CN104941672A - Preparation method of single-layer hexagonal Ag3PO4/Fe3O4/Co-Ni LDH (layered double hydroxide) composite material - Google Patents
Preparation method of single-layer hexagonal Ag3PO4/Fe3O4/Co-Ni LDH (layered double hydroxide) composite material Download PDFInfo
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- CN104941672A CN104941672A CN201510205780.8A CN201510205780A CN104941672A CN 104941672 A CN104941672 A CN 104941672A CN 201510205780 A CN201510205780 A CN 201510205780A CN 104941672 A CN104941672 A CN 104941672A
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Abstract
The invention provides a preparation method of a single-layer hexagonal Ag3PO4/Fe3O4/Co-Ni LDH (layered double hydroxide) composite material. The preparation method comprises the following steps: dissolving Co-Ni LDH, Fe3O4 nano particles and Na2HPO4 into water, stirring, performing suction filtration to acquire black precipitates, and dissolving the black precipitates into CH3COOAg and stirring to obtain the black single-layer hexagonal Ag3PO4/Fe3O4/Co-Ni LDH composite material. The composite material prepared by the method can degrade methyl orange of azo dyes under a condition of visible light.
Description
Technical field
The invention belongs to photocatalyst technology field, be specifically related to a kind of individual layer hexagon Ag
3pO
4/ Fe
3o
4the preparation method of/Co-Ni LDH composite.
Background technology
2010, magazine " nature " reported a kind of visible-light photocatalyst silver orthophosphate (Ag with strong oxidizing property
3pO
4), this Novel silver phosphate photocatalyst absorbing wavelength can be less than the sunshine of 520nm, quantum yield under visible light up to 90%, and creates strong oxidability under visible light, in the degradation experiment of many organic dyestuff, all show extremely superior photocatalysis performance.As a kind of emerging material, photochemical catalyst can utilize sunshine processing environment pollutant, for mankind's Environment control opens an effective new way.Titanium dioxide (TiO
2) there is high catalytic activity, good chemical stability, with low cost, the characteristics such as safety non-toxic are one of green catalysts studying hottest point at present.But most of catalyst such as titanium dioxide can only produce catalytic activity under ultraviolet light (accounting for 5% of solar radiation), and low sunshine utilization rate makes photocatalytic activity restricted greatly.As a kind of functional material, photochemical catalyst should possess following characteristics: high activity and high efficiency; Stability and anti-poisoning capability is kept under high temperature, long-time reaction; Mechanical stability and wear resistance; Keep physical stability and chemical property under various conditions; Raw material prepared by photochemical catalyst are cheap.
Azo dyes refers to the dyestuff of the azo structure containing connection two aromatic radicals (singly do not refer to aryl radical, also refer to the hydridization alkyl containing armaticity) in dye molecule, and general formula is Ar-N=N-Ar '.Azo dyes is connected with aromatic ring system the chromogen of formation conjugated system as dyestuff.This kind of dyestuff is with a long history, and synthesis is convenient, and stable in properties is cheap, is extensively liked.If textile garment uses the azo dyes containing forbidding, with the Long Term Contact of human body in may to produce absorb by the skin of human body, spread in human body, if can not discharge via metabolism in time, under the condition that these dyestuffs react in the metabolism of human normal, may reduction reaction be there is, and then decomposite carcinogenic aromatic amine.Carcinogenic aromatic amine, via activation, changes the DNA structure of human body, finally causes human body mutagenesis and cause cancer.
Methyl orange is a kind of typical azo dyes, and micro-poison, is difficult to biodegradation.Printing dye discharge capacity containing methyl orange is large, and organic concentration is high, is difficult to biodegradation, is the industrial wastewater received much concern.Therefore, a kind of material of methyl orange of can degrading need be found.
Summary of the invention
The invention provides a kind of individual layer hexagon Ag
3pO
4/ Fe
3o
4the preparation method of/Co-Ni LDH composite, the composite adopting method of the present invention to obtain can degrade azo dyestuff methyl orange under visible light.
The invention provides a kind of individual layer hexagon Ag
3pO
4/ Fe
3o
4the preparation method of/Co-Ni LDH composite, by Co-Ni LDH, Fe
3o
4nano particle and Na
2hPO
4stirring soluble in water, suction filtration obtains black precipitate, and black precipitate is dissolved in CH
3stir in COOAg, obtain the individual layer hexagon Ag of black
3pO
4/ Fe
3o
4/ Co-Ni LDH composite.
Preferably, described CH
3cOOAg and Na
2hPO
4mol ratio be (1-3): (0.5-1.5).Wherein, it is best when both ratios are 3:1.
The mol ratio that silver acetate and sodium hydrogen phosphate generate silver orthophosphate reaction is exactly 3:1, can make both complete reactions just.
Preferably, described Co-Ni LDH and Fe
3o
4the mol ratio of raw material is (1.5-3): (0.5-1.2); Most preferably be 2.5:1.When selecting other ratios, what prepare is not complete hexagon, and hexagon can be broken into fractionlet.
Further, the preparation method of described Co-Ni LDH is: by CoCl
26H
2o, NiCl
26H
2o and urotropine join in distilled water and dissolve, and are reacted by mixed liquor at 120 DEG C, suction filtration after cooling, and washing is to neutral, dry, obtains Co-Ni LDH.
Further, described CH
3the preparation method of COOAg is: in SAS, dropwise add AgNO
3solution, CH
3cOONa and AgNO
3mol ratio be 1:1; Separating reaction liquid, the powder acetic acid obtained is washed, dry after removing acetic acid, obtains CH
3cOOAg; As preferably, the concentration of SAS is 0.05-0.15g/ml; As preferably, described pickling is washed with acetic acid.
When sodium acetate concentration is too little, the time needed when obtaining silver acetate precipitation is too of a specified duration, and deposit seed that is that formed is less because of too intensive for the precipitation generated when concentration is too large; The silver acetate jaundice prepared when not washing with acetic acid, when the silver acetate washing out with acetic acid is white flash shape material.
Further, the concentration of described AgNO3 is 0.5-2.5mol/L.Adopt this concentration can prepare 12 silver orthophosphates.
Second object of the present invention is to provide the individual layer hexagon Ag that application said method prepares
3pO
4/ Fe
3o
4/ Co-Ni LDH composite.
3rd object of the present invention is to provide above-mentioned individual layer hexagon Ag
3pO
4/ Fe
3o
4the application of/Co-Ni LDH composite in degraded methyl orange.
Preferably, described degraded is degraded under visible light.
Preferably, the pH of described methyl orange is 8.During pH=8, degradation effect is best.
The present invention utilizes Co-Ni LDH compound Ag
3pO
4and Fe
3o
4, greatly improve the ability of visible light photocatalytic degradation methyl orange.Due to exciting of visible ray, Ag
3pO
4electron transition in valence band is on conduction band, and the electron transmission on conduction band is to Fe
3o
4.And Ag is transferred in the hole in valence band
3pO
4surface, makes the hydroxyl in Co-Ni double-hydroxide become OH, and meanwhile, methyl orange also can be oxidized to CO by the hole on Ag
2and H
2o.And Fe
3o
4oxygen can be become ultra-oxygen anion free radical by the electronics on upper conduction band, and ultra-oxygen anion free radical has strong oxidability.
Accompanying drawing explanation
Accompanying drawing is used to provide a further understanding of the present invention, and forms a part for description, together with embodiments of the present invention for explaining the present invention, is not construed as limiting the invention.In the accompanying drawings:
In Fig. 1, A is Co-Ni nonwoven fabric from filaments of the present invention, and B is Ag prepared by the present invention
3pO
4nano particle, C, D are hexagon Ag prepared by the present invention
3pO
4/ Fe
3o
4the scanning electron microscope (SEM) photograph of/Co-Ni LDH composite;
Fig. 2 is hexagon Ag prepared by the present invention
3pO
4/ Fe
3o
4the X-ray powder diffraction spectrogram of/Co-Ni LDH composite;
Fig. 3 is the curve map of composite degradation methyl orange prepared by the present invention;
Fig. 4 is the principle schematic of methyl orange degradation.
Detailed description of the invention
Following embodiment is convenient to understand the present invention better, but does not limit the present invention.Experimental technique in following embodiment, if no special instructions, is conventional method.
The water used in experimentation is redistilled water (abbreviation intermediate water), test reagent used be analyze pure.
The instrument that this experiment uses and reagent:
The automatic dual pure water distiller (1810B, Asian-Pacific Glass-Tech. Co., Shanghai City) of quartz ampoule heated type is for the preparation of redistilled water; Electronic balance (Beijing Sai Duolisi Instrument Ltd.) is for weighing medicine; JSM-6701F cold field emission type ESEM (Jeol Ltd.) is for morphology characterization; UV1102 (Shanghai Techcomp Instrument Ltd.); Ultrasonic cleaner (Kunshan Ultrasonic Instruments Co., Ltd.); CoCl
26H
2o, NiCl
26H
2o, Na
2hPO
4(Tianjin Kai Xin chemical industry Co., Ltd), urotropine, oleic acid (Aladdin), AgNO
3(Tianjin Chemical Co., Ltd.'s all generations).
Embodiment 1
Individual layer hexagon Ag of the present invention
3pO
4/ Fe
3o
4the preparation method of/Co-Ni LDH composite is as follows:
1, the preparation of Co-Ni LDH
(1) by 0.1189g CoCl
26H
2o, 0.059gNiCl
26H
2o and 0.6308g urotropine joins in the distilled water of 100ml;
(2) it is made fully to dissolve mixed liquor ultrasonic disperse 10min; The not requirement of frequency size, as long as disperseed.
(3) mixed liquor is transferred to 120 DEG C of reaction 5h in the reactor of 100ml; At the OH that 120 DEG C of reactions contain compared with the Co-Ni LDH 95 DEG C of reaction preparations
-more, be conducive to generating OH;
(4) after cooling by mixed liquor suction filtration, with intermediate water washing to neutral, pale yellow precipitate is obtained, at room temperature dry, prepare Co-Ni LDH.Figure 1A is the scanning electron microscope (SEM) photograph of the Co-Ni LDH prepared, and has as can be seen from the figure prepared the Co-Ni LDH of individual layer.
2, Fe
3o
4preparation
By 4.31gFeSO
47H
2o and 9.5gFeCl
36H
2o is dissolved in the deionized water of 50ml, and with nitrogen protection, then solution is heated to 353K and stirs 30min, adds 40mlNH fast subsequently
4oH (28wt%), stirs 15min, adds 1g oleic acid.Dispersion liquid is heated to 353K and Keep agitation 3h.Subsequently solution is cooled to room temperature.Collect with external magnetic field and be washed till neutrality by deionized water, then ethanolic solution washes three times.
3, CH
3the preparation of COOAg
(1) get 0.5-1.5g sodium acetate solid and be dissolved in 10ml water;
(2), under stirring, in the mixed liquor of step (1), the AgNO of the 1.5mol/L configured in advance is dropwise added
3solution; CH
3cOONa and AgNO
3mol ratio be 1:1;
(3) by the reactant liquor centrifugation of step (2), be separated the powder acetic acid obtained and wash;
(4) powder that obtains of step (3) is at room temperature dry.
4, hexagon Ag
3pO
4/ Fe
3o
4the preparation of/Co-Ni LDH composite
Get the 0.058g Fe prepared in above-mentioned steps
3o
4nano particle, 0.059gCo-Ni LDH and Na
2hPO
40.947g is dissolved in the deionized water of 100ml, stirs 24h, rinses out unnecessary Na
2hPO
4, suction filtration obtains black precipitate, is dissolved in black precipitate containing 3.36g CH
3in the 50ml deionized water of COOAg, stir 24h, suction filtration obtains black powder at room temperature drying and obtains Co-Ni loaded Ag
3pO
4and Fe
3o
4the hexagon nonwoven fabric from filaments of nano particle, i.e. hexagon Ag
3pO
4/ Fe
3o
4/ Co-Ni LDH composite.If added CH before suction filtration
3cOOAg, CH
3cOOAg can and solution in a large amount of sodium hydrogen phosphate reaction existed, generate a large amount of silver orthophosphates, so filter the rear compound that just can not separate silver orthophosphate and preparation, more can not compare both degradation effects.
Fig. 1 C and D is the hexagon Ag prepared
3pO
4/ Fe
3o
4the scanning electron microscope (SEM) photograph of/Co-Ni LDH composite, the material prepared as can be seen from Figure is the regular hexagon laminated structure of individual layer, is deposited in together.The pattern of the Co-Ni LDH of individual layer changes, and may be to there is CH3COO in the process owing to preparing composite
-.Co-Ni LDH has large specific area, can as good base, and containing hydroxyl, be easy to generate hydroxyl radical free radical, methyl orange is conducive to be converted into carbon dioxide, tri-iron tetroxide can by reduction silver orthophosphate energy gap, and silver orthophosphate the experiment proved that good catalytic performance under visible light.
Individual layer hexagon Ag of the present invention
3pO
4/ Fe
3o
4the degradation experiment of/Co-Ni LDH composite azo dyes methyl orange:
The composite of the present invention of 0.2g/l is joined 25mg/l, and pH is in the methyl orange solution of 8, places 30min, make material surface and methyl orange dye reach adsorption equilibrium at dark place.Mixed liquor is placed in white light under the Xe lamp of 150W, gets once every 5min, measure the ultraviolet curve of different time solution.Result is see Fig. 3, and its degradation principles is see Fig. 4.Can find out that composite of the present invention has obvious degradation effect to methyl orange by the degradation curve of Fig. 3.But having occurred obvious blue shift during 15min, may be because methyl orange generates new product in the process of degraded.The XRD diffraction maximum of composite and the carrying out of standard card are contrasted, determines the silver orthophosphate defining 12.
Embodiment 2
The difference of the present embodiment and embodiment 1 is:
Step 3CH
3in the preparation of COOAg, AgNO
3the concentration of solution is 1.0mol/L.
In step 4, hexagon Ag
3pO
4/ Fe
3o
4the preparation method of/Co-Ni LDH composite is: get the 0.089g Fe prepared in above-mentioned steps
3o
4nano particle (0.387mmol), 0.065g Co-Ni LDH (0.698mmol) and Na
2hPO
40.80g (0.0056mol) is dissolved in the deionized water of 100ml, stirs 24h, rinses out unnecessary Na
2hPO
4, suction filtration obtains black precipitate, is dissolved in black precipitate containing 2.804g CH
3in the 50ml deionized water of COOAg (0.0168mol), stir 24h, suction filtration obtains black powder at room temperature drying and obtains Co-Ni loaded Ag
3pO
4and Fe
3o
4the hexagon nonwoven fabric from filaments of nano particle, i.e. hexagon Ag
3pO
4/ Fe
3o
4/ Co-Ni LDH composite.
Embodiment 3
The difference of the present embodiment and embodiment 1 is:
Step 3CH
3in the preparation of COOAg, AgNO
3the concentration of solution is 2.5mol/L.
In step 4, hexagon Ag
3pO
4/ Fe
3o
4the preparation method of/Co-Ni LDH composite is: get the 0.0479g Fe prepared in above-mentioned steps
3o
4nano particle (0.2067mmol), 0.050gCo-Ni LDH (0.5376mmol) and Na
2hPO
41.130g (0.0079mol) is dissolved in the deionized water of 100ml, stirs 24h, rinses out unnecessary Na
2hPO
4, suction filtration obtains black precipitate, is dissolved in black precipitate containing 3.985g CH
3in the 50ml deionized water of COOAg (0.0237mol), stir 24h, suction filtration obtains black powder at room temperature drying and obtains Co-Ni loaded Ag
3pO
4and Fe
3o
4the hexagon nonwoven fabric from filaments of nano particle, i.e. hexagon Ag
3pO
4/ Fe
3o
4/ Co-Ni LDH composite.
Embodiment 4
The difference of the present embodiment and embodiment 1 is:
Step 3CH
3in the preparation of COOAg, AgNO
3the concentration of solution is 2.5mol/L.
In step 4, hexagon Ag
3pO
4/ Fe
3o
4the preparation method of/Co-Ni LDH composite is: get the 0.05g Fe prepared in above-mentioned steps
3o
4nano particle (0.2155mmol), 0.0417g Co-Ni LDH (0.4489mmol) and 1.130g Na
2hPO
4(0.0079mol) be dissolved in the deionized water of 100ml, stir 24h, rinse out unnecessary Na
2hPO
4, suction filtration obtains black precipitate, is dissolved in black precipitate containing 3.985g CH
3in the 50ml deionized water of COOAg (0.0237mol), stir 24h, suction filtration obtains black powder at room temperature drying and obtains Co-Ni loaded Ag
3pO
4and Fe
3o
4the hexagon nonwoven fabric from filaments of nano particle, i.e. hexagon Ag
3pO
4/ Fe
3o
4/ Co-Ni LDH composite.
Embodiment 5
The difference of the present embodiment and embodiment 1 is:
Step 3CH
3in the preparation of COOAg, AgNO
3the concentration of solution is 2.5mol/L.
In step 4, hexagon Ag
3pO
4/ Fe
3o
4the preparation method of/Co-Ni LDH composite is: get the 0.0398g Fe prepared in above-mentioned steps
3o
4nano particle (0.172mmol), 0.05g Co-Ni LDH (0.537mmol) and 1.130g Na
2hPO
4(0.0079mol) be dissolved in the deionized water of 100ml, stir 24h, rinse out unnecessary Na
2hPO
4, suction filtration obtains black precipitate, is dissolved in black precipitate containing 3.985g CH
3in the 50ml deionized water of COOAg (0.0237mol), stir 24h, suction filtration obtains black powder at room temperature drying and obtains Co-Ni loaded Ag
3pO
4and Fe
3o
4the hexagon nonwoven fabric from filaments of nano particle, i.e. hexagon Ag
3pO
4/ Fe
3o
4/ Co-Ni LDH composite.
Last it is noted that the foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, although with reference to previous embodiment to invention has been detailed description, for a person skilled in the art, it still can be modified to the technical scheme described in foregoing embodiments, or carries out equivalent replacement to wherein portion of techniques feature.Within the spirit and principles in the present invention all, any amendment done, equivalent replacement, improvement etc., all should be included within protection scope of the present invention.
Claims (10)
1. an individual layer hexagon Ag
3pO
4/ Fe
3o
4the preparation method of/Co-Ni LDH composite, is characterized in that: by Co-Ni LDH, Fe
3o
4nano particle and Na
2hPO
4stirring soluble in water, suction filtration obtains black precipitate, and black precipitate is dissolved in CH
3stir in COOAg, obtain the individual layer hexagon Ag of black
3pO
4/ Fe
3o
4/ Co-Ni LDH composite.
2. preparation method according to claim 1, is characterized in that: described CH
3cOOAg and Na
2hPO
4mol ratio be (1-3): (0.5-1.5).
3. preparation method according to claim 1, is characterized in that: described Co-Ni LDH and Fe
3o
4the mol ratio of raw material is (1.5-3): (0.5-1.2); Most preferably be 2.5:1.
4., according to the arbitrary described preparation method of claim 1-3, it is characterized in that: the preparation method of described Co-Ni LDH is: by CoCl
26H
2o, NiCl
26H
2o and urotropine join in distilled water and dissolve, and are reacted by mixed liquor at 120 DEG C, suction filtration after cooling, and washing is to neutral, dry, obtains Co-Ni LDH.
5., according to the arbitrary described preparation method of claim 1-3, it is characterized in that: described CH
3the preparation method of COOAg is: in SAS, dropwise add AgNO
3solution, CH
3cOONa and AgNO
3mol ratio be 1:1; Separating reaction liquid, the powder pickling obtained, except dry after disacidify, obtains CH
3cOOAg; As preferably, the concentration of SAS is 0.05-0.15g/ml; As preferably, described pickling is washed with acetic acid.
6. method according to claim 5, is characterized in that: the concentration of described AgNO3 is 0.5-2.5mol/L.
7. application rights requires the individual layer hexagon Ag that the arbitrary described method of 1-6 prepares
3pO
4/ Fe
3o
4/ Co-Ni LDH composite.
8. individual layer hexagon Ag according to claim 7
3pO
4/ Fe
3o
4the application of/Co-Ni LDH composite in degraded methyl orange.
9. application according to claim 8, is characterized in that: described degraded is degraded under visible light.
10. application according to claim 8 or claim 9, is characterized in that: the pH of described methyl orange is 8.
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CN105428246A (en) * | 2015-10-09 | 2016-03-23 | 北京师范大学 | Two-dimensional composite hydroxide micron crystal applied to field effect transistor semiconductor material and preparation process thereof |
CN106513021A (en) * | 2016-11-05 | 2017-03-22 | 上海大学 | Layered hydroxide/BiOCl photocatalytic material and preparation method thereof |
CN107899590A (en) * | 2017-10-27 | 2018-04-13 | 江苏大学 | The preparation and its application of metal Ag nanoparticle deposition NiCo LDH composite photo-catalysts |
CN108579776A (en) * | 2017-12-29 | 2018-09-28 | 南京农业大学 | Multi-lager semiconductor visible light catalyst and the preparation method and application thereof |
CN108704653A (en) * | 2018-06-14 | 2018-10-26 | 浙江理工大学 | It is a kind of to have magnetic silver phosphate composite photocatalyst and its preparation method and application |
CN111471997A (en) * | 2020-04-09 | 2020-07-31 | 西华师范大学 | Metal material containing layered double hydroxide composite coating and plating layer and preparation method thereof |
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CN105428246A (en) * | 2015-10-09 | 2016-03-23 | 北京师范大学 | Two-dimensional composite hydroxide micron crystal applied to field effect transistor semiconductor material and preparation process thereof |
CN105428246B (en) * | 2015-10-09 | 2018-05-29 | 北京师范大学 | A kind of two-dimentional complex hydroxide micro-crystal and its preparation process applied to field effect transistor semiconductor material |
CN106513021A (en) * | 2016-11-05 | 2017-03-22 | 上海大学 | Layered hydroxide/BiOCl photocatalytic material and preparation method thereof |
CN106513021B (en) * | 2016-11-05 | 2019-06-04 | 上海大学 | Layered hydroxide/BiOCl photocatalytic material and preparation method thereof |
CN107899590A (en) * | 2017-10-27 | 2018-04-13 | 江苏大学 | The preparation and its application of metal Ag nanoparticle deposition NiCo LDH composite photo-catalysts |
CN107899590B (en) * | 2017-10-27 | 2020-01-24 | 江苏大学 | Preparation and application of metal Ag nano-particle deposited NiCo-LDH composite photocatalyst |
CN108579776A (en) * | 2017-12-29 | 2018-09-28 | 南京农业大学 | Multi-lager semiconductor visible light catalyst and the preparation method and application thereof |
CN108579776B (en) * | 2017-12-29 | 2021-03-23 | 南京农业大学 | Multilayer semiconductor visible-light-driven photocatalyst and preparation method and application thereof |
CN108704653A (en) * | 2018-06-14 | 2018-10-26 | 浙江理工大学 | It is a kind of to have magnetic silver phosphate composite photocatalyst and its preparation method and application |
CN111471997A (en) * | 2020-04-09 | 2020-07-31 | 西华师范大学 | Metal material containing layered double hydroxide composite coating and plating layer and preparation method thereof |
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