CN107265508A - A kind of self assembly sea urchin shape α FeOOH preparation method - Google Patents

A kind of self assembly sea urchin shape α FeOOH preparation method Download PDF

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Publication number
CN107265508A
CN107265508A CN201710568021.7A CN201710568021A CN107265508A CN 107265508 A CN107265508 A CN 107265508A CN 201710568021 A CN201710568021 A CN 201710568021A CN 107265508 A CN107265508 A CN 107265508A
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China
Prior art keywords
product
feooh
sea urchin
solution
self assembly
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CN201710568021.7A
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Chinese (zh)
Inventor
曹丽云
马萌
齐慧
李嘉胤
黄剑锋
吴桂娟
陈文卓
姚恺
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Shaanxi University of Science and Technology
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Shaanxi University of Science and Technology
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Priority to CN201710568021.7A priority Critical patent/CN107265508A/en
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G49/00—Compounds of iron
    • C01G49/02—Oxides; Hydroxides
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
    • C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/30—Particle morphology extending in three dimensions
    • C01P2004/32—Spheres
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/50—Agglomerated particles

Abstract

A kind of self assembly sea urchin shape α FeOOH preparation method, by deionized water and glycerol solution A；Analytically pure soluble ferric iron salt ferrous sulfate is dissolved in solution A, stirring makes molysite fully dissolve to obtain solution B；Solution B is poured into polytetrafluoroethylene (PTFE) water heating kettle liner, hydrothermal reaction kettle is then sealed, put it into microwave hydrothermal reactor, reaction naturally cools to room temperature after terminating, by products therefrom C；Product C is washed with washing, alcohol respectively, the product after washing is dispersed in water to obtain product D；Self assembly sea urchin shape α FeOOH products finally are obtained after product D is freeze-dried.The present invention is ingenious to apply microwave solvothermal method, and method is simple, time-consuming short, with low cost, it is easy to accomplish；By regulating and controlling the ratio of water and glycerine, to adjust self assembly sea urchin shape α FeOOH particle diameter and pattern.

Description

A kind of preparation method of self assembly sea urchin shape alpha-feooh
Technical field
The invention belongs to electrochemical technology field, and in particular to a kind of preparation method of self assembly sea urchin shape alpha-feooh.
Background technology
Alpha-feooh (goethite type FeOOH) is important part in ferriferous oxide, due to its high power capacity (> 1000mAh/g), abundant natural resources, non-toxic and low cost, are considered as that having for negative material of new generation is uncommon for a long time The candidate of prestige.At present, the method for preparing ferriferous oxide is varied, can be divided into liquid phase method, gas according to the difference of preparing raw material Phase method and solid phase method.Liquid phase method is because equipment is simple, raw material is readily available, purity high, uniformity is good, chemical composition precise control The advantages of, using more extensive.Liquid phase method mainly includes Hydrolyze method, the precipitation method, hydro-thermal method, solvent-thermal method and sol-gal process Deng.In recent years, study hotspot of the appearance as nano material preparation technology of hydro-thermal method and solvent-thermal method.Perhaps pretty dove et al. is (high Deng the chemical journal of school, 2015, Isosorbide-5-Nitrae 5-54) using ferrous sulfate, urea and ethanol as raw material, flowed back using the step of low-temperature atmosphere-pressure one Method is prepared for the alpha-FeOOH nano material with three-dimensional flower-shaped structure；Ou Ping et al. (Materials Letters, 2008,62, The alpha-feooh nano wire of extensive uniform diameters and high aspect ratio, but two 914-917) have been synthesized at 100 DEG C using hydro-thermal method Person is respectively provided with the shortcoming of reaction time consumption length, need to further shorten the reaction time.
The content of the invention
Microwave solvothermal method is used it is an object of the invention to provide one kind, self assembly sea urchin shape is prepared within a short period of time The method of alpha-feooh.
To reach above-mentioned purpose, the technical solution adopted by the present invention is as follows：
1) by deionized water and glycerine with 3~9：1 volume ratio prepares solution A；
2) analytically pure soluble ferric iron salt ferrous sulfate is dissolved in solution A, stirring makes molysite fully dissolve to obtain iron Salinity is 0.05~2mol/L solution B；
3) solution B is poured into polytetrafluoroethylene (PTFE) water heating kettle liner, then seals hydrothermal reaction kettle, put it into Microwave Water In thermal reactor, reaction temperature control is at 80~200 DEG C, and reaction time control naturally cools to room in 1~3h, reaction after terminating Temperature, by products therefrom C；
4) product C is washed with washing, alcohol respectively, the product after washing is dispersed in water to obtain product D；
5) by product D in being freeze-dried at -40 DEG C, holding vacuum is 10~60Pa, and dried sample is final Self assembly sea urchin shape alpha-feooh product.
The step 3) water heating kettle compactedness be 30%-80%.
The step 4) washing washed respectively using centrifuge, alcohol is washed 3 times, each 1~4min of centrifugation time, centrifugation turn Speed is 3000~9000rpm.
The step 5) drying time be 10~20h.
Beneficial effects of the present invention are embodied in：
1) present invention is ingenious applies microwave solvothermal method, and method is simple, time-consuming short, with low cost, it is easy to accomplish；
2) by regulating and controlling the ratio of water and glycerine, to adjust the particle diameter and pattern of self assembly sea urchin shape alpha-feooh.
Brief description of the drawings
Fig. 1 is that product particles Rigaku D/max2000PCX- x ray diffractometer xs analysis sample prepared by embodiment 1 shines Piece.
Fig. 2, Fig. 3 and Fig. 4 are that the JSM-6700F types scanning electron that product prepared by embodiment 1 is produced with Japanese firm shows Micro mirror photo.
Fig. 5, Fig. 6 and Fig. 7 are that the JSM-6700F types scanning electron that product prepared by embodiment 2 is produced with Japanese firm shows Micro mirror photo.
Embodiment
Embodiment 1：
1) by deionized water and glycerine with 7：1 volume ratio prepares solution A；
2) analytically pure soluble ferric iron salt ferrous sulfate is dissolved in solution A, stirring makes molysite fully dissolve to obtain iron Salinity is 1mol/L solution B；
3) solution B is poured into polytetrafluoroethylene (PTFE) water heating kettle liner, compactedness is controlled 50%, then seals hydro-thermal reaction Kettle, puts it into microwave hydrothermal reactor, and reaction temperature control is at 80 DEG C, and reaction time control is reacted after terminating certainly in 3h Room temperature so is cooled to, by products therefrom C；
4) product C is washed respectively using centrifuge, alcohol is washed 3 times, each centrifugation time 1min, centrifugal rotational speed is 9000rpm, product D is dispersed in water to obtain by the product after washing；
5) by product D in being freeze-dried at -40 DEG C, holding vacuum is 10Pa, dries 20h, and dried sample is Final self assembly sea urchin shape alpha-feooh product.
Product can be had an optimistic view of out for goethite type FeOOH, i.e. alpha-feooh by Fig. 1, card serial number PDF#29-0713.
It can be seen that the made alpha-feooh product of the present embodiment is assembled into by even rod by Fig. 2, Fig. 3 and Fig. 4 Sea urchin sphere, the wide about 20~30nm of nanometer rods is about 200~300nm, the diameter of sea urchin sphere be distributed in 1~3um it Between.
Embodiment 2：
1) by deionized water and glycerine with 3：1 volume ratio prepares solution A；
2) analytically pure soluble ferric iron salt ferrous sulfate is dissolved in solution A, stirring makes molysite fully dissolve to obtain iron Salinity is 0.8mol/L solution B；
3) solution B is poured into polytetrafluoroethylene (PTFE) water heating kettle liner, compactedness is controlled 60%, then seals hydro-thermal reaction Kettle, puts it into microwave hydrothermal reactor, and reaction temperature control is at 150 DEG C, and reaction time control is reacted after terminating certainly in 2h Room temperature so is cooled to, by products therefrom C；
4) product C is washed respectively using centrifuge, alcohol is washed 3 times, each centrifugation time 4min, centrifugal rotational speed is 7000rpm, product D is dispersed in water to obtain by the product after washing；
5) by product D in being freeze-dried at -40 DEG C, holding vacuum is 15Pa, dries 15h, and dried sample is Final self assembly sea urchin shape alpha-feooh product.
It can be seen that the made alpha-feooh product of the present embodiment is assembled into by even rod by Fig. 5, Fig. 6 and Fig. 7 Sea urchin sphere, the wide about 10~20nm of nanometer rods, is about 100~200nm, and the diameter of sea urchin sphere is distributed in 0.5~1.5um Between.It can be seen that, with the increase of glycerine ratio, the volume of Sea urchin ball is gradually reduced.
Embodiment 3：
1) by deionized water and glycerine with 5：1 volume ratio prepares solution A；
2) analytically pure soluble ferric iron salt ferrous sulfate is dissolved in solution A, stirring makes molysite fully dissolve to obtain iron Salinity is 2mol/L solution B；
3) solution B is poured into polytetrafluoroethylene (PTFE) water heating kettle liner, compactedness is controlled 30%, then seals hydro-thermal reaction Kettle, puts it into microwave hydrothermal reactor, and reaction temperature control is at 200 DEG C, and reaction time control is reacted after terminating certainly in 1h Room temperature so is cooled to, by products therefrom C；
4) product C is washed respectively using centrifuge, alcohol is washed 3 times, each centrifugation time 3min, centrifugal rotational speed is 5000rpm, product D is dispersed in water to obtain by the product after washing；
5) by product D in being freeze-dried at -40 DEG C, holding vacuum is 60Pa, dries 20h, and dried sample is Final self assembly sea urchin shape alpha-feooh product.
Embodiment 4：
1) by deionized water and glycerine with 9：1 volume ratio prepares solution A；
2) analytically pure soluble ferric iron salt ferrous sulfate is dissolved in solution A, stirring makes molysite fully dissolve to obtain iron Salinity is 0.05mol/L solution B；
3) solution B is poured into polytetrafluoroethylene (PTFE) water heating kettle liner, compactedness is controlled 80%, then seals hydro-thermal reaction Kettle, puts it into microwave hydrothermal reactor, and reaction temperature control is at 180 DEG C, and reaction time control is in 1.5h, after reaction terminates Room temperature is naturally cooled to, by products therefrom C；
4) product C is washed respectively using centrifuge, alcohol is washed 3 times, each centrifugation time 4min, centrifugal rotational speed is 3000rpm, product D is dispersed in water to obtain by the product after washing；
5) by product D in being freeze-dried at -40 DEG C, holding vacuum is 25Pa, dries 10h, and dried sample is Final self assembly sea urchin shape alpha-feooh product.

Claims (4)

1. a kind of preparation method of self assembly sea urchin shape alpha-feooh, it is characterised in that：
1) by deionized water and glycerine with 3~9：1 volume ratio prepares solution A；
2) analytically pure soluble ferric iron salt ferrous sulfate is dissolved in solution A, stirring molysite is fully dissolved to obtain molysite dense Spend the solution B for 0.05~2mol/L；
3) solution B is poured into polytetrafluoroethylene (PTFE) water heating kettle liner, then seals hydrothermal reaction kettle, put it into microwave hydrothermal anti- Answer in device, reaction temperature control is at 80~200 DEG C, and reaction time control naturally cools to room temperature in 1~3h, reaction after terminating, By products therefrom C；
4) product C is washed with washing, alcohol respectively, the product after washing is dispersed in water to obtain product D；
5) by product D in being freeze-dried at -40 DEG C, holdings vacuum is 10~60Pa, and dried sample is final oneself Assemble sea urchin shape alpha-feooh product.
2. a kind of preparation method of self assembly sea urchin shape alpha-feooh according to claim 1, it is characterised in that：The step Rapid 3) water heating kettle compactedness is 30%-80%.
3. a kind of preparation method of self assembly sea urchin shape alpha-feooh according to claim 1, it is characterised in that：The step Rapid washing 4) is washed respectively using centrifuge, alcohol is washed 3 times, each 1~4min of centrifugation time, centrifugal rotational speed be 3000~ 9000rpm。
4. a kind of preparation method of self assembly sea urchin shape alpha-feooh according to claim 1, it is characterised in that：The step Rapid 5) drying time is 10~20h.
CN201710568021.7A 2017-07-13 2017-07-13 A kind of self assembly sea urchin shape α FeOOH preparation method Pending CN107265508A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108927101A (en) * 2018-07-06 2018-12-04 济南大学 A kind of acicular nanometer FeOOH adsorbent and preparation method thereof
CN109852993A (en) * 2019-02-18 2019-06-07 山东大学 Ferrite oxygen-separating catalyst, preparation method and its electro-catalysis based on eutectic solvent analyse oxygen application
RU2748801C1 (en) * 2020-11-03 2021-05-31 федеральное государственное бюджетное образовательное учреждение высшего образования «Оренбургский государственный университет» Method for obtaining goethite
CN114563451A (en) * 2022-03-08 2022-05-31 浙江大学 Water body heavy metal real-time detection device and method based on iron oxyhydroxide nano material

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101734726A (en) * 2009-12-15 2010-06-16 浙江师范大学 Method for preparing urchin-shaped hydroxyferric oxide and urchin-shaped ferric oxide nano material
CN102153146A (en) * 2011-04-18 2011-08-17 中国科学院化学研究所 Method for controllably preparing hydroxyl oxidize iron, iron sesquioxide and ferroferric oxide

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101734726A (en) * 2009-12-15 2010-06-16 浙江师范大学 Method for preparing urchin-shaped hydroxyferric oxide and urchin-shaped ferric oxide nano material
CN102153146A (en) * 2011-04-18 2011-08-17 中国科学院化学研究所 Method for controllably preparing hydroxyl oxidize iron, iron sesquioxide and ferroferric oxide

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
BAO WANG ET AL.: ""Template-free Formation of Uniform Urchin-like α-FeOOH Hollow Spheres with Superior Capability for Water Treatment"", 《ADV. MATER.》 *

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108927101A (en) * 2018-07-06 2018-12-04 济南大学 A kind of acicular nanometer FeOOH adsorbent and preparation method thereof
CN109852993A (en) * 2019-02-18 2019-06-07 山东大学 Ferrite oxygen-separating catalyst, preparation method and its electro-catalysis based on eutectic solvent analyse oxygen application
CN109852993B (en) * 2019-02-18 2019-12-24 山东大学 Iron alkoxide oxygen evolution catalyst based on eutectic solvent, preparation method and electrocatalytic oxygen evolution application thereof
RU2748801C1 (en) * 2020-11-03 2021-05-31 федеральное государственное бюджетное образовательное учреждение высшего образования «Оренбургский государственный университет» Method for obtaining goethite
CN114563451A (en) * 2022-03-08 2022-05-31 浙江大学 Water body heavy metal real-time detection device and method based on iron oxyhydroxide nano material

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Application publication date: 20171020