CN107754823A - Bi/BiOI/Fe3O4/ attapulgite clay can Magneto separate visible light catalytic material preparation method - Google Patents
Bi/BiOI/Fe3O4/ attapulgite clay can Magneto separate visible light catalytic material preparation method Download PDFInfo
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- CN107754823A CN107754823A CN201710942888.4A CN201710942888A CN107754823A CN 107754823 A CN107754823 A CN 107754823A CN 201710942888 A CN201710942888 A CN 201710942888A CN 107754823 A CN107754823 A CN 107754823A
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- attapulgite clay
- bioi
- magneto separate
- visible light
- catalytic material
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- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 title claims abstract description 75
- 239000004927 clay Substances 0.000 title claims abstract description 70
- 229960000892 attapulgite Drugs 0.000 title claims abstract description 60
- 229910052625 palygorskite Inorganic materials 0.000 title claims abstract description 60
- 239000000463 material Substances 0.000 title claims abstract description 46
- 230000003197 catalytic effect Effects 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims abstract description 38
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000002131 composite material Substances 0.000 claims abstract description 25
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 23
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 9
- 229910002554 Fe(NO3)3·9H2O Inorganic materials 0.000 claims abstract description 6
- PPNKDDZCLDMRHS-UHFFFAOYSA-N dinitrooxybismuthanyl nitrate Chemical class [Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PPNKDDZCLDMRHS-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000000725 suspension Substances 0.000 claims description 16
- 235000019441 ethanol Nutrition 0.000 claims description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 230000032683 aging Effects 0.000 claims description 10
- 238000007789 sealing Methods 0.000 claims description 10
- 238000002525 ultrasonication Methods 0.000 claims description 10
- 239000007787 solid Substances 0.000 claims description 8
- 239000012265 solid product Substances 0.000 claims description 7
- 238000005119 centrifugation Methods 0.000 claims description 5
- CRPOUZQWHJYTMS-UHFFFAOYSA-N dialuminum;magnesium;disilicate Chemical compound [Mg+2].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-].[O-][Si]([O-])([O-])[O-] CRPOUZQWHJYTMS-UHFFFAOYSA-N 0.000 claims description 5
- 239000012153 distilled water Substances 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 125000005909 ethyl alcohol group Chemical group 0.000 claims description 5
- 238000010992 reflux Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- -1 polytetrafluoroethylene Polymers 0.000 claims description 2
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims 2
- 239000004810 polytetrafluoroethylene Substances 0.000 claims 2
- 238000007605 air drying Methods 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 abstract description 7
- 238000006555 catalytic reaction Methods 0.000 abstract description 6
- 238000001179 sorption measurement Methods 0.000 abstract description 5
- 239000011941 photocatalyst Substances 0.000 abstract description 4
- 238000011084 recovery Methods 0.000 abstract description 4
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 239000002904 solvent Substances 0.000 abstract 3
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract 2
- 229910052797 bismuth Inorganic materials 0.000 abstract 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 abstract 1
- 238000003837 high-temperature calcination Methods 0.000 abstract 1
- 229910052742 iron Inorganic materials 0.000 abstract 1
- 239000000203 mixture Substances 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- 239000003054 catalyst Substances 0.000 description 8
- 239000003344 environmental pollutant Substances 0.000 description 6
- 231100000719 pollutant Toxicity 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 230000001699 photocatalysis Effects 0.000 description 5
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 4
- 238000001816 cooling Methods 0.000 description 4
- 230000003647 oxidation Effects 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 238000007146 photocatalysis Methods 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- 239000005416 organic matter Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000003795 desorption Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 150000003254 radicals Chemical class 0.000 description 2
- 230000003595 spectral effect Effects 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 241000208340 Araliaceae Species 0.000 description 1
- 206010019133 Hangover Diseases 0.000 description 1
- 235000005035 Panax pseudoginseng ssp. pseudoginseng Nutrition 0.000 description 1
- 235000003140 Panax quinquefolius Nutrition 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010170 biological method Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000000254 damaging effect Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000004332 deodorization Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000005684 electric field Effects 0.000 description 1
- 235000008434 ginseng Nutrition 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000002779 inactivation Effects 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 230000005415 magnetization Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Classifications
-
- 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
- B01J27/06—Halogens; Compounds thereof
- B01J27/128—Halogens; Compounds thereof with iron group metals or platinum group metals
-
- B01J35/33—
-
- B01J35/39—
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
Abstract
The invention discloses a kind of Bi/BiOI/Fe3O4/ attapulgite clay can Magneto separate visible light catalytic material preparation method, belong to catalysis material preparation field.The inventive method uses secondary solvent thermal process：First, attapulgite clay is carrier, Fe (NO3)3·9H2O is source of iron, and diethylene glycol is solvent, isothermal reaction a few hours, Magneto separate, ethanol washing, dries, obtains Fe3O4/ attapulgite clay composite；Then with Fe3O4/ attapulgite clay composite is carrier, and five water bismuth nitrates are bismuth source, and ethylene glycol/alcohol mixture is solvent, isothermal reaction a few hours, Magneto separate, washes, dries, obtain Bi/BiOI/Fe3O4/ attapulgite clay can Magneto separate visible light catalytic material.The present invention has the advantages that easy to operate, safe and environmental nonpollution without high-temperature calcination.Prepared adsorption photochemical catalysis material specific surface area is big, is easily isolated under magnetic fields, solves nano-photocatalyst material recovery difficult problem.
Description
Technical field
The invention belongs to catalysis material preparation field, is related to a kind of Bi/BiOI/Fe3O4/ attapulgite clay can Magneto separate
Visible light catalytic material.
Background technology
In numerous environmental problems of facing mankind, the processing of the organic pollution of bio-refractory is a difficulty in sewage
Topic.This pollutant is removed due to being difficult to biological method, and very big damaging effect can be produced to environment by being discharged into environment,
So people are seeking to new method to handle this problem.High-level oxidation technology is that had based on formation during the course of the reaction
The free radical of Strong oxdiative ability especially hydroxyl radical free radical decomposes to pollutant, due to free radical oxidability very
By force, can be by various organic matter non-selectivity oxidation Decompositions, so high-level oxidation technology contains difficult degradation particularly suitable for processing
The waste water of organic matter.
As one kind of high-level oxidation technology, photocatalysis method is more than or equal to semiconductor energy gap using energy
Light source irradiates semiconductor, causes the electron transition in valence band to produce hole (h in valence band to conduction band+), electronics is produced on conduction band
(e-), wherein hole can be with adsorbing the hydroxyl (OH in particle surface-) and hydrone (H2O) reaction can be with oxygen into OH, OH
Change organic matter and be degraded to CO2And H2The inorganic molecules such as O.In many semi-conducting materials as photochemical catalyst, TiO2
(Detitanium-ore-type) with its band-gap energy is moderate, strong to the adsorption capacity of pollutant, photocatalytic activity is high and nontoxic, stably, it is inexpensive,
Have the advantages of self-cleaning, deodorization, sterilizing etc. are unique concurrently and widely studied and applied, turn into the green ring with application prospect
One of guarantor's type catalyst.
In numerous novel photocatalysis materials, BiOI is because with unique internal electric field, layer structure, effectively realizing photoproduction
Electronics and the separation in hole, show excellent photocatalysis performance, and enjoy researcher to pay close attention to.But simple BiOI visible rays are urged
Agent is easily reunited inactivation in aqueous, and is difficult to reclaim and the drawback such as recycling makes its application be severely limited.Therefore,
It is big to prepare specific surface area, good dispersion, easily recovery, the BiOI photochemical catalysts that can be recycled turn into the one of current photocatalysis field
Individual focus.
Numerous studies show, can photocatalyst to having on magnetic carrier be effective method：One side
Face, absorption and surface enrichment by carrier, the higher pollutant atmosphere of concentration is formed around visible light catalyst, be visible
Photochemical catalyst provides the light-catalyzed reaction environment of high concentration organic contaminant, and the collision for adding catalyst and pollutant is several
Rate, it is favorably improved the speed of pollutant photocatalytic degradation reaction；On the other hand, photochemical catalyst is made from body by external magnetic field
Fast enriching reclaims in system, and realization recycles.
The content of the invention
Goal of the invention：For the problems of prior art and deficiency, the present invention is intended to provide a kind of Bi/BiOI/
Fe3O4/ attapulgite clay can Magneto separate visible light catalytic material preparation method.This method have it is easy to operate, security compared with
Height, it is environmentally safe the advantages that, the Bi/BiOI/Fe of preparation3O4/ attapulgite clay can Magneto separate visible light catalytic material compare table
Area is big, is easily isolated under magnetic fields, solves nano-photocatalyst material recovery difficult problem, for answering based on Bi/BiOI
Closing light catalysis material opens new development prospect.
Technical scheme：A kind of Bi/BiOI/Fe3O4/ attapulgite clay can Magneto separate visible light catalytic material preparation method,
Comprise the following steps：
1) sour modified attapulgite clay is prepared
2g attapulgite clays are taken to be added in the hydrochloric acid solution that 50mL concentration is 1~5mol/L, in 80~110 DEG C of oil baths
In, 2~6h is stirred at reflux with 300~700r/min of rotating speed；Centrifugation is washed to pH as neutrality, the air blast at 105 DEG C of gained solid
Dry, ground 200 mesh sieve is standby；
2) Fe is prepared3O4/ attapulgite clay composite
Take 0.79g Fe (NO3)3·9H2O is dissolved in 65mL diethylene glycols, then adds the above-mentioned Fe of 0.5g3O4/ concave convex rod
Clay composite material, 15~60min of ultrasonication, is uniformly dispersed, and it is polytetrafluoro that above-mentioned suspension is transferred into 100mL liners
12~24h of ageing, natural cooling in 180~240 DEG C of electric drying oven with forced convection are placed in the autoclave of ethene, after sealing
To room temperature, solid product is collected with magnet, after being washed 5-6 times with ethanol, dry 8~12h produces Fe at 60 DEG C3O4/ concave convex rod
Clay composite material；
3) Bi/BiOI/Fe is prepared3O4/ attapulgite clay can Magneto separate visible light catalytic material
Take the water bismuth nitrates of 0.024g five to be dissolved in 5mL ethylene glycol and form solution A；0.008g KIs are taken to be dissolved in 5mL ethylene glycol
Form solution B；By 0.02~0.06g Fe3O4/ attapulgite clay composite is scattered in 25mL absolute ethyl alcohols under ultrasonication
Middle formation suspension C.It is added dropwise to after A and B solution are well mixed in suspension C, 50mL height is transferred to after stirring
Press in reactor, 12~48h of ageing in 160~240 DEG C of air dry ovens is placed in after sealing, room temperature is naturally cooled to, uses magnet
Solid product is collected, is alternately washed with distilled water and ethanol, 8~12h is dried at 60 DEG C and produces Bi/BiOI/Fe3O4/ concave convex rod
Clay can Magneto separate visible light catalytic material.
Beneficial effect：It is of the invention to be compared with existing technology, successfully synthesize Bi/BiOI/Fe3O4/ attapulgite clay can magnetic
Visible light catalytic material is separated, the preparation method has the advantages that easy to operate, safe and environmental nonpollution, prepared
Bi/BiOI/Fe3O4/ attapulgite clay can Magneto separate visible light catalytic material specific surface area be big, is easy under magnetic fields point
From, solve the problems, such as nano-photocatalyst material recovery it is difficult, opened for the composite visible light catalytic material based on Bi/BiOI
New development prospect.
Brief description of the drawings
Fig. 1 is sour modified attapulgite clay (a), Fe3O4/ attapulgite clay composite (b), Bi/BiOI/Fe3O4/ recessed
Convex rod clay can Magneto separate visible light catalytic material (c) X diffraction (XRD) figure.
Fig. 2 is Bi/BiOI/Fe3O4/ attapulgite clay can Magneto separate visible light catalytic material adsorption isothermal curve figure and
Graph of pore diameter distribution (illustration).
Fig. 3 is Fe3O4/ attapulgite clay composite (a), Bi/BiOI/Fe3O4/ attapulgite clay can Magneto separate it is visible
Vibrating specimen magnetometer (VSM) figure of catalysis material (b).
Embodiment
With reference to specific embodiment, the present invention will be described in detail.
Specific embodiment 1：
A kind of Bi/BiOI/Fe3O4/ attapulgite clay can Magneto separate visible light catalytic material preparation method, it is including following
Step：
1) sour modified attapulgite clay is prepared
2g attapulgite clays are taken to be added in the hydrochloric acid solution that 50mL concentration is 1~5mol/L, in 80~110 DEG C of oil baths
In, 2~6h is stirred at reflux with 300~700r/min of rotating speed；Centrifugation is washed to pH as neutrality, the air blast at 105 DEG C of gained solid
Dry, ground 200 mesh sieve is standby；
2) Fe is prepared3O4/ attapulgite clay composite
Take 0.79g Fe (NO3)3·9H2O is dissolved in 65mL diethylene glycols, then adds the above-mentioned Fe of 0.5g3O4/ concave convex rod
Clay composite material, 15~60min of ultrasonication, is uniformly dispersed, and it is polytetrafluoro that above-mentioned suspension is transferred into 100mL liners
12~24h of ageing, natural cooling in 180~240 DEG C of electric drying oven with forced convection are placed in the autoclave of ethene, after sealing
To room temperature, solid product is collected with magnet, after being washed 5-6 times with ethanol, dry 8~12h produces Fe at 60 DEG C3O4/ concave convex rod
Clay composite material；
3) Bi/BiOI/Fe is prepared3O4/ attapulgite clay can Magneto separate visible light catalytic material
Take the water bismuth nitrates of 0.024g five to be dissolved in 5mL ethylene glycol and form solution A；0.008g KIs are taken to be dissolved in 5mL ethylene glycol
Form solution B；By 0.02g Fe3O4/ attapulgite clay composite, which is scattered under ultrasonication in 25mL absolute ethyl alcohols, to be formed
Suspension C.It is added dropwise to after A and B solution are well mixed in suspension C, 50mL reaction under high pressures is transferred to after stirring
12~48h of ageing in 160~240 DEG C of air dry ovens is placed in kettle, after sealing, naturally cools to room temperature, is collected with magnet solid
Body product, is alternately washed with distilled water and ethanol, and 8~12h is dried at 60 DEG C and produces Bi/BiOI/Fe3O4/ attapulgite clay can
Magneto separate visible light catalytic material.
Specific embodiment 2：
A kind of Bi/BiOI/Fe3O4/ attapulgite clay can Magneto separate visible light catalytic material preparation method, it is including following
Step：
1) sour modified attapulgite clay is prepared
2g attapulgite clays are taken to be added in the hydrochloric acid solution that 50mL concentration is 1~5mol/L, in 80~110 DEG C of oil baths
In, 2~6h is stirred at reflux with 300~700r/min of rotating speed；Centrifugation is washed to pH as neutrality, the air blast at 105 DEG C of gained solid
Dry, ground 200 mesh sieve is standby；
2) Fe is prepared3O4/ attapulgite clay composite
Take 0.79g Fe (NO3)3·9H2O is dissolved in 65mL diethylene glycols, then adds the above-mentioned Fe of 0.5g3O4/ concave convex rod
Clay composite material, 15~60min of ultrasonication, is uniformly dispersed, and it is polytetrafluoro that above-mentioned suspension is transferred into 100mL liners
12~24h of ageing, natural cooling in 180~240 DEG C of electric drying oven with forced convection are placed in the autoclave of ethene, after sealing
To room temperature, solid product is collected with magnet, after being washed 5-6 times with ethanol, dry 8~12h produces Fe at 60 DEG C3O4/ concave convex rod
Clay composite material；
3) Bi/BiOI/Fe is prepared3O4/ attapulgite clay can Magneto separate visible light catalytic material
Take the water bismuth nitrates of 0.024g five to be dissolved in 5mL ethylene glycol and form solution A；0.008g KIs are taken to be dissolved in 5mL ethylene glycol
Form solution B；By 0.04g Fe3O4/ attapulgite clay composite, which is scattered under ultrasonication in 25mL absolute ethyl alcohols, to be formed
Suspension C.It is added dropwise to after A and B solution are well mixed in suspension C, 50mL reaction under high pressures is transferred to after stirring
12~48h of ageing in 160~240 DEG C of air dry ovens is placed in kettle, after sealing, naturally cools to room temperature, is collected with magnet solid
Body product, is alternately washed with distilled water and ethanol, and 8~12h is dried at 60 DEG C and produces Bi/BiOI/Fe3O4/ attapulgite clay can
Magneto separate visible light catalytic material.
Specific embodiment 3：
A kind of Bi/BiOI/Fe3O4/ attapulgite clay can Magneto separate visible light catalytic material preparation method, it is including following
Step：
1) sour modified attapulgite clay is prepared
2g attapulgite clays are taken to be added in the hydrochloric acid solution that 50mL concentration is 1~5mol/L, in 80~110 DEG C of oil baths
In, 2~6h is stirred at reflux with 300~700r/min of rotating speed；Centrifugation is washed to pH as neutrality, the air blast at 105 DEG C of gained solid
Dry, ground 200 mesh sieve is standby；
2) Fe is prepared3O4/ attapulgite clay composite
Take 0.79g Fe (NO3)3·9H2O is dissolved in 65mL diethylene glycols, then adds the above-mentioned Fe of 0.5g3O4/ concave convex rod
Clay composite material, 15~60min of ultrasonication, is uniformly dispersed, and it is polytetrafluoro that above-mentioned suspension is transferred into 100mL liners
12~24h of ageing, natural cooling in 180~240 DEG C of electric drying oven with forced convection are placed in the autoclave of ethene, after sealing
To room temperature, solid product is collected with magnet, after being washed 5-6 times with ethanol, dry 8~12h produces Fe at 60 DEG C3O4/ concave convex rod
Clay composite material；
3) Bi/BiOI/Fe is prepared3O4/ attapulgite clay can Magneto separate visible light catalytic material
Take the water bismuth nitrates of 0.024g five to be dissolved in 5mL ethylene glycol and form solution A；0.008g KIs are taken to be dissolved in 5mL ethylene glycol
Form solution B；By 0.06g Fe3O4/ attapulgite clay composite, which is scattered under ultrasonication in 25mL absolute ethyl alcohols, to be formed
Suspension C.It is added dropwise to after A and B solution are well mixed in suspension C, 50mL reaction under high pressures is transferred to after stirring
12~48h of ageing in 160~240 DEG C of air dry ovens is placed in kettle, after sealing, naturally cools to room temperature, is collected with magnet solid
Body product, is alternately washed with distilled water and ethanol, and 8~12h is dried at 60 DEG C and produces Bi/BiOI/Fe3O4/ attapulgite clay can
Magneto separate visible light catalytic material.
Experimental result
The Bi/BiOI/Fe that embodiment 2 is prepared3O4/ attapulgite clay can the X ray of Magneto separate visible light catalytic material spread out
Test result is penetrated as shown in spectral line c in Fig. 1.Both occurred BiOI diffraction maximum in spectral line c, and illustrated BiOI crystal structures shape
Into also there is simple substance Bi diffraction maximum, come from BiOI and decompose under the high temperature conditions and generate metal simple-substance Bi；On the other hand,
Attapulgite clay and Fe3O4Diffraction maximum still have, it is meant that prepare Bi/BiOI/Fe3O4/ attapulgite clay can Magneto separate
Without change attapulgite clay and Fe during visible light catalytic material3O4Structure, illustrate that the inventive method is successfully prepared
Bi/BiOI/Fe3O4/ attapulgite clay can Magneto separate visible light catalytic material.
The Bi/BiOI/Fe that embodiment 2 is prepared3O4/ attapulgite clay can Magneto separate visible light catalytic material absorption etc.
Warm curve is as shown in Figure 2.Bi/BiOI/Fe3O4/ attapulgite clay can Magneto separate visible light catalytic material nitrogen adsorption and desorption
Thermoisopleth belongs to IV types characterization of adsorption and H3 types return stagnant ring.Return stagnant ring all to start to occur in medium relative pressure, illustrate Bi/
BiOI/Fe3O4/ attapulgite clay can Magneto separate visible light catalytic material exist a certain amount of mesoporous, and be by gathering particle mostly
The irregular slit pore formed.In relative pressure close to 1 region, thermoisopleth has the hangover of last rising, with reference to Fig. 2
Knowable to illustration pore size distribution curve, Bi/BiOI/Fe3O4/ attapulgite clay can Magneto separate visible light catalytic material pore-size distribution compared with
Extensively, there is mesoporous and macropore diameter.Analysis based on BJH methods to desorption curve, Bi/BiOI/Fe3O4/ attapulgite clay can magnetic
It is 13.62nm, pore volume 0.37cm to separate visible light catalytic material aperture3/g.Analysis method based on BET, Bi/BiOI/
Fe3O4/ attapulgite clay can the specific surface area of Magneto separate visible light catalytic material be 114.32m2/g。
The Bi/BiOI/Fe that embodiment 2 is prepared3O4/ attapulgite clay can Magneto separate visible light catalytic material magnetic ginseng
For number test result as shown in curve b in Fig. 3, its saturation magnetization is 13.24emu/g, illustrates that the compound is at room temperature
Existing superparamagnetism.In the suspension that can be seen that after degraded from Fig. 3 illustration, catalyst is firmly adsorbed on magnet, explanation
Magnetic property is good, is easily recycled.
Claims (1)
- A kind of 1. Bi/BiOI/Fe3O4/ attapulgite clay can Magneto separate visible light catalytic material preparation method, it is characterised in that This method comprises the following steps：1) sour modified attapulgite clay is prepared2g attapulgite clays are taken to be added in the hydrochloric acid solution that 50mL concentration is 1~5mol/L, in 80~110 DEG C of oil baths, with 300~700r/min of rotating speed is stirred at reflux 2~6h；Centrifugation is washed to pH as neutrality, the forced air drying at 105 DEG C of gained solid, Ground 200 mesh sieve, it is standby；2) Fe is prepared3O4/ attapulgite clay compositeTake 0.79g Fe (NO3)3·9H2O is dissolved in 65mL diethylene glycols, then adds the above-mentioned Fe of 0.5g3O4/ attapulgite clay Composite, 15~60min of ultrasonication, is uniformly dispersed, and it is polytetrafluoroethylene (PTFE) that above-mentioned suspension is transferred into 100mL liners Autoclave in, 12~24h of ageing is placed in 180~240 DEG C of electric drying oven with forced convection after sealing, naturally cools to room Temperature, solid product is collected with magnet, after being washed 5-6 times with ethanol, dry 8~12h produces Fe at 60 DEG C3O4/ attapulgite clay Composite；3) Bi/BiOI/Fe is prepared3O4/ attapulgite clay can Magneto separate visible light catalytic materialTake the water bismuth nitrates of 0.024g five to be dissolved in 5mL ethylene glycol and form solution A；Take 0.008g KIs to be dissolved in 5mL ethylene glycol to be formed Solution B；By 0.02~0.06g Fe3O4/ attapulgite clay composite is scattered in shape in 25mL absolute ethyl alcohols under ultrasonication Into suspension C.It is added dropwise to after A and B solution are well mixed in suspension C, it is anti-that 50mL high pressures is transferred to after stirring Answer in kettle, 12~48h of ageing in 160~240 DEG C of air dry ovens is placed in after sealing, room temperature is naturally cooled to, is collected with magnet Solid product, is alternately washed with distilled water and ethanol, and 8~12h is dried at 60 DEG C and produces Bi/BiOI/Fe3O4/ attapulgite clay Can Magneto separate visible light catalytic material.
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| CN110586067A (en) * | 2019-09-20 | 2019-12-20 | 太原理工大学 | Bi/Bi2SiO5Preparation method and application of photocatalyst |
| CN110586067B (en) * | 2019-09-20 | 2022-08-05 | 太原理工大学 | Bi/Bi 2 SiO 5 Preparation method and application of photocatalyst |
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