CN104941672B - A kind of side Ag of individual layer six3PO4/Fe3O4The preparation method of/Co Ni LDH composites - Google Patents
A kind of side Ag of individual layer six3PO4/Fe3O4The preparation method of/Co Ni LDH composites Download PDFInfo
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Abstract
The present invention provides a kind of side Ag of individual layer six3PO4/Fe3O4The preparation method of/Co Ni LDH composites, by Co Ni LDH, Fe3O4Nano-particle and Na2HPO4Stirring soluble in water, suction filtration obtains black precipitate, and black precipitate is dissolved in into CH3Stirred in COOAg, obtain the side Ag of individual layer six of black3PO4/Fe3O4/ Co Ni LDH composites.Adopting the composite being obtained by the present invention can degrade Azo Dye-Methyl Orange under visible light.
Description
Technical field
The invention belongs to photocatalyst technology field, and in particular to a kind of side Ag of individual layer six3PO4/Fe3O4/Co-Ni LDH
The preparation method of composite.
Background technology
, magazine in 2010《It is natural》Report a kind of visible-light photocatalyst silver orthophosphate (Ag with strong oxidizing property3PO4),
This Novel silver phosphate photocatalyst can be less than the sunshine of 520nm with absorbing wavelength, and quantum yield under visible light is up to
90%, and strong oxidability is generated under visible light, all shown extremely in the degradation experiment of many organic dyestuff
Superior photocatalysis performance.Used as a kind of emerging material, photochemical catalyst can utilize sunshine processing environment pollutant, be people
Class Environment control opens an effective new way.Titanium dioxide (TiO2) there is catalysis activity high, good change
Stability is learned, with low cost, the characteristic such as safety non-toxic is to study one of green catalyst of hottest point at present.But titanium dioxide
Catalysis activity, low sun light utilization efficiency can only be produced under ultraviolet light (accounting for the 5% of solar radiation) etc. most of catalyst
So that photocatalytic activity is greatly restricted.Used as a kind of functional material, photochemical catalyst should possess following characteristics：High activity and height
Efficiency；Stability and anti-poisoning capability are kept under high temperature, reaction for a long time；Mechanical stability and wear resistance；In various bars
Physical stability and chemical property are kept under part；Raw material prepared by photochemical catalyst are cheap.
Azo dyes refers to (not refer to aryl radical singly, also refer to containing fragrant containing two aromatic radicals of connection in dye molecule
Property hydridization alkyl) azo structure dyestuff, formula be Ar-N=N-Ar '.Azo dyes is connected with aromatic ring system and constitutes one
Individual conjugated system as dyestuff chromogen.This kind of dyestuff is with a long history, and synthesis is convenient, stable in properties, cheap, is extensively liked
Love.If textile garment may be produced by human body using the azo dyes containing disabling in the Long Term Contact with human body
Skin is absorbed, and is spread in human body, if can not be discharged via metabolism in time, these dyestuffs are in the new old of human normal
Under conditions of metabolic response, it may occur however that reduction reaction, and then decomposite carcinogenic aromatic amine.Carcinogenic aromatic amine is made via activation
With, change the DNA structure of human body, finally cause human body mutagenesis and trigger cancer.
Methyl orange is a kind of typical azo dyes, micro- poison, it is difficult to biodegradable.Printing dye discharge containing methyl orange
Amount is big, and organic concentration is high, it is difficult to biodegradable, is the industrial wastewater for receiving much concern.Therefore, need to find one kind can degrade first
The material of base orange.
The content of the invention
The invention provides a kind of side Ag of individual layer six3PO4/Fe3O4The preparation method of/Co-Ni LDH composites, uses
The composite that the method for the present invention is obtained can degrade Azo Dye-Methyl Orange under visible light.
The present invention provides a kind of side Ag of individual layer six3PO4/Fe3O4The preparation method of/Co-Ni LDH composites, by Co-Ni
LDH、Fe3O4Nano-particle and Na2HPO4Stirring soluble in water, suction filtration obtains black precipitate, and black precipitate is dissolved in into CH3In COOAg
Stirring, obtains the side Ag of individual layer six of black3PO4/Fe3O4/ Co-Ni LDH composites.
Preferably, the CH3COOAg and Na2HPO4Mol ratio be (1-3):(0.5-1.5).Wherein, both ratios are
3:It is optimal when 1.
Silver acetate and the mol ratio of disodium hydrogen phosphate generation silver orthophosphate reaction are exactly 3：1, both can be made just completely anti-
Should.
Preferably, the Co-Ni LDH and Fe3O4The mol ratio of raw material is (1.5-3)：(0.5-1.2)；Most preferably
2.5:1.When selecting other ratios, what is prepared is not complete hexagon, and hexagon can be broken into fractionlet.
Further, the preparation method of the Co-Ni LDH is：By CoCl2·6H2O, NiCl2·6H2O and the methylene of ring six
Urotropine is dissolved in being added to distilled water, mixed liquor is reacted at 120 DEG C, suction filtration after cooling, and washing to neutrality is dried, and is obtained
To Co-Ni LDH.
Further, the CH3The preparation method of COOAg is：AgNO is added dropwise in SAS3Solution,
CH3COONa and AgNO3Mol ratio be 1：1；Reaction solution is separated, the powder for obtaining is washed with acetic acid, dried after removing acetic acid, obtained final product
CH3COOAg；Preferably, the concentration of SAS is 0.05-0.15g/ml；Preferably, the pickling is to use acetic acid
Wash.
When sodium acetate concentration is too small, the time for obtaining being needed when silver acetate is precipitated is too long, the precipitation generated when concentration is too big
Because of too intensive, precipitation particle that is being formed is smaller；The silver acetate jaundice prepared when not washed with acetic acid, washes out when with acetic acid
The silver acetate for coming is white flash shape material.
Further, the concentration of the AgNO3 is 0.5-2.5mol/L.12 faces can be prepared using the concentration
Silver orthophosphate.
Second object of the present invention is to provide the side Ag of individual layer six prepared using the above method3PO4/Fe3O4/Co-
Ni LDH composites.
Third object of the present invention is to provide the side Ag of above-mentioned individual layer six3PO4/Fe3O4/ Co-Ni LDH composites are in drop
Application in solution methyl orange.
Preferably, the degraded is to degrade under visible light.
Preferably, the pH of the methyl orange is 8.Degradation effect is best during pH=8.
The present invention is using the compound Ag of Co-Ni LDH3PO4And Fe3O4, greatly improve visible light photocatalytic degradation methyl orange
Ability.Due to exciting for visible ray, Ag3PO4, on conduction band, the electron transmission on conduction band is given for electron transition in valence band
Fe3O4.And the hole in valence band is transferred to Ag3PO4Surface so that the hydroxyl in Co-Ni double-hydroxides becomes OH, together
When, methyl orange can also be oxidized to CO by the hole on Ag2And H2O.And Fe3O4Electronics on upper conduction band can become oxygen
Ultra-oxygen anion free radical, ultra-oxygen anion free radical has strong oxidability.
Brief description of the drawings
Accompanying drawing is used for providing a further understanding of the present invention, and constitutes a part for specification, with reality of the invention
Applying example is used to explain the present invention together, is not construed as limiting the invention.In the accompanying drawings：
A is Co-Ni nonwoven fabric from filaments of the invention in Fig. 1, and B is Ag prepared by the present invention3PO4Nano-particle, C, D are the present invention
The six side Ag for preparing3PO4/Fe3O4The scanning electron microscope (SEM) photograph of/Co-Ni LDH composites；
Fig. 2 is six side Ag prepared by the present invention3PO4/Fe3O4The X-ray powder diffraction spectrum of/Co-Ni LDH composites
Figure；
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.
Specific embodiment
Following embodiment facilitates a better understanding of the present invention, but does not limit the present invention.Experiment in following embodiments
Method, unless otherwise specified, is conventional method.
The water used in experimentation is redistilled water (abbreviation secondary water), and experiment reagent used is analysis
It is pure.
Instrument and reagent that this experiment is used：
The automatic dual pure water distiller (1810B, Asian-Pacific Glass-Tech. Co., Shanghai City) of quartz ampoule heated type is used to prepare two
Secondary distilled water；Electronic balance (Beijing Sai Duolisi Instrument Ltd.) is used to weigh medicine；JSM-6701F cold field emission types
ESEM (Jeol Ltd.) is used for morphology characterization；UV1102 (Shanghai Techcomp Instrument Ltd.)；Ultrasound
Ripple washer (Kunshan Ultrasonic Instruments Co., Ltd.)；CoCl2·6H2O、NiCl2·6H2O、Na2HPO4(the triumphant letter chemistry in Tianjin
Industrial Co., Ltd), urotropine, oleic acid (Aladdin), AgNO3(Tianjin all generations Chemical Co., Ltd.).
Embodiment 1
The side Ag of individual layer of the invention six3PO4/Fe3O4The preparation method of/Co-Ni LDH composites is as follows：
1st, the preparation of Co-Ni LDH
(1) by 0.1189g CoCl2·6H2O, 0.059gNiCl2·6H2O and 0.6308g urotropines are added
To in the distilled water of 100ml；
(2) it is made fully to dissolve mixed liquor ultrasonic disperse 10min；Frequency size is not required, as long as being disperseed i.e.
Can.
(3) mixed liquor is transferred to 120 DEG C of reaction 5h in the reactor of 100ml；In 120 DEG C of reactions compared with 95 DEG C of reaction systems
The OH that standby Co-Ni LDH contain-It is more, be conducive to generating OH；
(4) mixed liquor suction filtration, with secondary water washing to neutrality, is obtained into pale yellow precipitate after cooling, is dried at room temperature for,
Prepare Co-Ni LDH.Figure 1A is the scanning electron microscope (SEM) photograph of the Co-Ni LDH for preparing, and is as can be seen from the figure prepared
The Co-Ni LDH of individual layer.
2、Fe3O4Preparation
By 4.31gFeSO4·7H2O and 9.5gFeCl3·6H2O is dissolved in the deionized water of 50ml, is protected with nitrogen,
Then solution is heated to 353K stirring 30min, then rapidly joins 40mlNH4OH (28wt%), stirs 15min, adds 1g oil
Acid.Dispersion liquid is heated to 353K and continues to stir 3h.Solution is then cooled to room temperature.Deionization is collected and used with external magnetic field
Neutrality is washed to, then ethanol solution is washed three times.
3、CH3The preparation of COOAg
(1) 0.5-1.5g sodium acetate solids are taken and is dissolved in 10ml water；
(2) under stirring, the AgNO of 1.5mol/L for configuring in advance is added dropwise in the mixed liquor to step (1)3Solution；
CH3COONa and AgNO3Mol ratio be 1：1；
(3) by the reaction solution centrifugation of step (2), isolated powder is washed with acetic acid；
(4) powder that step (3) is obtained is dried at room temperature for.
4th, six side Ag3PO4/Fe3O4The preparation of/Co-Ni LDH composites
Take the 0.058g Fe prepared in above-mentioned steps3O4Nano-particle, 0.059gCo-Ni LDH and
Na2HPO40.947g is dissolved in the deionized water of 100ml, stirs 24h, rinses out unnecessary Na2HPO4, suction filtration obtains black precipitate,
Black precipitate is dissolved in CH containing 3.36g3In the 50ml deionized waters of COOAg, 24h is stirred, suction filtration obtains black powder at room temperature
It is dried to obtain Co-Ni loaded Ags3PO4And Fe3O4Six side nonwoven fabric from filaments of nano-particle, i.e. six side Ag3PO4/Fe3O4/Co-Ni LDH
Composite.If adding CH before suction filtration3COOAg, CH3COOAg can be anti-with a large amount of disodium hydrogen phosphates for existing in solution
Should, generate substantial amounts of silver orthophosphate, then silver orthophosphate and the compound for preparing cannot be separated after filtering, can not be to both drops
Solution effect is compared.
Fig. 1 C and Fig. 1 D are the six side Ag for preparing3PO4/Fe3O4The scanning electron microscope (SEM) photograph of/Co-Ni LDH composites,
The material for preparing as can be seen from Figure is packed together in the six regular side laminated structures of individual layer.The Co-Ni LDH of individual layer
Pattern change, it may be possible to there is CH3COO during due to preparing composite-.Co-Ni LDH possess big ratio
Surface area, as good base, and can contain hydroxyl, it is easy to generate hydroxyl radical free radical, be conducive to for methyl orange being converted into two
Carbonoxide, ferroso-ferric oxide can will reduce silver orthophosphate energy gap, and silver orthophosphate the experiment proved that under visible light good
Catalytic performance.
The side Ag of individual layer of the invention six3PO4/Fe3O4The degraded reality of/Co-Ni LDH composite azo dyes methyl oranges
Test：
The composite of the invention of 0.2g/l is added to 25mg/l, during pH is 8 methyl orange solution, is put at dark place
Put 30min so that material surface and methyl orange dye reach adsorption equilibrium.White light shines under mixed liquor to be placed in the Xe lamps of 150W
Penetrate, taken once every 5min, measure the ultraviolet curve of different time solution., referring to Fig. 3, its degradation principles is referring to Fig. 4 for result.By
The degradation curve of Fig. 3 can be seen that composite of the invention has obvious degradation effect to methyl orange.But occurred in that during 15min
Obvious blue shift, it may be possible to because methyl orange generates new product during degraded.By the XRD diffraction maximums of composite
Carrying out with standard card contrasts, it is determined that foring the silver orthophosphate in 12 faces.
Embodiment 2
The present embodiment is with the difference of embodiment 1：
Step 3CH3In the preparation of COOAg, AgNO3The concentration of solution is 1.0mol/L.
In step 4, six side Ag3PO4/Fe3O4The preparation method of/Co-Ni LDH composites is：Take system in above-mentioned steps
The standby 0.089g Fe for obtaining3O4Nano-particle (0.387mmol), 0.065g Co-Ni LDH (0.698mmol) and
Na2HPO40.80g (0.0056mol) is dissolved in the deionized water of 100ml, stirs 24h, rinses out unnecessary Na2HPO4, suction filtration
Black precipitate is obtained, black precipitate is dissolved in CH containing 2.804g3In the 50ml deionized waters of COOAg (0.0168mol), stirring
24h, suction filtration obtains black powder and is dried at room temperature for obtaining Co-Ni loaded Ags3PO4And Fe3O4Six side nonwoven fabric from filaments of nano-particle,
That is six side Ag3PO4/Fe3O4/ Co-Ni LDH composites.
Embodiment 3
The present embodiment is with the difference of embodiment 1：
Step 3CH3In the preparation of COOAg, AgNO3The concentration of solution is 2.5mol/L.
In step 4, six side Ag3PO4/Fe3O4The preparation method of/Co-Ni LDH composites is：Take system in above-mentioned steps
The standby 0.0479g Fe for obtaining3O4Nano-particle (0.2067mmol), 0.050gCo-Ni LDH (0.5376mmol) and
Na2HPO41.130g (0.0079mol) is dissolved in the deionized water of 100ml, stirs 24h, rinses out unnecessary Na2HPO4, suction filtration
Black precipitate is obtained, black precipitate is dissolved in CH containing 3.985g3In the 50ml deionized waters of COOAg (0.0237mol), stirring
24h, suction filtration obtains black powder and is dried at room temperature for obtaining Co-Ni loaded Ags3PO4And Fe3O4Six side nonwoven fabric from filaments of nano-particle,
That is six side Ag3PO4/Fe3O4/ Co-Ni LDH composites.
Embodiment 4
The present embodiment is with the difference of embodiment 1：
Step 3CH3In the preparation of COOAg, AgNO3The concentration of solution is 2.5mol/L.
In step 4, six side Ag3PO4/Fe3O4The preparation method of/Co-Ni LDH composites is：Take system in above-mentioned steps
The standby 0.05g Fe for obtaining3O4Nano-particle (0.2155mmol), 0.0417g Co-Ni LDH (0.4489mmol) and 1.130g
Na2HPO4(0.0079mol) is dissolved in the deionized water of 100ml, stirs 24h, rinses out unnecessary Na2HPO4, suction filtration obtains black
Precipitation, CH containing 3.985g is dissolved in by black precipitate3In the 50ml deionized waters of COOAg (0.0237mol), 24h, suction filtration are stirred
Black powder is obtained to be dried at room temperature for obtaining Co-Ni loaded Ags3PO4And Fe3O4Six side nonwoven fabric from filaments of nano-particle, i.e. six sides
Ag3PO4/Fe3O4/ Co-Ni LDH composites.
Embodiment 5
The present embodiment is with the difference of embodiment 1：
Step 3CH3In the preparation of COOAg, AgNO3The concentration of solution is 2.5mol/L.
In step 4, six side Ag3PO4/Fe3O4The preparation method of/Co-Ni LDH composites is：Take system in above-mentioned steps
The standby 0.0398g Fe for obtaining3O4Nano-particle (0.172mmol), 0.05g Co-Ni LDH (0.537mmol) and 1.130g
Na2HPO4(0.0079mol) is dissolved in the deionized water of 100ml, stirs 24h, rinses out unnecessary Na2HPO4, suction filtration obtains black
Precipitation, CH containing 3.985g is dissolved in by black precipitate3In the 50ml deionized waters of COOAg (0.0237mol), 24h, suction filtration are stirred
Black powder is obtained to be dried at room temperature for obtaining Co-Ni loaded Ags3PO4And Fe3O4Six side nonwoven fabric from filaments of nano-particle, i.e. six sides
Ag3PO4/Fe3O4/ Co-Ni LDH composites.
Finally it should be noted that：The preferred embodiments of the present invention are the foregoing is only, are not intended to limit the invention,
Although being described in detail to the present invention with reference to the foregoing embodiments, for a person skilled in the art, it still may be used
Modified with to the technical scheme described in foregoing embodiments, or equivalent is carried out to which part technical characteristic.
All any modification, equivalent substitution and improvements within the spirit and principles in the present invention, made etc., should be included in of the invention
Within protection domain.
Claims (11)
1. the side Ag of a kind of individual layer six3PO4/Fe3O4The preparation method of/Co-Ni LDH composites, it is characterised in that：By Co-Ni
LDH、Fe3O4Nano-particle and Na2HPO4Stirring soluble in water, suction filtration obtains black precipitate, and black precipitate is dissolved in into CH3In COOAg
Stirring, obtains the side Ag of individual layer six of black3PO4/Fe3O4/ Co-Ni LDH composites；Wherein,
The preparation method of the Co-Ni LDH is：By CoCl2·6H2O, NiCl2·6H2O and urotropine are added to
Dissolved in distilled water, mixed liquor is reacted at 120 DEG C, suction filtration after cooling, washing to neutrality is dried, and obtains Co-Ni LDH；
The Co-Ni LDH and Fe3O4The mol ratio of raw material is（1.5-3）：（0.5-1.2）.
2. preparation method according to claim 1, it is characterised in that：The CH3COOAg and Na2HPO4Mol ratio for (
1-3) : (0.5-1.5)。
3. preparation method according to claim 1, it is characterised in that：The Co-Ni LDH and Fe3O4The mol ratio of raw material
It is 2.5:1.
4. according to any described preparation methods of claim 1-3, it is characterised in that：The CH3The preparation method of COOAg is：
AgNO is added dropwise in SAS3Solution, CH3COONa and AgNO3Mol ratio be 1：1；Separate reaction solution, the powder for obtaining
End pickling, dries after removing acid, obtains final product CH3COOAg。
5. method according to claim 4, it is characterised in that：The concentration of the SAS is 0.05-0.15g/ml.
6. method according to claim 4, it is characterised in that：The pickling is washed with acetic acid.
7. method according to claim 4, it is characterised in that：The AgNO3 Concentration be 0.5-2.5mol/L.
8. the side Ag of individual layer six3PO4/Fe3O4/ Co-Ni LDH composites, it is characterised in that：The composite is to apply right
It is required that what any described methods of 1-7 were prepared from.
9. the side Ag of individual layer six described in claim 83PO4/Fe3O4/ Co-Ni LDH composites answering in methyl orange of degrading
With.
10. application according to claim 9, it is characterised in that：The degraded is to degrade under visible light.
11. application according to claim 9 or 10, it is characterised in that：The pH of the methyl orange is 8.
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| 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 |
| CN106513021B (en) * | 2016-11-05 | 2019-06-04 | 上海大学 | Layered hydroxide/BiOCl photocatalytic material and preparation method thereof |
| 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 |
| 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 |
| CN111471997B (en) * | 2020-04-09 | 2022-08-05 | 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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| CN102000594A (en) * | 2010-11-26 | 2011-04-06 | 大连理工大学 | Preparation method of visible light photo catalyst silver and silver phosphate and application thereof |
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| CN102000594A (en) * | 2010-11-26 | 2011-04-06 | 大连理工大学 | Preparation method of visible light photo catalyst silver and silver phosphate and application thereof |
| CN102151577A (en) * | 2011-01-28 | 2011-08-17 | 东华大学 | Ag3PO4/Mg-Al LDO (Layered Double Oxide) visible light composite photo catalyst, preparation and application thereof |
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