CN106517130B - A method of di iron micro-nano powder material is prepared with rich phosphorus biomass - Google Patents
A method of di iron micro-nano powder material is prepared with rich phosphorus biomass Download PDFInfo
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- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 74
- 239000000463 material Substances 0.000 title claims abstract description 30
- 229910052742 iron Inorganic materials 0.000 title claims abstract description 29
- 239000011858 nanopowder Substances 0.000 title claims abstract description 28
- 229910052698 phosphorus Inorganic materials 0.000 title claims abstract description 20
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 239000011574 phosphorus Substances 0.000 title claims abstract description 19
- 239000002028 Biomass Substances 0.000 title claims abstract description 17
- 238000000034 method Methods 0.000 title claims abstract description 17
- 238000006243 chemical reaction Methods 0.000 claims abstract description 24
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 claims abstract description 14
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 10
- 210000000988 bone and bone Anatomy 0.000 claims abstract description 9
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims abstract description 7
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims abstract description 4
- 239000007864 aqueous solution Substances 0.000 claims abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 239000000243 solution Substances 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000005119 centrifugation Methods 0.000 claims description 4
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 238000003760 magnetic stirring Methods 0.000 claims description 4
- 238000012545 processing Methods 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- 229910001220 stainless steel Inorganic materials 0.000 claims description 4
- 239000010935 stainless steel Substances 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 238000011049 filling Methods 0.000 claims description 3
- 238000002604 ultrasonography Methods 0.000 claims 1
- 241000251468 Actinopterygii Species 0.000 abstract description 8
- 239000011807 nanoball Substances 0.000 abstract description 7
- 239000002994 raw material Substances 0.000 abstract description 7
- 238000009826 distribution Methods 0.000 abstract description 6
- 239000000843 powder Substances 0.000 abstract description 6
- 241001465754 Metazoa Species 0.000 abstract description 5
- 239000007772 electrode material Substances 0.000 abstract description 4
- 239000002245 particle Substances 0.000 abstract description 4
- 239000003054 catalyst Substances 0.000 abstract description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 abstract description 2
- 239000012620 biological material Substances 0.000 abstract description 2
- 238000012512 characterization method Methods 0.000 abstract description 2
- 229910052744 lithium Inorganic materials 0.000 abstract description 2
- 239000002086 nanomaterial Substances 0.000 abstract description 2
- 230000003287 optical effect Effects 0.000 abstract description 2
- 239000000047 product Substances 0.000 description 24
- 238000002360 preparation method Methods 0.000 description 19
- 229910019142 PO4 Inorganic materials 0.000 description 16
- 238000010521 absorption reaction Methods 0.000 description 7
- 230000001699 photocatalysis Effects 0.000 description 7
- 238000007146 photocatalysis Methods 0.000 description 6
- 238000002835 absorbance Methods 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000000921 elemental analysis Methods 0.000 description 2
- 238000005286 illumination Methods 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- CXKWCBBOMKCUKX-UHFFFAOYSA-M methylene blue Chemical compound [Cl-].C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 CXKWCBBOMKCUKX-UHFFFAOYSA-M 0.000 description 2
- 229960000907 methylthioninium chloride Drugs 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 238000000634 powder X-ray diffraction Methods 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- VTLYFUHAOXGGBS-UHFFFAOYSA-N Fe3+ Chemical class [Fe+3] VTLYFUHAOXGGBS-UHFFFAOYSA-N 0.000 description 1
- 229910052493 LiFePO4 Inorganic materials 0.000 description 1
- DMGNFLJBACZMRM-UHFFFAOYSA-N O[P] Chemical compound O[P] DMGNFLJBACZMRM-UHFFFAOYSA-N 0.000 description 1
- 240000007817 Olea europaea Species 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000011805 ball Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000010835 comparative analysis Methods 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 229910000399 iron(III) phosphate Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 238000001782 photodegradation Methods 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/26—Phosphates
- C01B25/37—Phosphates of heavy metals
- C01B25/375—Phosphates of heavy metals of iron
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/14—Phosphorus; Compounds thereof
- B01J27/185—Phosphorus; Compounds thereof with iron group metals or platinum group metals
- B01J27/1853—Phosphorus; Compounds thereof with iron group metals or platinum group metals with iron, cobalt or nickel
-
- B01J35/39—
-
- B01J35/40—
-
- 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
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/84—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by UV- or VIS- data
-
- 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
- C01P2004/30—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
- C01P2004/51—Particles with a specific particle size distribution
- C01P2004/52—Particles with a specific particle size distribution highly monodisperse size distribution
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
Abstract
A method of di iron micro-nano powder material is prepared with rich phosphorus biomass, is related to micro Nano material and biological material applied technical field.Di iron micro-nano powder material is mainly prepared through hydrothermal synthesis reaction using ferric chloride in aqueous solution and rich phosphorus biomass.When selecting fish scale, animal bone as reaction raw materials respectively, the micromorphology of micro-nano powder material obtained is respectively micro-nano ball, polyhedron.The present invention uses conventional soluble molysite and discarded rich phosphorus biomass as reaction raw materials, successfully obtains di iron micro-nano powder material by one step of hydrothermal synthesis reaction.Pass through the characterization of series, it was demonstrated that the di iron micro-nano powder material of acquisition have narrower particle size distribution, performance it is stable etc. characteristics.The Fe of acquisition5(PO4)4(OH)3·2H2O micro-nano-scale powder morphology is controllable, it is seen that optical property is excellent, can be used as the electrode material and photochemical catalyst of lithium battery.
Description
Technical field
The present invention relates to micro Nano material and biological material applied technical fields, are specifically related to a kind of with rich phosphorus biology
The method that matter prepares di iron micro-nano powder material.
Background technique
Fe5(PO4)4(OH)3·2H2O is widely present in mineral in nature, and color is olive green, and crystal shape is logical
Often there are needle-shaped, sheet and raft shape, in electrode material LiFePO4The photodegradation of organic pollutant in preparation and nature rises important
Effect.Fe5(PO4)4(OH)3·2H2O, usually Fe2+Product made from some additives is prepared or is added with phosphate oxidation,
Its structure and property and FePO4It is different.Industrial production Fe5(PO4)4(OH)3·2H2The technique of O is mainly in partial reduction condition
Lower preparation, easy to oxidize, energy consumption is high for preparation.
The present invention is matched appropriate amount richness phosphorus biomass, Fe is made through hydrothermal synthesis reaction using soluble ferric iron salt as reactant5
(PO4)4(OH)3·2H2O, i.e. di iron micro-nano powder material.
Summary of the invention
In order to overcome drawbacks described above existing in the prior art, the purpose of the present invention is to provide a kind of simple process, at
This method that is low, being suitble to industrialization quantity-produced to prepare di iron micro-nano powder material with rich phosphorus biomass.
To realize the purpose, the invention adopts the following technical scheme:
A method of di iron micro-nano powder material, including hydrothermal synthesis method are prepared with rich phosphorus biomass, it is main
If preparing Fe through hydrothermal synthesis reaction using ferric chloride in aqueous solution and rich phosphorus biomass5(PO4)4(OH)3·2H2O, i.e. hydroxyl phosphorus
Sour iron micro-nano powder material.Specifically comprise the following steps:
1) suitable FeCl, is weighed3·6H2O solid is added in the beaker for filling a certain amount of deionized water, and puts it to
It is stirred on magnetic stirring apparatus；
2), suitable rich phosphorus biomass is added into above-mentioned solution, reaction system is then transferred to stainless steel cauldron
Middle carry out hydrothermal synthesis reaction；
3) it, after reaction, is cooled to room temperature, will generate after product is collected by centrifugation successively with deionized water and dehydrated alcohol
Supersound washing is several times；
4), carrying out drying and processing in an oven can be prepared by blackish green di iron micro-nano powder material.
As the optimal technical scheme of preparation method of the invention, the richness phosphorus biomass is fish scale or Animal Bone
Head, when selecting fish scale as reaction raw materials, the micromorphology of micro-nano powder material obtained is micro-nano ball.It is elected
When selecting animal bone as reaction raw materials, the micromorphology of micro-nano powder material obtained is polyhedron.
As the optimal technical scheme of preparation method of the invention, the rich phosphorus biomass in step 2) is according to FeCl3·
6H2O: rich phosphorus biomass=0.075~0.3:1~1.5 (mmol:g) addition.The reaction temperature of hydrothermal synthesis is in step 2)
160~200 DEG C, the reaction time is 5~15h.
The present invention uses conventional soluble molysite and discarded rich phosphorus biomass as reaction raw materials, anti-by hydrothermal synthesis
A step is answered to successfully obtain di iron micro-nano powder material.Pass through the characterization of series, it was demonstrated that the di iron of acquisition is micro-
Nano-powder material have narrower particle size distribution, performance it is stable etc. characteristics.It is of the invention compared with reported preparation method
Preparation method has easy to operate, required the advantages that raw material cost is low, and yield is big.Meanwhile the Fe of acquisition5(PO4)4(OH)3·
2H2O micro-nano-scale powder morphology is controllable, it is seen that optical property is excellent, can be used as the electrode material and photochemical catalyst of lithium battery.
Compared with prior art, the invention has the following advantages that
1. the present invention is realized using discarded rich phosphorus biomass (including but not limited to fish scale, bone etc.) as raw material,
Fe can be quickly obtained under hydrothermal condition5(PO4)4(OH)3·2H2O micro-nano powder material is Fe5(PO4)4(OH)3·2H2O
Synthesis provide a kind of new approach.
2. present invention process is simple, the easy building of entire preparation system, easy to operate, condition is easily-controllable, low in cost, product
Easily-controllable, product is formed to be evenly distributed, is not easy to reunite, being suitable for large-scale industrial production.
3. the present invention is using conventional soluble molysite as reactant, the by-product generated during the preparation process is few, right
Environmental pollution is smaller, is a kind of environment-friendly type synthesis technology.
It, can be with 4. product prepared by the present invention has preferable water-soluble, environmental-friendly, high-specific surface area and high adsorption
Apply electrode material, organic pollutant in terms of, have more wide application prospect.
Detailed description of the invention
Fig. 1 is the size distribution plot of target product prepared by embodiment 1, and illustration is low range SEM photograph.
Fig. 2 a is the high magnification SEM photograph of target product prepared by embodiment 1, and Fig. 2 b is that target prepared by embodiment 1 produces
The elemental analysis figure of object.
Fig. 3 is the SEM photograph of target product prepared by embodiment 2, and illustration is high magnification photo.
Fig. 4 is the XRD spectra of the target product of embodiment 1 (a) and embodiment 2 (b) preparation.
Fig. 5 is the visible absorption spectrogram of the target product of embodiment 1 (a) and embodiment 2 (b) preparation, and illustration is two kinds
The appearance photo of target product.
Fig. 6 is that the dynamics of the photocatalysis methylene blue of the target product of embodiment 1 (a) and embodiment 2 (b) preparation is bent
Line.
Specific embodiment
With reference to embodiments and attached drawing present invention is further described in detail.
The method of the present invention using X-ray powder diffraction (XRD), field emission scanning electron microscope (FE-SEM), it is ultraviolet can
See that the equipment such as spectral investigator (UV-vis) characterize structure, the form etc. of products therefrom.
Embodiment 1
Di iron micro-nano powder material is prepared with fish scale, the method is as follows:
1) FeCl of 0.2mmol, is weighed3·6H2O solid is added in the beaker for the deionized water for filling 20mL, and is put
It is stirred on to magnetic stirring apparatus.
2), the fish scale of 1g is added into above-mentioned solution, then reaction system is transferred in stainless steel cauldron, carries out water
Thermal synthesis reaction, reaction temperature are 180 DEG C, reaction time 10h.
3) it, after reaction, is cooled to room temperature, will generate after product is collected by centrifugation successively with deionized water and dehydrated alcohol
Supersound washing is several times.
4), carrying out drying and processing in an oven can be prepared by blackish green di iron micro-nano powder material.
Fig. 1 is the size distribution plot of target product prepared by embodiment 1, and illustration is low range SEM photograph.Fig. 2 a is to implement
The high magnification SEM photograph of target product prepared by example 1, Fig. 2 b are the elemental analysis figure of target product prepared by embodiment 1.
In conjunction with Fig. 1 and 2 as can be seen that being in micro-nano ball with the di iron micro-nano powder material of fish scale preparation
Form, narrower particle size distribution, average grain diameter are 1.6 ± 0.05 μm, while can also be seen that the di iron of acquisition by Fig. 1
In Gauss normal distribution rule, the di iron micro-nano ball that can also be seen that acquisition by Fig. 2 a is the partial size of micro-nano ball
It is made of countless nanometer little particles, the chemical composition that can be seen that single di iron micro-nano ball by Fig. 2 b is mainly
Tri- kinds of elements of O, Fe and P, and C and Ca constituent content is seldom, what can be further confirmed that is di iron micro-nano ball.
Embodiment 2
Di iron micro-nano powder material is prepared with bone, the method is as follows:
1) FeCl of 0.15mmol, is weighed3·6H2O solid be added fill 15mL deionized water beaker in, and by its
It is put on magnetic stirring apparatus and is stirred.
2), the bone of 1g is added into above-mentioned solution, then reaction system is transferred in stainless steel cauldron, carries out water
Thermal synthesis reaction, reaction temperature are 180 DEG C, reaction time 10h.
3) it, after reaction, is cooled to room temperature, will generate after product is collected by centrifugation successively with deionized water and dehydrated alcohol
Supersound washing is several times.
4), carrying out drying and processing in an oven can be prepared by blackish green di iron micro-nano powder material.
Fig. 3 is the SEM photograph of target product prepared by embodiment 2, and illustration is high magnification photo.As seen in Figure 3,
Di iron micro-nano powder material with animal bone preparation is in polyhedron morphology, and average-size is about 5~15 μm.
Fig. 4 is the XRD spectra of the target product of embodiment 1 (a) and embodiment 2 (b) preparation.As seen in Figure 4, it adopts
With both fish scale and animal bone phosphorus source, the target product obtained under the same conditions is Fe5(PO4)4(OH)3·2H2O powder
Material (after standard card comparative analysis).
Fig. 5 is the visible absorption spectrogram of the target product of embodiment 1 (a) and embodiment 2 (b) preparation, and illustration is two kinds
The appearance photo of target product.As seen in Figure 5, the Fe of two kinds of forms5(PO4)4(OH)3·2H2O powder presents blackish green
Color.Meanwhile the ball that the case where the two is to visible absorption is different, prepared by embodiment 1 can be seen that by visible absorption spectrogram
Shape Fe5(PO4)4(OH)3·2H2The absorption maximum band edge (~430nm) of O absorption visible light is than polyhedron prepared by embodiment 2
Fe5(PO4)4(OH)3·2H2The absorption band edge (~460nm) of O is small.
Embodiment 3
The Visible Light Induced Photocatalytic dyestuff performance of di iron micro-nano powder material, experimental procedure are as follows:
(1), using methylenum careuleum as target contaminant, add in the solution that 100mL methylenum careuleum initial concentration is 20mg/L respectively
Enter the Fe of the preparation of 0.1g embodiment 1,25(PO4)4(OH)3·2H2O powder obtains mixed liquor a after Quick uniform dispersion, then puts
Enter progress photocatalysis experiment in photocatalysis apparatus.
(2), illumination t1After minute, 10mL is taken out from mixed liquor a and is centrifuged, supernatant b is obtained.
(3), with the absorbance A of ultraviolet-visible spectrometer test supernatant b1, after being completed, refund test tube and together with
Remaining solution and catalyst are backed after shaking up in mixed liquor a, and photocatalysis experiment is continued.
(4), illumination t2Minute, t3Minute and t4Minute, t5Minute and t6Sampling and test process and (2) after minute and
(3) two steps are identical, and the serial absorbance measured is respectively labeled as A2、A3、A4、A5And A6。
(5), make time tiAnd absorbance Ai(i=0,1,2,3,4,5,6) curve.Again according to absorbance A and concentration C relationship
Adsorption time t and concentration C is calculated in (langbobier law)tRelation curve.
Fig. 6 is that the dynamics of the photocatalysis methylene blue of the target product of embodiment 1 (a) and embodiment 2 (b) preparation is bent
Line.The Fe of two kinds of forms as seen in Figure 65(PO4)4(OH)3·2H2O powder all has excellent photocatalysis performance, compares
Under, the Fe of the preparation of embodiment 25(PO4)4(OH)3·2H2The polyhedral visible light catalytic performance of O wants higher.
Claims (1)
1. a kind of method for preparing di iron micro-nano powder material with rich phosphorus biomass, including hydrothermal synthesis method, special
Sign is: mainly preparing Fe through hydrothermal synthesis reaction using ferric chloride in aqueous solution and rich phosphorus biomass5(PO4)4(OH)3·
2H2O, i.e. di iron micro-nano powder material；Specifically comprise the following steps:
1) FeCl of 0.15mmol, is weighed3·6H2O solid is added in the beaker for the deionized water for filling 15mL, and puts it to
It is stirred on magnetic stirring apparatus；
2), the bone of 1g is added into above-mentioned solution, then reaction system is transferred in stainless steel cauldron, carries out hydro-thermal conjunction
At reaction, reaction temperature is 180 DEG C, reaction time 10h；
3) it, after reaction, is cooled to room temperature, will generate after product is collected by centrifugation successively with deionized water and dehydrated alcohol ultrasound
Washing is several times；
4), drying and processing can be prepared by blackish green di iron micro-nano powder material, and material is in blackish green, structure
Formula is Fe5(PO4)4(OH)3·2H2O, micromorphology are polyhedron, and average-size is 5~15 μm.
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| CN108452817B (en) * | 2017-02-17 | 2020-04-07 | 中国科学院化学研究所 | Supported transition metal phosphide, preparation method thereof and application thereof in catalytic hydrogen production |
| CN109759101A (en) * | 2019-03-27 | 2019-05-17 | 合肥学院 | A kind of method that wood fiber biomass prepares carbon carried heteropoly acid material |
| CN110586027A (en) * | 2019-09-10 | 2019-12-20 | 济南大学 | Preparation method of porous microcrystalline glass containing photocatalytic functional crystalline phase and obtained product |
| CN113078328B (en) * | 2021-03-17 | 2023-01-31 | 浙江大学 | Co-FPOH microsphere material for water system zinc-air battery and preparation method thereof |
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| CN103311543A (en) * | 2012-12-10 | 2013-09-18 | 上海电力学院 | Anode material hydroxyl iron phosphate for lithium ion batteries and preparation method thereof |
| CN103569983A (en) * | 2013-10-29 | 2014-02-12 | 张苗 | Method for preparing calcium hydrogen phosphate by using animal bones |
| CN105236375A (en) * | 2015-09-17 | 2016-01-13 | 上海第二工业大学 | Method for preparing hydrated hydroxyl ferric phosphates by utilizing waste phosphatization slag for extraction |
| CN106082155B (en) * | 2016-06-07 | 2018-04-06 | 广西壮族自治区药用植物园 | The method that hydroxyapatite is prepared using fish-bone |
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