invention is at the synthetic Fe of hydro-thermal coprecipitation
3O
4Add attapulgite in the process, the Fe of synthetic support type
3O
4Catalyst, this support type Fe
3O
4Ratio is the Fe of load not
3O
4Have bigger specific area, easier catalysis hydrogen peroxide produces hydroxyl radical free radical; Because attapulgite itself has very strong absorption property, polar organic matter can be adsorbed in the catalyst duct, can be rapidly and Fe
3O
4The hydroxyl free radical reaction that catalysis produces reaches the purpose of degradation of organic substances, has significantly reduced the invalid decomposition of hydrogen peroxide.
Compared with prior art beneficial effect of the present invention is embodied in:
1, at attapulgite load Fe
3O
4In the preparation process, except the process of preliminary treatment attapulgite, with the synthetic Fe of hydro-thermal coprecipitation
3O
4Process compare, do not increase miscellaneous equipment and operating procedure;
2, the Fe of support type
3O
4With the Fe of load not
3O
4, have bigger specific area, also corresponding increase of adsorption capacity simultaneously, and improved the performance of catalytic oxidation;
3, preparation method of the present invention simple, to equipment require little, feasibility is strong, but also prepared in batches attapulgite load type Fe
3O
4
Description of drawings:
Fig. 1 is Fe
3O
4X-ray diffraction XRD figure;
Fig. 2 is the XRD figure of attapulgite;
Fig. 3 is attapulgite load Fe
3O
4XRD figure;
Fig. 4 is load Fe not
3O
4Transmission electron microscope TEM figure;
Fig. 5 is attapulgite load Fe
3O
4TEM figure.
The specific embodiment:
For technological means, creation characteristic that the present invention is realized, reach purpose and effect is easy to understand, below in conjunction with concrete diagram and specific embodiment, further set forth the present invention, but be not to limit protection scope of the present invention.
Characteristic peak and Fe as can be seen among Fig. 1
3O
4Standard card (PDF ﹣ #19-0629) basically identical, and do not have other impurity peaks, but index turns to Fe
3O
4Half-peak breadth in the spectrogram is bigger, is because Fe
3O
4The less reason of the crystal grain of catalyst causes.Choose five diffraction maximums the strongest, (in the formula: d is particle diameter, α=0.89 by Scherrer (Scherrer) formula d=α λ cos θ/β, λ=0.154056 nm, β is halfwidth, and θ is the angle of diffraction) calculate the size of particle diameter respectively, and to obtain its average grain diameter be 26 nm.
Peak position is consistent with PDF-#31-0783 card peak position in Fig. 2, be the attapulgite crystal, and peak intensity is bigger.Choose five diffraction maximums the strongest, calculate the size of particle diameter respectively by the Scherrer formula, and to obtain its average grain diameter be about 15 nm.
Two groups of diffraction maximums are arranged among Fig. 3, but index turns to PDF-#31-0783 and PDF ﹣ #19-0629, i.e. attapulgite and Fe respectively
3O
4Two kinds of crystal have formed attapulgite load Fe
3O
4Structure.Choose five diffraction maximums the strongest among Fig. 3, calculate the size of particle diameter respectively by the Scherrer formula, and to obtain its average grain diameter be about 21 nm.
Fig. 4 is prepared not load Fe
3O
4The transmission electron microscope photo of catalyst.Mainly present spherical or subglobose graininess pattern among the figure, size is comparatively even, and the surface is comparatively smooth, and dispersive property is better, measures its size between 25～35 nm, and this matches with the particle diameter that calculates through the Scherrer formula.
Fig. 5 is attapulgite load Fe
3O
4TEM figure, Fe
3O
4Granular size is more consistent, and particle diameter is between 21～25nm.
Embodiment 1: duty factor is the attapulgite load Fe of 2:1.13
3O
4Preparation
1, Concave-convex clay rod (official mountain, Mingguang City, Anhui Province attapulgite clay pit) is crossed 200 mesh sieves after fragmentation, grinding, it is standby to obtain the canescence powder;
2, in 100 mL there-necked flasks, feed N
2Behind the air, add the attapulgite powder that 2g gets ready in the eliminating bottle, add the FeSO of 4.06 g
47H
2O adds 30 mL distilled water, adds thermal agitation 20 min in 60 ℃ of water-baths, makes attapulgite fully adsorb Fe
2+
3, being added dropwise to 3 mL mass fractions is 10% hydrogen peroxide, is added dropwise to complete the back and continues reaction 10 min;
4, dripping the NaOH solution of 1 mol/L in there-necked flask, is 12 until the pH of reaction system, continues reaction 10 min;
5, the system in the there-necked flask all is transferred in the polytetrafluoroethylene (PTFE) reactor, reacts 11h down in 180 ℃; Carry out filtering and washing until neutrality after reaction is finished, after 60 ℃ of following dryings, pulverize.
Embodiment 2: duty factor is the attapulgite load Fe of 1:2
3O
4Preparation
1, Concave-convex clay rod (official mountain, Mingguang City, Anhui Province attapulgite clay pit) is crossed 200 mesh sieves after fragmentation, grinding, it is standby to obtain the canescence powder;
2, in 100 mL there-necked flasks, feed N
2Behind the air, add the attapulgite powder that 1 g gets ready in the eliminating bottle, add the FeSO of 7.2 g
47H
2O adds 40 mL distilled water, adds thermal agitation 20 min in 60 ℃ of water-baths, makes attapulgite fully adsorb Fe
2+
3, being added dropwise to 1 mL mass fraction is 16.8% hydrogen peroxide, is added dropwise to complete the back and continues reaction 10 min;
4, dripping the NaOH solution of 2 mol/L in there-necked flask, is 13 until the pH of reaction system, continues reaction 10 min;
5, the system in the there-necked flask all is transferred in the polytetrafluoroethylene (PTFE) reactor, reacts 12h down in 170 ℃; Reaction is carried out filtering and washing until neutrality after finishing, dry by grind powdery solid.
Embodiment 3: attapulgite load Fe
3O
4The performance of catalyzing oxidizing degrading methylene blue.
In 250 mL there-necked flasks, adding 100 mL concentration is 250 μ mol/L methylene blue solutions, and regulating its pH is 4, adds 0.1g attapulgite load Fe
3O
4Catalyst (duty factor 3:1) adds thermal agitation in 60 ℃ of water-baths.Be added dropwise to the hydrogen peroxide of 1 mL mass fraction 17%, react 40 min, detect remaining methylene blue concentration (spectrophotometer detects with 10 mm cuvettes at 664 nm places, and detecting needs the drawing curve).Be provided with two groups of contrast experiments: one group only adds catalyst and does not add hydrogen peroxide, and one group only adds hydrogen peroxide and do not add catalyst, methylene blue residual quantity (μ mol/L) result such as following table in the water after reaction a period of time:
Embodiment 4: attapulgite load Fe
3O
4The performance of catalyzing oxidizing degrading phenol.
In 250 mL there-necked flasks, adding 100 mL concentration is 216 mg/L phenol solution, and regulating its pH is 3, adds 0.3 g attapulgite load Fe
3O
4Catalyst (duty factor 2:1.13) adds thermal agitation in 60 ℃ of water-baths.Be added dropwise to the hydrogen peroxide of 1 mL mass fraction 10% every 10 min; add 5 mL altogether; adopting 4-amino-antipyrine AAS (the state environment protecting standard HJ of the People's Republic of China (PRC) 503-2009) to detect phenol concentration is 0.45 mg/L, phenol clearance 99.8%.
Embodiment 5: attapulgite load Fe
3O
4The performance of catalyzing oxidizing degrading metanitrophenol.
In 250 mL there-necked flasks, adding 100 mL concentration is 256 mg/L m-nitro phenol solutions, and regulating its pH is 3, adds 0.4g attapulgite load Fe
3O
4Catalyst (duty factor 2:1) adds thermal agitation in 65 ℃ of water-baths.Be added dropwise to the hydrogen peroxide of 1 mL mass fraction 30% every 10 min, add 6 mL altogether, gas chromatographic detection metanitrophenol concentration is 5 mg/L, metanitrophenol clearance 98.0%.
Embodiment 6: attapulgite load Fe
3O
4The performance of catalyzing oxidizing degrading hydroquinones.
In 250 mL there-necked flasks, adding 100 mL concentration is 300 mg/L hydroquinones solution, and regulating its pH is 4, adds 0.2g attapulgite load Fe
3O
4Catalyst (duty factor 1:1.13) adds thermal agitation in 70 ℃ of water-baths.Be added dropwise to the hydrogen peroxide of 1 mL mass fraction 30% every 10 min, add 4 mL altogether, gas chromatographic detection hydroquinones concentration is 0.3 mg/L, hydroquinones clearance 99.9%.
It should be noted that at last: above embodiment is only in order to illustrate the present invention and unrestricted technical scheme described in the invention; Therefore, although this specification has been described in detail with reference to above-mentioned the present invention of each embodiment,, those of ordinary skill in the art should be appreciated that still and can make amendment or be equal to replacement the present invention; And all do not break away from technical scheme and the improvement thereof of the spirit and scope of the present invention, and it all should be encompassed in the claim scope of the present invention.
Claims (2)
1. the preparation method of an attapulgite load tri-iron tetroxide is characterized in that, carrier is attapulgite, FeSO
47H
2O is source of iron, attapulgite and Fe
3O
4Mass ratio is 1:3～5:1, and the key step of its preparation method comprises: (1) is with attapulgite powder and FeSO
47H
2O is hybridly prepared into the aqueous solution, makes attapulgite fully adsorb Fe
2+(2) H in molar ratio
2O
2: Fe
2+=1:3 is added dropwise to the hydrogen peroxide of mass concentration 10%～30%, and temperature is 40～80 ℃; (3) dripping NaOH solution and carry out sedimentation, is 10～13 until the pH of reaction system, in 120～200 ℃ of following sedimentation 8～16h.
2. the preparation method of attapulgite load tri-iron tetroxide according to claim 1 is characterized in that, this preparation method's concrete steps are:
(1) 200 mesh sieves are crossed in the Concave-convex clay rod ore deposit after fragmentation, grinding, it is standby to obtain the canescence powder;
(2) use FeSO
47H
2The amount of O is calculated Fe
3O
4Theoretical yield;
(3) in the 100mL there-necked flask, feed N
2Behind the air, add the attapulgite powder that 2g gets ready in the eliminating bottle, add the FeSO of certain mass
47H
2O, the quality of attapulgite and the Fe that gets as calculated
3O
4The ratio of theoretical yield is between 1:3～5:1;
(4) add 20mL distilled water, in 40～80 ℃ of water-baths, add thermal agitation 20min, make attapulgite fully adsorb Fe
2+
(5) according to mol ratio H
2O
2: Fe
2+=1:3 drips hydrogen peroxide in there-necked flask, hydrogen peroxide is added dropwise to complete the back and continues reaction 10min;
(6) dripping NaOH solution in there-necked flask, is 10～13 until the pH of reaction system, continues reaction 10min;
(7) system in the there-necked flask all is transferred in the polytetrafluoroethylene (PTFE) reactor, reacts 8～16 h down in 120～200 ℃;
(8) carry out filtering and washing until neutrality after reaction is finished, after 40～60 ℃ of following dryings, pulverize.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104310568A (en) * | 2014-11-07 | 2015-01-28 | 华东理工大学 | Wastewater treatment method by utilizing Fenton reaction |
| CN104399486A (en) * | 2014-12-02 | 2015-03-11 | 安徽星宇化工有限公司 | Preparation method for manganese dioxide composite catalyst and synthetic method for 2-pyridylaldehyde |
| CN105776738A (en) * | 2016-03-22 | 2016-07-20 | 中国环境科学研究院 | Method and device for pre-treating organic wastewater |
| CN105859019A (en) * | 2016-03-22 | 2016-08-17 | 中国环境科学研究院 | Treating and recycling method and apparatus for organic wastewater |
| CN106693971A (en) * | 2016-12-14 | 2017-05-24 | 河南理工大学 | Preparation method of heterogeneous Fenton catalyst taking opoka as carrier |
| CN109896549A (en) * | 2019-03-12 | 2019-06-18 | 淮阴工学院 | The preparation method of fibrous amorphous state di-iron trioxide |
| CN110092505A (en) * | 2019-05-26 | 2019-08-06 | 北京化工大学 | A kind of method of Concave-convex clay rod processing wastewater containing phenol |
| CN110252304A (en) * | 2018-03-12 | 2019-09-20 | 中国石油化工股份有限公司 | Fe-series catalyst and its preparation method and application and carbon nanotube and preparation method thereof |
| CN110817893A (en) * | 2019-11-14 | 2020-02-21 | 淮阴工学院 | Preparation method of iron-doped attapulgite photoelectric material |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104310568A (en) * | 2014-11-07 | 2015-01-28 | 华东理工大学 | Wastewater treatment method by utilizing Fenton reaction |
| CN104399486A (en) * | 2014-12-02 | 2015-03-11 | 安徽星宇化工有限公司 | Preparation method for manganese dioxide composite catalyst and synthetic method for 2-pyridylaldehyde |
| US10501355B2 (en) | 2016-03-22 | 2019-12-10 | Chinese Research Academy Of Environmental Sciences | Method for treating and recycling organic wastewater and apparatus |
| CN105859019A (en) * | 2016-03-22 | 2016-08-17 | 中国环境科学研究院 | Treating and recycling method and apparatus for organic wastewater |
| WO2017161640A1 (en) * | 2016-03-22 | 2017-09-28 | 中国环境科学研究院 | Method for treating and recycling organic wastewater and apparatus |
| CN105776738A (en) * | 2016-03-22 | 2016-07-20 | 中国环境科学研究院 | Method and device for pre-treating organic wastewater |
| CN106693971A (en) * | 2016-12-14 | 2017-05-24 | 河南理工大学 | Preparation method of heterogeneous Fenton catalyst taking opoka as carrier |
| CN110252304A (en) * | 2018-03-12 | 2019-09-20 | 中国石油化工股份有限公司 | Fe-series catalyst and its preparation method and application and carbon nanotube and preparation method thereof |
| CN110252304B (en) * | 2018-03-12 | 2021-12-17 | 中国石油化工股份有限公司 | Iron-based catalyst, preparation method and application thereof, carbon nano tube and preparation method thereof |
| CN109896549A (en) * | 2019-03-12 | 2019-06-18 | 淮阴工学院 | The preparation method of fibrous amorphous state di-iron trioxide |
| CN109896549B (en) * | 2019-03-12 | 2021-04-23 | 淮阴工学院 | Preparation method of fibrous amorphous ferric oxide |
| CN110092505A (en) * | 2019-05-26 | 2019-08-06 | 北京化工大学 | A kind of method of Concave-convex clay rod processing wastewater containing phenol |
| CN110817893A (en) * | 2019-11-14 | 2020-02-21 | 淮阴工学院 | Preparation method of iron-doped attapulgite photoelectric material |
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Application publication date: 20130807 |