CN107029757A - A kind of preparation method of BiOX diatomite composite photocatalytic agent - Google Patents
A kind of preparation method of BiOX diatomite composite photocatalytic agent Download PDFInfo
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- CN107029757A CN107029757A CN201710364831.0A CN201710364831A CN107029757A CN 107029757 A CN107029757 A CN 107029757A CN 201710364831 A CN201710364831 A CN 201710364831A CN 107029757 A CN107029757 A CN 107029757A
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- diatomite
- biox
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- composite photocatalytic
- photocatalytic agent
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 114
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 54
- 239000002131 composite material Substances 0.000 title claims abstract description 53
- 238000002360 preparation method Methods 0.000 title claims abstract description 32
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 239000000463 material Substances 0.000 claims abstract description 22
- 229910001868 water Inorganic materials 0.000 claims abstract description 17
- 238000005406 washing Methods 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 11
- 238000001914 filtration Methods 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims description 15
- BWOROQSFKKODDR-UHFFFAOYSA-N oxobismuth;hydrochloride Chemical group Cl.[Bi]=O BWOROQSFKKODDR-UHFFFAOYSA-N 0.000 claims description 13
- 239000000047 product Substances 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 238000002156 mixing Methods 0.000 claims description 11
- 239000011941 photocatalyst Substances 0.000 claims description 7
- 239000000725 suspension Substances 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 239000002002 slurry Substances 0.000 claims description 6
- 238000003828 vacuum filtration Methods 0.000 claims description 6
- 230000015572 biosynthetic process Effects 0.000 claims description 5
- 238000003786 synthesis reaction Methods 0.000 claims description 5
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- JHJLBTNAGRQEKS-UHFFFAOYSA-M sodium bromide Chemical compound [Na+].[Br-] JHJLBTNAGRQEKS-UHFFFAOYSA-M 0.000 claims description 4
- 239000012065 filter cake Substances 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 239000002689 soil Substances 0.000 claims description 3
- 239000004566 building material Substances 0.000 claims description 2
- 239000011780 sodium chloride Substances 0.000 claims description 2
- 238000004887 air purification Methods 0.000 claims 1
- 239000010426 asphalt Substances 0.000 claims 1
- 239000011248 coating agent Substances 0.000 claims 1
- 238000000576 coating method Methods 0.000 claims 1
- 239000003607 modifier Substances 0.000 claims 1
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 abstract description 21
- 229940043267 rhodamine b Drugs 0.000 abstract description 18
- 239000003054 catalyst Substances 0.000 abstract description 14
- 238000000034 method Methods 0.000 abstract description 10
- 230000015556 catabolic process Effects 0.000 abstract description 7
- 238000006731 degradation reaction Methods 0.000 abstract description 7
- 239000000975 dye Substances 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 4
- 230000007062 hydrolysis Effects 0.000 abstract description 4
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 4
- 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 abstract description 2
- 239000000126 substance Substances 0.000 abstract description 2
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 abstract 2
- IOLCXVTUBQKXJR-UHFFFAOYSA-M potassium bromide Chemical compound [K+].[Br-] IOLCXVTUBQKXJR-UHFFFAOYSA-M 0.000 abstract 1
- 235000011164 potassium chloride Nutrition 0.000 abstract 1
- 239000001103 potassium chloride Substances 0.000 abstract 1
- 238000001556 precipitation Methods 0.000 abstract 1
- 239000000523 sample Substances 0.000 description 32
- 238000007146 photocatalysis Methods 0.000 description 10
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 description 9
- 238000010521 absorption reaction Methods 0.000 description 8
- JHXKRIRFYBPWGE-UHFFFAOYSA-K bismuth chloride Chemical compound Cl[Bi](Cl)Cl JHXKRIRFYBPWGE-UHFFFAOYSA-K 0.000 description 8
- 239000005909 Kieselgur Substances 0.000 description 7
- 229910002651 NO3 Inorganic materials 0.000 description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 6
- 230000003197 catalytic effect Effects 0.000 description 6
- 238000010586 diagram Methods 0.000 description 6
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 5
- 229910052710 silicon Inorganic materials 0.000 description 5
- 239000010703 silicon Substances 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 4
- 238000006555 catalytic reaction Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 239000000356 contaminant Substances 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 238000005286 illumination Methods 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 239000004408 titanium dioxide Substances 0.000 description 3
- 241000206761 Bacillariophyta Species 0.000 description 2
- 241001025261 Neoraja caerulea Species 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- -1 diatomite series compound Chemical class 0.000 description 2
- 239000000686 essence Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 230000001788 irregular Effects 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 229910017488 Cu K Inorganic materials 0.000 description 1
- 229910017541 Cu-K Inorganic materials 0.000 description 1
- 241001269238 Data Species 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 238000003915 air pollution Methods 0.000 description 1
- 238000003556 assay Methods 0.000 description 1
- 230000000035 biogenic effect Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- 239000012496 blank sample Substances 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- RKTYLMNFRDHKIL-UHFFFAOYSA-N copper;5,10,15,20-tetraphenylporphyrin-22,24-diide Chemical compound [Cu+2].C1=CC(C(=C2C=CC([N-]2)=C(C=2C=CC=CC=2)C=2C=CC(N=2)=C(C=2C=CC=CC=2)C2=CC=C3[N-]2)C=2C=CC=CC=2)=NC1=C3C1=CC=CC=C1 RKTYLMNFRDHKIL-UHFFFAOYSA-N 0.000 description 1
- 239000007857 degradation product Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- OGGXGZAMXPVRFZ-UHFFFAOYSA-N dimethylarsinic acid Chemical compound C[As](C)(O)=O OGGXGZAMXPVRFZ-UHFFFAOYSA-N 0.000 description 1
- 230000003292 diminished effect Effects 0.000 description 1
- 239000003937 drug carrier Substances 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 238000013032 photocatalytic reaction Methods 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000010408 sweeping Methods 0.000 description 1
- ZWYDDDAMNQQZHD-UHFFFAOYSA-L titanium(ii) chloride Chemical compound [Cl-].[Cl-].[Ti+2] ZWYDDDAMNQQZHD-UHFFFAOYSA-L 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 238000003911 water pollution Methods 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
-
- 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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
- C02F1/32—Treatment of water, waste water, or sewage by irradiation with ultraviolet light
-
- 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
- C02F2101/308—Dyes; Colorants; Fluorescent agents
Abstract
The invention belongs to catalyst technical field, disclose a kind of preparation method of BiOX diatomite composite photocatalytic agent, it is carrier by the smart diatomite of raw material, using five water bismuth nitrates, potassium chloride, KBr and KI as presoma, BiOX/diatomite composite photocatalytic material is synthesized using the normal temperature direct hydrolysis precipitation method, composite obtains finished product after filtering, washing, drying.The BiOX of the present invention is successfully loaded on diatomite rotary strainer and is sheet hierarchy；It is 15mg/L in dyestuff initial concentration, catalyst amount is that the degradation rate of rhodamine B under conditions of 0.15g, 50W LED blue light light irradiations 50min has reached 86.7% under equal conditions；Preparation technology is simple, and raw material is easy to get, and product can be removed thoroughly in air and harmful substance in water under visible light, with low cost, be had a good application prospect.
Description
Technical field
The invention belongs to the system of catalyst technical field, more particularly to a kind of BiOX-diatomite composite photocatalytic agent
Preparation Method.
Background technology
With industrialized rapid deployment, poisonous and harmful organic pollution materials enter environment, and pollution also begins to serious threat
The psychosomatic development of the mankind.Diatomite is biogenic siliceous sedimentary rock, because its light weight, porous and hole are in regular point
Cloth, aperture can be used for adsorbing organic and inorganic substances work(between more than ten nanometers to hundreds of nanometers with larger specific surface area
Can, there is good application prospect in terms of field of environment protection particularly water pollution and Air Pollution Control.But research is found,
It is simple to mainly use diatomaceous absorption property to adsorb contaminant molecule on its surface using Process of Wastewater with Diatomite waste gas
In duct, environment temperature it is higher etc. it is special in the case of, adsorbed contaminant molecule desorbs to form secondary dirt again
Dye.Also there is researcher that the composite photocatalyst material of titanium dioxide/diatomite will be made on titanium dichloride load to diatomite, can be with
Make full use of the organic pollution in the photocatalysis and the thorough environment purification of diatomaceous absorption property of titanium dioxide.But
Also in preparation technology long flow path, it is necessary to high-temperature calcination, and titanium dioxide forbidden band is wider, obtained product visible light catalytic effect
It is undesirable, so using being subject to certain restrictions.
In summary, the problem of prior art is present be：BiOX is easy to get as a kind of photochemical catalyst with raw material,
Preparation technology is simple, can be removed the organic pollution in environment directly as visible-light photocatalysis material by excited by visible light,
But it is smaller to there is specific surface area, the problem of limited sorption capacity.
The content of the invention
The problem of existing for prior art, the invention provides a kind of BiOX-diatomite composite photocatalytic agent
Preparation method.
The present invention is achieved in that a kind of preparation method of BiOX/diatomite composite photocatalytic agent, the oxyhalogen
The preparation method for changing bismuth/diatomite composite photocatalytic agent comprises the following steps：
Step one, according to parts by weight KX or NaX：Water：The ﹣ 500 of smart diatomite=20：2000 ﹣ 10000：100 ﹣'s 4000
After ratio mixing, 5 ﹣ 30min are stirred, slurry is made；X is Cl, Br, I；
Step 2, according to parts by weight Bi (NO3)3·5H2O：KX or NaX=500 ﹣ 1500:20 ﹣ 400, weigh Bi
(NO3)3·5H2O is added in above-mentioned slurrying liquid, 5 ﹣ 30min of quick stirring, and reaction is hydrolyzed, BiOX/diatomite is synthesized
Compound particle；
Step 3, the BiOX of above-mentioned synthesis/composite diatomite particle slurry is filtered, according to weight fraction essence
Diatomite：The ﹣ 4000 of water=100：1000 ﹣ 40000 ratio adds water and carries out filtration washing；
Step 4, the filter cake after above-mentioned filtration washing is put into drying box and is dried, and drying temperature is 60 DEG C of ﹣ 300
DEG C, to moisture content be 0% ﹣ 7% when stop drying, by after dried material scattering pack obtain finished product.
Further, the BiOX/diatomite is BiOCl/ diatomite, BiOI/ diatomite, BiOBr/ diatomite.
Further, the preparation method of the BiOX/diatomite composite photocatalytic agent comprises the following steps：
It is prepared by the BiOCl/ diatomite:Precise 2.8mmol KCl or NaCl, be completely dissolved in 80mL go from
In sub- water, then a certain proportion of diatomite is added thereto, 10min, then precise 2.8mmol Bi (NO is stirred3)3·
5H2Stirring mixing 30min in the O above-mentioned suspension of addition；Resulting solution is subjected to vacuum filtration washing, most after dry at 95 DEG C
Dry rear material moisture obtains finished product less than 7%.
Further, the preparation method of the BiOX/diatomite composite photocatalytic agent comprises the following steps：
It is prepared by the BiOBr/ diatomite:Precise 2.8mmol KBr or NaBr, be completely dissolved in 80mL go from
In sub- water, then a certain proportion of diatomite is added thereto, 10min, then precise 2.8mmol Bi (NO is stirred3)3·
5H2Stirring mixing 30min in the O above-mentioned suspension of addition；Resulting solution is subjected to vacuum filtration washing, most after dry at 95 DEG C
Dry rear material moisture obtains finished product less than 7%.
Further, the preparation method of the BiOX/diatomite composite photocatalytic agent comprises the following steps：
It is prepared by the BiOI/ diatomite:Precise 2.8mmol KI or NaI, is completely dissolved in 80mL deionized water
In, then a certain proportion of diatomite is added thereto, 10min, then precise 2.8mmol Bi (NO is stirred3)3·5H2O's
Add stirring mixing 30min in above-mentioned suspension；Resulting solution is subjected to vacuum filtration washing, the thing most after being dried at 95 DEG C
Material moisture obtains finished product less than 7%.
Another object of the present invention is to provide a kind of preparation by the=BiOX-diatomite composite photocatalytic agent
BiOX-diatomite composite photocatalytic agent prepared by method.
Another object of the present invention is to provide a kind of life prepared by the BiOX-diatomite composite photocatalytic agent
State building materials.
Another object of the present invention is to provide a kind of agriculture prepared by the BiOX-diatomite composite photocatalytic agent
Drug carrier.
Another object of the present invention is to provide a kind of drip prepared by the BiOX-diatomite composite photocatalytic agent
Blue or green modifying agent.
It is a kind of by prepared by the BiOX-diatomite composite photocatalytic agent answering another object of the present invention is to provide
Condensation material.
Advantages of the present invention and good effect are：Using this porosity of diatomite as carrier, using a kind of easy to implement
Method, which loads to BiOX on diatomite, is prepared for BiOX (X=Br, Cl, I)；With five water bismuth nitrates, KX (X=Cl, Br, I), silicon
Diatomaceous earth is raw material, is prepared for the different BiOX/ diatomite composite photocatalytic agent of mass ratio using direct hydrolysis method, and carry out
XRD and SEM phenetic analysis, while using rhodamine B for target degradation product, is investigated using 50W LED purple lights/blue-ray light as light source
Prepare the visible light photocatalysis performance of photochemical catalyst.As a result show that BiOX is successfully loaded on diatomite rotary strainer and is classified for sheet
Under structure, equal conditions, there is the composite photo-catalyst that 1.0g tripolite loadings BiOBr is obtained in hydrolyzation system optimal light to urge
Change performance, be 15mg/L in dyestuff initial concentration, under conditions of catalyst amount is 0.15g, 50WLED blue light light irradiations 50min
The degradation rate of rhodamine B has reached 86.7%.
Brief description of the drawings
Fig. 1 is the preparation method flow chart of BiOX provided in an embodiment of the present invention-diatomite composite photocatalytic agent.
Fig. 2 is SEM figures (A, the B of sample provided in an embodiment of the present invention:Pure silicon diatomaceous earth；C,D:No. 1 sample).
Fig. 3 is the XRD schematic diagrames of sample provided in an embodiment of the present invention.
Fig. 4 is that different samples are degraded schematic diagram to rhodamine B under blue light provided in an embodiment of the present invention.
Fig. 5 is that different samples are degraded schematic diagram to rhodamine B under purple light provided in an embodiment of the present invention.
Fig. 6 be under blue light provided in an embodiment of the present invention different quality than shadow that BiOBr/ diatomite is degraded to rhodamine B
Ring schematic diagram.
Fig. 7 be under purple light provided in an embodiment of the present invention different quality than shadow that BiOBr/ diatomite is degraded to rhodamine B
Ring schematic diagram.
Fig. 8 is the XRD schematic diagrames of sample provided in an embodiment of the present invention.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.
The application principle of the present invention is explained in detail below in conjunction with the accompanying drawings.
As shown in figure 1, the preparation method of BiOX provided in an embodiment of the present invention-diatomite composite photocatalytic agent includes
Following steps：
S101：According to parts by weight KX or NaX：Water：The ﹣ 500 of smart diatomite=20：2000 ﹣ 10000：100 ﹣ 4000 ratio
After example mixing, 5 ﹣ 30min are stirred, slurry is made；X is Cl, Br, I；
S102：According to parts by weight Bi (NO3)3·5H2O：KX or NaX=500 ﹣ 1500:20 ﹣ 400, weigh Bi (NO3)3·
5H2O is added in above-mentioned slurrying liquid, 5 ﹣ 30min of quick stirring, and reaction, synthesis BiOX/composite diatomite grain is hydrolyzed
Son；
S103：The BiOX of above-mentioned synthesis/composite diatomite particle slurry is filtered, according to the smart silicon of weight fraction
Diatomaceous earth：The ﹣ 4000 of water=100：1000 ﹣ 40000 ratio adds water and carries out filtration washing；
S104：Filter cake after above-mentioned filtration washing is put into drying box and is dried, drying temperature is 60 DEG C of 300 DEG C of ﹣,
To moisture content be 0% ﹣ 7% when stop drying, by after dried material scattering pack obtain finished product.
In BiOBr/ diatomite：
Diatomite 1.0g, bismuth nitrate 2.8mmol, KBr2.8mmol.
Diatomite 1.5g, bismuth nitrate 2.8mmol, KBr2.8mmol.
Diatomite 2g, bismuth nitrate 2.8mmol, KBr2.8mmol.
In BiOI/ diatomite：
Diatomite 1.0g, bismuth nitrate 2.8mmol, KI2.8mmol.
Diatomite 1.5g, bismuth nitrate 2.8mmol, KI2.8mmol.
Diatomite 2g, bismuth nitrate 2.8mmol, KI2.8mmol.
In BiOCl/ diatomite：
Diatomite 1.0g, bismuth nitrate 2.8mmol, KCl2.8mmol.
Diatomite 1.5g, bismuth nitrate 2.8mmol, KCl2.8mmol.
Diatomite 2g, bismuth nitrate 2.8mmol, KCl2.8mmol.
The application effect of the present invention is explained in detail with reference to experiment.
1 experimental section
The preparation of 1.1 BiOXs-diatomite composite photocatalytic agent
Precise 2.8mmol KX (X=Cl, Br, I), is completely dissolved in 80mL deionized water, then will be certain
The diatomite of ratio is added thereto, quick dispersed with stirring 10min, then precise 2.8mmolBi (NO3)3·5H2In O addition
State quick stirring mixing mixing 30min in suspension.Resulting solution is filtered by vacuum, it is most standby after drying 6h at 95 DEG C
With.Sample Prep Protocol is as shown in table 1：
Table 1 different samples prepare experimental program
The sign of 1.2 samples
Test obtained sample powder and its phase structure is characterized using RigakuD/max-2550 diffractometers, XRD tests are adopted
It is Cu-K α targets, it is 2 θ angles from 5 ° to 90 ° that accelerating potential and electric current, which are respectively 40kV and 200mA. surface sweepings scope, and step-length is
0.02°.To observe the pattern and fine structure of material, the surface topography of prepared sample is aobvious using Quanta-250 scanning electrons
Micro mirror (SEM) is observed.
1.3 photocatalytic activities are tested
Catalytic activity experiment is carried out in homemade photocatalytic reaction device, and the reaction instrument is (main equipped with 50W LED ultraviolet lights
Wavelength 400nm), blue-ray light (dominant wavelength 450nm), between light source and reaction solution distance is 14cm, and reaction solution is 100mL
15mg/L rhodamine Bs (structural information is as shown in table 2) deionized water solution, the catalyst sample for adding 0.15g is fully dispersed mixed
Close uniform.Before light-catalyzed reaction, first dark reaction 30 minutes makes to reach that adsorption/desorption is balanced between dyestuff and catalyst sample,
Then open light source, continue to react in 50min, course of reaction every 10min samplings with water system syringe filter (diameter 13mm,
0.45 μm of aperture) separation, supernatant is finally used into UV, visible light spectrophotometric at the maximum absorption wavelength 554nm of rhodamine B
Meter (UV-1800, Shimadzu, Japan) determines its concentration and analyzed.
The molecular structure of the rhodamine B of table 2
2 results are with discussing
2.1 phenetic analysis
Fig. 2 is the SEM figures for preparing sample.Wherein, Fig. 2A, Fig. 2 B correspondences are the SEM figures of pure diatomaceous earth sample, from figure
It can be seen that diatomite is the diatomite of rotary strainer shape, diameter possesses 300nm or so micropore on 30 microns, rotary strainer,
It is that, with pore passage structure, this has certain adsorption capacity for polluter to illustrate diatomite.Fig. 2 C and Fig. 2 D are corresponded to
Hydrolyze method is in the sample SEM figures obtained using diatomite as substrate loading BiOBr.As seen from the figure, compared with blank sample, on rotary strainer
The duct being largely evenly distributed has been reduced or diminished, while it is irregular to possess substantial amounts of nanometer sheet composition on sieve aperture
Hierarchy, this sheet hierarchy material that newly increases should be the BiOBr visible light photocatalysis formed in hydrolytic process
Material, this is confirmed in subsequent XRD analysis of spectrum.Thus morphology analysis is understood, BiOX/ silicon is prepared by neutralizing hydrolysis
Diatomaceous earth composite photo-catalyst is feasible, and its fundamental reaction principle is by such as formula (1) of BiOCl to shown in (4).
Convert Bi (NO3)3+ 3KCl=BiCl3+3NaNO3 (1)
Hydrolyze Bi3++Cl-+2H2O=Bi (OH)2Cl+2H+ (2)
Bi(OH)2Cl=BiOCl ↓+H2O (3)
Overall reaction is BiCl3+H2O=BiOCl ↓+2HCl (4)
Fig. 3 illustrates prepared BiOX/ diatomite series compound and diatomaceous XRD spectra as seen from the figure, pure silicon
There is the Quartz Characteristics peak of high intensity in the diffraction maximum of diatomaceous earth sample, illustrate that diatomite is main by quartzy material composition.It is negative in hydrolysis
Carry after BiOX, the diffracted intensity at this feature peak has weakened, and occurs in that each material of BiOX respectively in the sample
Characteristic peak.Understood with reference to the data in powder diffraction JCPDS card datas storehouse, the diffractive features peak of diatomaceous earth sample all with standard
Card coincide.BiOX/ diatomite series compound can be not only detected from tetragonal crystal system BiOCl (JCPDS card NO.82-
0485), BiOBr (JCPDS card NO.78-0348), BiOI (JCPDS card NO.73-2062) diffraction maximum, these are said
Bright BiOX is successfully loaded.In addition, the diffraction maximum of three kinds of products is all more sharp, this shows that the crystallinity of crystal is higher.For
For BiOCl/ diatomite, BiOBr/ diatomite and BiOI/ diatomite, in (001) diffraction maximum observed near 10 ° then
It is that it is grown along c-axis caused by the periodic layer structure produced.
2.2 photocatalytic activity evaluation
Fig. 4 is prepared No. 1, No. 4, the degradation results of No. 7 samples rhodamine B under LED blue light light irradiations.Can from figure
To find out, under the conditions of blank assay, illumination is hardly degraded effect to rhodamine B.Meanwhile, by BiOX and 1.0g diatomite
In the composite photo-catalyst of both compositions, during 30min dark reaction, by it was found that No. 4 sample (BiOI/ diatoms
Soil) stronger absorption property is shown to rhodamine B, the absorption property of No. 7 samples (BiOCl/ diatomite) is most weak, this possible energy
Relevant with the specific surface area difference for preparing sample, after light source is opened, rhodamine B is dropped rapidly under photocatalysis
Solution, can significantly find out, although the suction-operated in the dark reaction of No. 1 sample (BiOBr/ diatomite) is not most strong from Fig. 4
, but rhodamine B generation photocatalysis Decomposition can be made most fast, show highest photocatalytic activity.This explanation, in Multi-phase light
In catalytic reaction process, reaction rate additionally depends on the pass for constituting this catalyst except having outside the Pass with specific surface area of catalyst
Key active component.Have been reported that and show, BiOCl energy gap is larger, be unfavorable for by the excited by visible light of long wavelength, although BiOI
With energy gap minimum in three, but be due to its valence band location it is higher so that formed Hole oxidation ability subtracted
It is weak, and BiOBr energy gaps are relatively small while the valence band hole of more strong oxidizing property can be formed, institute's catalytic activity is also stronger.
Fig. 5 is prepared No. 1, No. 4, the degradation results of No. 7 samples lower rhodamine B under LED purple light light irradiations.From figure
In find out, under violet exposure, the photocatalytic activities of different samples relative to there is different degrees of raising under blue light illumination, and
Be still No. 1 sample (BiOBr/ diatomite) photocatalysis effect preferably, this mainly by wavelength shorter violet exposure when,
The electron hole pair quantity of generation is more rich, and the active specy for participating in multiphase photocatalysis reaction is more, so more efficient.
Fig. 6 is prepared No. 1, No. 2, degradation results of No. 3 samples under LED blue light light irradiations to rhodamine B.
After BiOBr is by the composite diatomite with different proportion, photocatalytic activity is different, wherein No. 1 sample (1.0g diatomite/
BiOBr rhodamine B) can be made to occur most fast decomposition under photocatalysis, 1.5g diatomite/BiOBr takes second place, 2.0g diatoms
Soil/BiOBr is worst, but also shows higher photocatalytic activity.This be probably because with preparation process with diatomite
Mass ratio increase, BiOBr relative amounts have reduced, the active component in the composite photo-catalyst of unit mass under
Drop, specific surface area of catalyst can also be changed, and specific surface area of catalyst influences catalytic efficiency, composite catalyzing to a certain extent
The catalytic performance of agent has much relations with absorption with light-catalysed synergy.From the results of view, identical catalyst amountses,
The active component of No. 1 sample should be most, and diatomite is relatively minimal, but the dark reaction result of 30min minutes shows the sample
The suction-operated of product is best, it can be seen that, although diatomite is multi-pore channel material, the complex light that BiOX is constituted with diatomite
What catalysis material played a major role to rhdamine B absorption is BiOX
Fig. 7 is prepared No. 1, No. 2, degradation results of No. 3 samples under LED purple light light irradiations to rhodamine B.By scheming
Table understands that under the conditions of purple light, No. 1, No. 2, No. 3 samples have a certain degree of carry to the degradation efficiency of rhodamine B compared with blue light
Height, this is probably because short wavelength excites the lower more active materials of generation relevant, in addition, it was similarly observed that No. 1 sample tool
Have highest photocatalytic activity, next to that No. 2 and No. 3 samples, this is similar to the result obtained under blue light, it also hold that be with
With diatomaceous dosage increase in preparation process, the reason for photocatalytic activity component of unit mass is reduced is relevant, then
The deduction, analysis result are further confirmed with XRD analysis as shown in figure 8, Fig. 8 respectively show No. 1 sample and No. 3 sample differences herein
The sample XRD spectrum of diatomite amount, by it was found that being characterized as characteristic diffraction peak quartzy in diatomite in No. 1 sample than 3
Intensity in number sample has weakened, and characteristic peaks of the BiOBr in [101] and [110] two crystal faces has strengthened, and this is from structural table
The angle levied further demonstrate that than No. 2 samples of diatomite content in No. 3 samples are high, and the BiOBr in No. 1 sample is than 3 in turn
Number sample content is higher.
The preparation method of the present invention compared with prior art, has the advantage that：
1st, the agent of BiOX/ diatomite composite photocatalytics can successfully be prepared by Hydrolyze method, and this method is simple and easy to apply, it is easy to raw
Production, prepared sample has the irregular hierarchy of the sheet loaded on diatomite rotary strainer.
2nd, compared to BiOI/ diatomite, BiOCl/ diatomite, BiOBr/ diatomite has stronger visible light photocatalysis
Energy.
3rd, under the conditions of LED purple lights and blue light illumination test result indicates that each composite catalyst is imitated to catalysis under the conditions of purple light
Fruit increases compared with blue light.
4th, it is separately added into preparation process in 1.0g, 1.5g, the sample prepared by 2.0g diatomite, by 1.0g diatomite
The BiOX/ diatomite of preparation is best to the catalytic effect of rhodamine B, absorption of the BiOX to target contaminant in composite photo-catalyst
Play a major role.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
Any modifications, equivalent substitutions and improvements made within refreshing and principle etc., should be included in the scope of the protection.
Claims (10)
1. a kind of preparation method of BiOX/diatomite composite photocatalytic agent, it is characterised in that the BiOX/diatom
The preparation method of native composite photo-catalyst comprises the following steps：
Step one, according to parts by weight KX or NaX：Water：The ﹣ 500 of smart diatomite=20：2000 ﹣ 10000：100 ﹣ 4000 ratio
After mixing, 5 ﹣ 30min are stirred, slurry is made；X is Cl, Br, I；
Step 2, according to parts by weight Bi (NO3)3·5H2O：KX or NaX=500 ﹣ 1500:20 ﹣ 400, weigh Bi (NO3)3·
5H2O is added in above-mentioned slurrying liquid, 5 ﹣ 30min of quick stirring, and reaction, synthesis BiOX/composite diatomite grain is hydrolyzed
Son；
Step 3, the BiOX of above-mentioned synthesis/composite diatomite particle slurry is filtered, according to the smart diatom of weight fraction
Soil：The ﹣ 4000 of water=100：1000 ﹣ 40000 ratio adds water and carries out filtration washing；
Step 4, the filter cake after above-mentioned filtration washing is put into drying box and is dried, and drying temperature is 60 DEG C of 300 DEG C of ﹣, extremely
Moisture content stops drying when being 0% ﹣ 7%, and pack after dried material scattering is obtained into finished product.
2. the preparation method of BiOX as claimed in claim 1/diatomite composite photocatalytic agent, it is characterised in that described
BiOX/diatomite is BiOCl/ diatomite, BiOI/ diatomite, BiOBr/ diatomite.
3. the preparation method of BiOX as claimed in claim 2/diatomite composite photocatalytic agent, it is characterised in that described
The preparation method of BiOX/diatomite composite photocatalytic agent comprises the following steps：
It is prepared by the BiOCl/ diatomite:Precise 2.8mmol KCl or NaCl, is completely dissolved in 80mL deionized water
In, then a certain proportion of diatomite is added thereto, 10min, then precise 2.8mmol Bi (NO is stirred3)3·5H2O's
Add stirring mixing 30min in above-mentioned suspension；Resulting solution is subjected to vacuum filtration washing, the thing most after being dried at 95 DEG C
Material moisture obtains finished product less than 7%.
4. the preparation method of BiOX as claimed in claim 2/diatomite composite photocatalytic agent, it is characterised in that described
The preparation method of BiOX/diatomite composite photocatalytic agent comprises the following steps：
It is prepared by the BiOBr/ diatomite:Precise 2.8mmol KBr or NaBr, is completely dissolved in 80mL deionized water
In, then a certain proportion of diatomite is added thereto, 10min, then precise 2.8mmol Bi (NO is stirred3)3·5H2O's
Add stirring mixing 30min in above-mentioned suspension；Resulting solution is subjected to vacuum filtration washing, the thing most after being dried at 95 DEG C
Material moisture obtains finished product less than 7%.
5. the preparation method of BiOX as claimed in claim 2/diatomite composite photocatalytic agent, it is characterised in that described
The preparation method of BiOX/diatomite composite photocatalytic agent comprises the following steps：
It is prepared by the BiOI/ diatomite:Precise 2.8mmol KI or NaI, is completely dissolved in 80mL deionized water,
Then a certain proportion of diatomite is added thereto, stirs 10min, then precise 2.8mmol Bi (NO3)3·5H2O's adds
Enter stirring mixing 30min in above-mentioned suspension；Resulting solution is subjected to vacuum filtration washing, the material most after being dried at 95 DEG C
Moisture obtains finished product less than 7%.
6. it is prepared by a kind of preparation method of the BiOX as described in Claims 1 to 5 any one-diatomite composite photocatalytic agent
BiOX-diatomite composite photocatalytic agent.
7. a kind of ecologic coating building materials prepared as BiOX described in claim 6/diatomite composite photocatalytic agent.
8. a kind of material for air purification prepared as BiOX described in claim 6/diatomite composite photocatalytic agent.
9. a kind of asphalt modifier prepared as BiOX described in claim 6/diatomite composite photocatalytic agent.
10. a kind of composite prepared as BiOX described in claim 6/diatomite composite photocatalytic agent.
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| CN110227503A (en) * | 2019-06-11 | 2019-09-13 | 杭州电子科技大学 | A kind of method of one step of room temperature preparation halogenation oxygen bismuth nanometer sheet |
| CN110422905A (en) * | 2019-09-05 | 2019-11-08 | 太原师范学院 | A method of BiOCl catalytic eliminating bisphenol-A is loaded using coke |
| CN110422905B (en) * | 2019-09-05 | 2021-07-23 | 太原师范学院 | Method for removing bisphenol A by coke-loaded BiOCl catalysis |
| CN110743578A (en) * | 2019-11-21 | 2020-02-04 | 中国地质大学（北京） | Tourmaline-loaded BiOI photocatalyst and preparation method thereof |
| CN113333005A (en) * | 2021-05-13 | 2021-09-03 | 重庆南科环工环保科技有限公司 | Preparation and application of supported bismuth oxyhalide catalyst |
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| CN114797909B (en) * | 2022-05-16 | 2024-01-26 | 湖南城市学院 | Photocatalytic purification material based on rock wool fibers |
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