CN107866238A - A kind of BiOCl TiO2/Sb2S3The preparation method of composite photo-catalyst - Google Patents
A kind of BiOCl TiO2/Sb2S3The preparation method of composite photo-catalyst Download PDFInfo
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 85
- 239000002131 composite material Substances 0.000 title claims abstract description 42
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- BWOROQSFKKODDR-UHFFFAOYSA-N oxobismuth;hydrochloride Chemical compound Cl.[Bi]=O BWOROQSFKKODDR-UHFFFAOYSA-N 0.000 title abstract 2
- 229910052959 stibnite Inorganic materials 0.000 claims abstract description 57
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 27
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 15
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910000410 antimony oxide Inorganic materials 0.000 claims abstract description 10
- VTRUBDSFZJNXHI-UHFFFAOYSA-N oxoantimony Chemical compound [Sb]=O VTRUBDSFZJNXHI-UHFFFAOYSA-N 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 6
- KKSAZXGYGLKVSV-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO KKSAZXGYGLKVSV-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 44
- 239000000084 colloidal system Substances 0.000 claims description 34
- 238000003756 stirring Methods 0.000 claims description 31
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Inorganic materials [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 26
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 22
- 229910017604 nitric acid Inorganic materials 0.000 claims description 22
- 239000000843 powder Substances 0.000 claims description 20
- 238000004140 cleaning Methods 0.000 claims description 16
- 238000001035 drying Methods 0.000 claims description 16
- 239000011259 mixed solution Substances 0.000 claims description 15
- 239000000725 suspension Substances 0.000 claims description 15
- 230000008859 change Effects 0.000 claims description 13
- 238000001556 precipitation Methods 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 12
- 235000019441 ethanol Nutrition 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 8
- 238000005119 centrifugation Methods 0.000 claims description 7
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 claims description 6
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 6
- 230000002045 lasting effect Effects 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 239000003643 water by type Substances 0.000 claims description 5
- 238000013019 agitation Methods 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 4
- 238000000502 dialysis Methods 0.000 claims description 3
- 125000005909 ethyl alcohol group Chemical group 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- 239000007787 solid Substances 0.000 claims description 3
- 239000003292 glue Substances 0.000 claims 1
- 229910052797 bismuth Inorganic materials 0.000 abstract description 6
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 abstract description 6
- 238000005516 engineering process Methods 0.000 abstract description 5
- 239000002245 particle Substances 0.000 abstract description 5
- 230000001699 photocatalysis Effects 0.000 abstract description 3
- 239000003638 chemical reducing agent Substances 0.000 abstract description 2
- 230000001276 controlling effect Effects 0.000 abstract description 2
- 238000000280 densification Methods 0.000 abstract description 2
- 238000009826 distribution Methods 0.000 abstract description 2
- 238000011065 in-situ storage Methods 0.000 abstract description 2
- 230000004048 modification Effects 0.000 abstract description 2
- 238000012986 modification Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 230000001105 regulatory effect Effects 0.000 abstract description 2
- RWSOTUBLDIXVET-UHFFFAOYSA-N Dihydrogen sulfide Chemical compound S RWSOTUBLDIXVET-UHFFFAOYSA-N 0.000 abstract 1
- 238000000354 decomposition reaction Methods 0.000 abstract 1
- 239000003054 catalyst Substances 0.000 description 17
- 239000000047 product Substances 0.000 description 12
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 9
- 229940012189 methyl orange Drugs 0.000 description 9
- 230000000694 effects Effects 0.000 description 8
- 230000032683 aging Effects 0.000 description 6
- 239000005543 nano-size silicon particle Substances 0.000 description 6
- 238000006555 catalytic reaction Methods 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 239000002086 nanomaterial Substances 0.000 description 4
- 229910052814 silicon oxide Inorganic materials 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 239000002957 persistent organic pollutant Substances 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 2
- 235000002639 sodium chloride Nutrition 0.000 description 2
- 238000001694 spray drying Methods 0.000 description 2
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000010306 acid treatment Methods 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- TXKAQZRUJUNDHI-UHFFFAOYSA-K bismuth tribromide Chemical compound Br[Bi](Br)Br TXKAQZRUJUNDHI-UHFFFAOYSA-K 0.000 description 1
- 229910052980 cadmium sulfide Inorganic materials 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000010442 halite Substances 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 231100001231 less toxic Toxicity 0.000 description 1
- 238000010907 mechanical stirring Methods 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- -1 monothio salicylic acids Chemical class 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- 230000003612 virological effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 239000010457 zeolite 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
- B01J27/135—Halogens; Compounds thereof with titanium, zirconium, hafnium, germanium, tin or lead
-
- B01J35/39—
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/08—Heat treatment
- B01J37/10—Heat treatment in the presence of water, e.g. steam
-
- 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
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Abstract
The invention discloses a kind of BiOCl TiO2/Sb2S3Composite photo-catalyst preparation method, with butanol titanium, absolute ethyl alcohol, antimony oxide, hydrochloric acid, H2S、BiCl3And TiO2/Sb2S3For primary raw material, combined by solvent-thermal method and hydro-thermal method, in-situ preparation nanometer bismuth particle, nanometer bismuth even particle distribution, with reference to densification, makes bismoclite composite photo-catalyst have higher stability, by conditions such as regulating and controlling temperature, reducing agent dosages, the controllable of bismuth modification amount is realized；Preparation technology of the present invention is novel, both with good Visible Light Induced Photocatalytic effect, can reduce cost again, reduce pollution, have preferable application prospect and economic benefit in terms of organic pollution decomposition.
Description
Technical field
The present invention relates to a kind of BiOCl- TiO2/Sb2S3Composite photo-catalyst and preparation method thereof, belong to catalyst technology
Field.
Background technology
Photocatalysis technology refers to the energy that catalyst is converted light energy under illumination condition required for chemical reaction, and then
Catalytic action is produced, is a kind of novel high-efficient energy-saving environment-friendly technology.Photocatalytic degradation is to be produced using light radiation in reaction system
The bold and vigorous free radical of life, organic pollution is decomposed by carrying out the processes such as adduction, substitution and electronics transfer with organic pollution
For nontoxic or less toxic inorganic matter.Photocatalytic degradation is because it has reaction condition gentle, non-secondary pollution, directly utilizes sunshine
The advantages such as energy turn into the study hotspot for administering organic pollution；Problems of the prior art are, the broad stopband light such as traditional
Catalyst can only often absorb the ultraviolet light that small percentage is accounted in sunshine, and the efficiency of light energy utilization is low and the narrow taboo such as cadmium sulfide
Band photochemical catalyst is generally unstable, easily decomposites harmful substance.Therefore, finding new low energy gap photochemical catalyst has important skill
Art and application value.
The content of the invention
It is an object of the invention to provide a kind of BiOCl- TiO2/Sb2S3Composite photo-catalyst and preparation method thereof, catalysis
The stability of agent is high, has higher degradation rate to organic pollution.
A kind of BiOCl- TiO2/Sb2S3The preparation method of composite photo-catalyst, this method comprise the following steps：
Step 1, at room temperature, by 9mol BiCl3With 3mol TiO2/Sb2S3It is 1mol that composite photocatalyst colloid, which is dissolved in concentration,
L-1Dilute nitric acid solution in, then with concentration be 4molL-1NaOH solution the pH value of mixed solution is adjusted to 14, stirring is old
Change 2h, the suspension containing precipitation is transferred in reactor in 220 DEG C of heating 24h of baking oven.Precipitated made from hydro-thermal method from
After heart cleaning, drying, product as yellow powder Bi is obtained2O3- TiO2/Sb2S3；
Step 2, by mass fraction be 38% concentrated hydrochloric acid dilute to obtain 0.2molL-1Diluted hydrochloric acid aqueous solution, take above-mentioned yellow
Powder, magnetic agitation 1h in the dilute hydrochloric acid solution being put into, to the scheduled time after the drying of mixed solution eccentric cleaning, be finally
Obtain described BiOCl- TiO2/Sb2S3Composite photo-catalyst.
Described TiO2/Sb2S3Composite photocatalyst colloid preparation method is as follows：
Step 1, by 2ml concentration be 38% concentrated nitric acid slowly prolong wall add 100ml deionized waters in, be stirred and heated to
10 DEG C of obtained salpeter solutions；
Step 2,18g butanol titaniums are rapidly joined in 18ml absolute ethyl alcohols and stirred, the ethanol solution of butanol titanium is being stirred
Mix down and be slowly dropped in foregoing salpeter solution, drop finishes, and continues to stir, it is standby to obtain light blue transparent colloid A；
Step 3,1.5g antimony oxides are dissolved in the hydrochloric acid of 15ml concentration 36%, lasting stirring, and are led to 60ml/min flow
Enter H2S gases, until antimony oxide powder is all transformed into flocculent deposit, 50 DEG C are heated to, stirring, obtains pale yellow transparent colloid
B is standby；
Step 4, by above-mentioned A colloidal sols and B colloidal sols by volume 3:1 ratio mixing, persistently stirs 12h, by mixture by following
The dialysis of ring dialyzer obtains TiO to PH=62/Sb2S3Composite colloid, its solid content are 5Wt%.
Beneficial effect：Composite photocatalyst BiOCl- TiO prepared by the present invention2/Sb2S3Pass through solvent-thermal method and hydro-thermal
Method combines, and in-situ preparation nanometer bismuth particle, nanometer bismuth even particle distribution, with reference to densification, makes bismoclite composite photo-catalyst
With higher stability, by conditions such as regulating and controlling temperature, reducing agent dosages, the controllable of bismuth modification amount is realized；Due to catalysis
Agent is this lamellar structure compound of viral in Austria, and its energy gap is about 2.08eV, can effectively absorb visible ray, built-in electricity
Field and layer structure are all advantageous to photo-generate electron-hole to efficiently separating, so as to improve photocatalysis performance.Bismoclite is
Bi2O2 2+And Cl2-The layer structure of composition is alternately arranged, and band structure matches so as to quick with dyestuff with many dyestuffs
Change acts on, can be with more efficient decomposing organic pollutant.
Embodiment
Embodiment 1
A kind of BiOCl- TiO2/Sb2S3The preparation method of composite photo-catalyst, this method comprise the following steps：
Step 1, at room temperature, by 9mol BiCl3With 3mol TiO2/Sb2S3It is 1mol that composite photocatalyst colloid, which is dissolved in concentration,
L-1Dilute nitric acid solution in, then with concentration be 4molL-1NaOH solution the pH value of mixed solution is adjusted to 14, stirring is old
Change 2h, the suspension containing precipitation is transferred in reactor in 220 DEG C of heating 24h of baking oven.Precipitated made from hydro-thermal method from
After heart cleaning, drying, product as yellow powder Bi is obtained2O3- TiO2/Sb2S3；
Step 2, by mass fraction be 38% concentrated hydrochloric acid dilute to obtain 0.2molL-1Diluted hydrochloric acid aqueous solution, take above-mentioned yellow
Powder, magnetic agitation 1h in the dilute hydrochloric acid solution being put into, to the scheduled time after the drying of mixed solution eccentric cleaning, be finally
Obtain described BiOCl- TiO2/Sb2S3Composite photo-catalyst.
Described TiO2/Sb2S3Composite photocatalyst colloid preparation method is as follows：
Step 1, by 2ml concentration be 38% concentrated nitric acid slowly prolong wall add 100ml deionized waters in, be stirred and heated to
10 DEG C of obtained salpeter solutions；
Step 2,18g butanol titaniums are rapidly joined in 18ml absolute ethyl alcohols and stirred, the ethanol solution of butanol titanium is being stirred
Mix down and be slowly dropped in foregoing salpeter solution, drop finishes, and continues to stir, it is standby to obtain light blue transparent colloid A；
Step 3,1.5g antimony oxides are dissolved in the hydrochloric acid of 15ml concentration 36%, lasting stirring, and are led to 60ml/min flow
Enter H2S gases, until antimony oxide powder is all transformed into flocculent deposit, 50 DEG C are heated to, stirring, obtains pale yellow transparent colloid
B is standby；
Step 4, by above-mentioned A colloidal sols and B colloidal sols by volume 3:1 ratio mixing, persistently stirs 12h, by mixture by following
The dialysis of ring dialyzer obtains TiO to PH=62/Sb2S3Composite colloid, its solid content are 5Wt%.
Embodiment 2
Step 1, at room temperature, by 9mol BiCl3With 1mol TiO2/Sb2S3It is 1mol that composite photocatalyst colloid, which is dissolved in concentration,
L-1Dilute nitric acid solution in, then with concentration be 4molL-1NaOH solution the pH value of mixed solution is adjusted to 14, stirring is old
Change 2h, the suspension containing precipitation is transferred in reactor in 220 DEG C of heating 24h of baking oven.Precipitated made from hydro-thermal method from
After heart cleaning, drying, product as yellow powder Bi is obtained2O3- TiO2/Sb2S3；
Remaining step is the same as embodiment 1.
Embodiment 3
Step 1, at room temperature, by 9mol BiCl3With 0.5mol TiO2/Sb2S3Composite photocatalyst colloid is dissolved in concentration
1mol·L-1Dilute nitric acid solution in, then with concentration be 4molL-1NaOH solution the pH value of mixed solution is adjusted to 14,
Stirring ageing 2h, the suspension containing precipitation is transferred in reactor in 220 DEG C of heating 24h of baking oven.Made from hydro-thermal method
After pelleting centrifugation cleaning, drying, product as yellow powder Bi is obtained2O3- TiO2/Sb2S3；
Remaining step is the same as embodiment 1.
Embodiment 4
Step 1, at room temperature, by 9mol BiCl3With 0.1mol TiO2/Sb2S3Composite photocatalyst colloid is dissolved in concentration
1mol·L-1Dilute nitric acid solution in, then with concentration be 4molL-1NaOH solution the pH value of mixed solution is adjusted to 14,
Stirring ageing 2h, the suspension containing precipitation is transferred in reactor in 220 DEG C of heating 24h of baking oven.Made from hydro-thermal method
After pelleting centrifugation cleaning, drying, product as yellow powder Bi is obtained2O3- TiO2/Sb2S3；
Remaining step is the same as embodiment 1.
Embodiment 5
Step 1, at room temperature, by 6mol BiCl3With 3mol TiO2/Sb2S3It is 1mol that composite photocatalyst colloid, which is dissolved in concentration,
L-1Dilute nitric acid solution in, then with concentration be 4molL-1NaOH solution the pH value of mixed solution is adjusted to 14, stirring is old
Change 2h, the suspension containing precipitation is transferred in reactor in 220 DEG C of heating 24h of baking oven.Precipitated made from hydro-thermal method from
After heart cleaning, drying, product as yellow powder Bi is obtained2O3- TiO2/Sb2S3；
Remaining step is the same as embodiment 1.
Embodiment 6
Step 1, at room temperature, by 3mol BiCl3With 3mol TiO2/Sb2S3It is 1mol that composite photocatalyst colloid, which is dissolved in concentration,
L-1Dilute nitric acid solution in, then with concentration be 4molL-1NaOH solution the pH value of mixed solution is adjusted to 14, stirring is old
Change 2h, the suspension containing precipitation is transferred in reactor in 220 DEG C of heating 24h of baking oven.Precipitated made from hydro-thermal method from
After heart cleaning, drying, product as yellow powder Bi is obtained2O3- TiO2/Sb2S3；
Remaining step is the same as embodiment 1.
Embodiment 7
Step 1, at room temperature, by 1mol BiCl3With 3mol TiO2/Sb2S3It is 1mol that composite photocatalyst colloid, which is dissolved in concentration,
L-1Dilute nitric acid solution in, then with concentration be 4molL-1NaOH solution the pH value of mixed solution is adjusted to 14, stirring is old
Change 2h, the suspension containing precipitation is transferred in reactor in 220 DEG C of heating 24h of baking oven.Precipitated made from hydro-thermal method from
After heart cleaning, drying, product as yellow powder Bi is obtained2O3- TiO2/Sb2S3；
Remaining step is the same as embodiment 1.
Embodiment 8
Step 1, at room temperature, by 0.1mol BiCl3With 3mol TiO2/Sb2S3Composite photocatalyst colloid is dissolved in concentration
1mol·L-1Dilute nitric acid solution in, then with concentration be 4molL-1NaOH solution the pH value of mixed solution is adjusted to 14,
Stirring ageing 2h, the suspension containing precipitation is transferred in reactor in 220 DEG C of heating 24h of baking oven.Made from hydro-thermal method
After pelleting centrifugation cleaning, drying, product as yellow powder Bi is obtained2O3- TiO2/Sb2S3；
Remaining step is the same as embodiment 1.
Embodiment 9
Step 1, at room temperature, by 9mol BiCl3With 18mol TiO2/Sb2S3Composite photocatalyst colloid is dissolved in concentration
1mol·L-1Dilute nitric acid solution in, then with concentration be 4molL-1NaOH solution the pH value of mixed solution is adjusted to 14,
Stirring ageing 2h, the suspension containing precipitation is transferred in reactor in 220 DEG C of heating 24h of baking oven.Made from hydro-thermal method
After pelleting centrifugation cleaning, drying, product as yellow powder Bi is obtained2O3- TiO2/Sb2S3；
Remaining step is the same as embodiment 1.
Embodiment 10
Step 1, at room temperature, by 1.5mol BiCl3With 3mol TiO2/Sb2S3Composite photocatalyst colloid is dissolved in concentration
1mol·L-1Dilute nitric acid solution in, then with concentration be 4molL-1NaOH solution the pH value of mixed solution is adjusted to 14,
Stirring ageing 2h, the suspension containing precipitation is transferred in reactor in 220 DEG C of heating 24h of baking oven.Made from hydro-thermal method
After pelleting centrifugation cleaning, drying, product as yellow powder Bi is obtained2O3- TiO2/Sb2S3；
Remaining step is the same as embodiment 1.
Embodiment 11
Step 1, at room temperature, by 9mol BiCl3With 3mol TiO2/Sb2S3It is 1mol that composite photocatalyst colloid, which is dissolved in concentration,
L-1Dilute nitric acid solution in, add 50g Si-Na-LTA nano materials, then with concentration be 4molL-1NaOH solution will be mixed
The pH value for closing solution is adjusted to 14, stirring ageing 2h, the suspension containing precipitation is transferred in reactor in 220 DEG C of baking oven plus
Hot 24h.After pelleting centrifugation cleaning, drying made from hydro-thermal method, product as yellow powder Bi is obtained2O3- TiO2/Sb2S3；
Remaining step is the same as embodiment 1.
Described Si-Na-LTA preparation method of nano material is as follows：
Step 1, by 200g particle diameters be 30nm nano silicon oxide put into the aqueous solution, with 3000rpm stirring at 20 DEG C
After speed mechanical stirring 15min, the aqueous dispersions of nano silicon oxide are obtained；Add into the aqueous dispersions of obtained nano silicon oxide
Enter 15g modifer L monothio salicylic acids, at a temperature of 80 DEG C, stirred under 3000rpm rotating speed, obtain modified nano silicon oxide
Suspension；The suspension of gained is spray-dried, the rotating speed of spray drying is 16000rpm, and the temperature of spray drying is
100 DEG C, obtain organic acidifying nano-silicon；
Step 2, organic acidifying nano-silicon and 100gNa-LTA zeolite powders by 300g, activate at 500 DEG C, are distributed to
In 10L ethanol, the mixture of compound and ethanol is transferred in the three-necked flask equipped with 2L ammoniacal liquor after ball milling, by temperature
60 DEG C are increased to, 1h is heated, the 1L then added TEOS, continues stirring 6, the slurries filtration that will be obtained, 3 are washed with ethanol
It is secondary, finally obtain Si-Na-LTA nano materials.
Reference examples 1
It is with the difference of embodiment 1：In step 1 prepared by photochemical catalyst, by 9mol BiBr3With 3mol TiO2/Sb2S3It is multiple
It is 1molL that closing light catalysis colloid, which is dissolved in concentration,-1Dilute nitric acid solution in, remaining step is identical with embodiment 1.
Reference examples 2
It is with the difference of embodiment 1：In step 1 prepared by photochemical catalyst, by 3mol BiBr3With 9mol TiO2/Sb2S3It is multiple
It is 1molL that closing light catalysis colloid, which is dissolved in concentration,-1Dilute nitric acid solution in, remaining step is identical with embodiment 1.
Reference examples 3
It is with the difference of embodiment 1：In step 1 prepared by photochemical catalyst, by 3mol TiO2/Sb2S3Composite photocatalyst colloid
It is 1molL to be dissolved in concentration-1Dilute nitric acid solution in, remaining step is identical with embodiment 1.
Reference examples 4
It is with the difference of embodiment 1：In step 1 prepared by photochemical catalyst, by 9mol BiCl3With 3mol TiO2It is dissolved in concentration
For 1molL-1Dilute nitric acid solution in, remaining step is identical with embodiment 1.
Reference examples 5
It is with the difference of embodiment 1：TiO2/Sb2S3It is 16% by 2ml concentration in step 1 prepared by composite photocatalyst colloid
Concentrated nitric acid slowly prolongs wall and added in 100ml deionized waters, and remaining step is identical with embodiment 1.
Reference examples 6
It is with the difference of embodiment 1：TiO2/Sb2S3It is 8% by 2ml concentration in step 1 prepared by composite photocatalyst colloid
Concentrated nitric acid slowly prolongs wall and added in 100ml deionized waters, and remaining step is identical with embodiment 1.
Reference examples 7
It is with the difference of embodiment 1：TiO2/Sb2S3In step 3 prepared by composite photocatalyst colloid, 0.5g antimony oxides are dissolved
Lasting to stir in the hydrochloric acid of 15ml concentration 36%, remaining step is identical with embodiment 1.
Reference examples 8
It is with the difference of embodiment 1：TiO2/Sb2S3In step 3 prepared by composite photocatalyst colloid, 3.0g antimony oxides are dissolved
Lasting to stir in the hydrochloric acid of 15ml concentration 36%, remaining step is identical with embodiment 1.
Reference examples 9
It is with the difference of embodiment 1：：TiO2/Sb2S3In step 4 prepared by composite photocatalyst colloid, by above-mentioned A colloidal sols and B
Colloidal sol by volume 1:3 ratio mixing, persistently stirs 12h, remaining step is identical with embodiment 1.
Reference examples 10
It is with the difference of embodiment 1：：TiO2/Sb2S3In step 4 prepared by composite photocatalyst colloid, by above-mentioned A colloidal sols and B
Colloidal sol by volume 1:1 ratio mixing, persistently stirs 12h, remaining step is identical with embodiment 1.
Weigh the BiOCl- TiO that 0.5g embodiments and reference examples obtain2/Sb2S3Composite photo-catalyst, uniformly it is mixed in 800ml
Concentration is the Halite water system of 20.0mg/L methyl oranges（15%NaCl）, it is placed in the reactor with magnetic agitation, controls water-bath
Temperature is 30 DEG C, absorption 1 hour of turning off the light.After adsorption equilibrium, under the irradiation of dim light light source（4W ultra-violet back light lamp）, it is small to react 3
When after be sampled, centrifuge, take supernatant liquor, using TU-19 series ultraviolet visible spectrophotometers, determine methyl orange
Absorbance simultaneously obtains its change in concentration, obtains methyl orange organic pollutant removal rate.
As a result it is as shown in the table.
| Photochemical catalyst | Methyl orange removal/% |
| Embodiment 1 | 80.1 |
| Embodiment 2 | 75.3 |
| Embodiment 3 | 70.4 |
| Embodiment 4 | 64.6 |
| Embodiment 5 | 58.2 |
| Embodiment 6 | 52.7 |
| Embodiment 7 | 48.3 |
| Embodiment 8 | 56.1 |
| Embodiment 9 | 63.6 |
| Embodiment 10 | 70.8 |
| Embodiment 11 | 88.4 |
| Reference examples 1 | 41.9 |
| Reference examples 2 | 36.6 |
| Reference examples 3 | 57.1 |
| Reference examples 4 | 27.9 |
| Reference examples 5 | 44.4 |
| Reference examples 6 | 28.7 |
| Reference examples 7 | 23.1 |
| Reference examples 8 | 17.3 |
| Reference examples 9 | 19.1 |
| Reference examples 10 | 27.8 |
Test result indicates that photochemical catalyst has good removal effect to methyl orange organic pollution, it is certain in reaction condition
When, methyl orange clearance is higher, and catalytic performance is better, otherwise poorer；In BiCl3And TiO2/Sb2S3Mol ratio is 3:When 1, its
He fixes at dispensing, and removal effect is best, is with the difference of embodiment 1, and embodiment 2 to embodiment 10 changes photochemical catalyst respectively
Primary raw material BiCl3And TiO2/Sb2S3Dosage and proportioning, have different influences to the decomposability of photochemical catalyst, be worth note
Meaning is that embodiment 11 adds Si-Na-LTA nano materials, and methyl orange resolution ratio significantly improves, and illustrates Si-Na-LTA nanometers
Material has more preferable optimization function to the structure-activity of catalysis material；Reference examples 1 to reference examples 4 using bismuth bromide and change
Catalyst proportion, other steps are identical, cause the activity of catalyst to change, and methyl orange resolution ratio substantially reduces；It is right
5 to reference examples 6 as usual, reduce the concentration of salpeter solution, cause material acid treatment degree to reduce, degradation effect is still bad；It is right
7 to reference examples 8 as usual, change TiO2/Sb2S3The usage amount of antimony oxide is reduced, causes the structure-activity of catalyst colloid to become
Change, positive effect is deteriorated, reference examples 9 to reference examples 10, changes A colloidal sols and B sol volumes ratio, and methyl orange resolution ratio is still not
Height, only in volume ratio 3:When 1, effect is best；Therefore the photochemical catalyst prepared using the present invention is to methyl orange organic pollution
Removal there is excellent effect.
Claims (2)
- A kind of 1. BiOCl- TiO2/Sb2S3The preparation method of composite photo-catalyst, it is characterised in that this method includes following step Suddenly：Step 1, at room temperature, by 9mol BiCl3With 3mol TiO2/Sb2S3It is 1mol that composite photocatalyst colloid, which is dissolved in concentration, L-1Dilute nitric acid solution in, then with concentration be 4molL-1NaOH solution the pH value of mixed solution is adjusted to 14, stirring is old Change 2h, the suspension containing precipitation is transferred in reactor in 220 DEG C of heating 24h of baking oven；After pelleting centrifugation cleaning, drying made from hydro-thermal method, product as yellow powder Bi is obtained2O3- TiO2/Sb2S3；Step 2, by mass fraction be 38% concentrated hydrochloric acid dilute to obtain 0.2molL-1Diluted hydrochloric acid aqueous solution, take above-mentioned yellow Powder, magnetic agitation 1h in the dilute hydrochloric acid solution being put into, to the scheduled time after the drying of mixed solution eccentric cleaning, be finally Obtain described BiOCl- TiO2/Sb2S3Composite photo-catalyst.
- A kind of 2. BiOCl- TiO described in claim 12/Sb2S3The preparation method of composite photo-catalyst, it is characterised in that it is described,Described TiO2/Sb2S3Composite photocatalyst colloid preparation method is as follows：Step 1, by 2ml concentration be 38% concentrated nitric acid slowly prolong wall add 100ml deionized waters in, be stirred and heated to 10 DEG C of obtained salpeter solutions；Step 2,18g butanol titaniums are rapidly joined in 18ml absolute ethyl alcohols and stirred, the ethanol solution of butanol titanium is being stirred Mix down and be slowly dropped in foregoing salpeter solution, drop finishes, and continues to stir, it is standby to obtain light blue transparent colloid A；Step, 3,1.5g antimony oxides are dissolved in the hydrochloric acid of 15ml concentration 36%, lasting stirring, and with 60ml/min flow It is passed through H2S gases, until antimony oxide powder is all transformed into flocculent deposit, 50 DEG C are heated to, stirring, obtains pale yellow transparent glue Body B is standby；Step 4, by above-mentioned A colloidal sols and B colloidal sols by volume 3:1 ratio mixing, persistently stirs 12h, by mixture by following The dialysis of ring dialyzer obtains TiO to PH=62/Sb2S3Composite colloid, its solid content are 5Wt%.
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