CN109331845A - A kind of synthesis and application of high dispersive BiOCl/ diatomite photochemical catalyst - Google Patents
A kind of synthesis and application of high dispersive BiOCl/ diatomite photochemical catalyst Download PDFInfo
- Publication number
- CN109331845A CN109331845A CN201811499453.8A CN201811499453A CN109331845A CN 109331845 A CN109331845 A CN 109331845A CN 201811499453 A CN201811499453 A CN 201811499453A CN 109331845 A CN109331845 A CN 109331845A
- Authority
- CN
- China
- Prior art keywords
- diatomite
- biocl
- photochemical catalyst
- solution
- high dispersive
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 86
- BWOROQSFKKODDR-UHFFFAOYSA-N oxobismuth;hydrochloride Chemical compound Cl.[Bi]=O BWOROQSFKKODDR-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 239000003054 catalyst Substances 0.000 title claims abstract description 39
- 230000015572 biosynthetic process Effects 0.000 title abstract description 10
- 238000003786 synthesis reaction Methods 0.000 title abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 40
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 39
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims abstract description 26
- MYSWGUAQZAJSOK-UHFFFAOYSA-N ciprofloxacin Chemical compound C12=CC(N3CCNCC3)=C(F)C=C2C(=O)C(C(=O)O)=CN1C1CC1 MYSWGUAQZAJSOK-UHFFFAOYSA-N 0.000 claims abstract description 26
- 230000001699 photocatalysis Effects 0.000 claims abstract description 17
- 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 claims abstract description 16
- 229940043267 rhodamine b Drugs 0.000 claims abstract description 16
- 238000006731 degradation reaction Methods 0.000 claims abstract description 15
- 229960003405 ciprofloxacin Drugs 0.000 claims abstract description 13
- 239000001103 potassium chloride Substances 0.000 claims abstract description 13
- 235000011164 potassium chloride Nutrition 0.000 claims abstract description 13
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 12
- 239000002131 composite material Substances 0.000 claims abstract description 11
- 239000002957 persistent organic pollutant Substances 0.000 claims abstract description 9
- 238000005406 washing Methods 0.000 claims abstract description 9
- 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 8
- 239000000725 suspension Substances 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 230000001376 precipitating effect Effects 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 238000010189 synthetic method Methods 0.000 claims description 7
- 125000001559 cyclopropyl group Chemical group [H]C1([H])C([H])([H])C1([H])* 0.000 claims description 2
- 238000002604 ultrasonography Methods 0.000 claims description 2
- 230000015556 catabolic process Effects 0.000 abstract description 12
- 230000000694 effects Effects 0.000 abstract description 10
- 239000011941 photocatalyst Substances 0.000 abstract description 8
- 239000000843 powder Substances 0.000 abstract description 8
- 238000006555 catalytic reaction Methods 0.000 abstract description 6
- 230000007062 hydrolysis Effects 0.000 abstract description 5
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 5
- 238000004064 recycling Methods 0.000 abstract description 5
- 150000001875 compounds Chemical class 0.000 abstract description 3
- 230000002153 concerted effect Effects 0.000 abstract description 3
- 230000000593 degrading effect Effects 0.000 abstract description 3
- 238000001035 drying Methods 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 3
- 239000012046 mixed solvent Substances 0.000 abstract description 2
- 230000009257 reactivity Effects 0.000 abstract description 2
- 238000004062 sedimentation Methods 0.000 abstract description 2
- 238000001914 filtration Methods 0.000 abstract 1
- 238000000034 method Methods 0.000 description 9
- 239000000975 dye Substances 0.000 description 7
- 230000006872 improvement Effects 0.000 description 7
- 229960000935 dehydrated alcohol Drugs 0.000 description 5
- 238000004821 distillation Methods 0.000 description 5
- 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 5
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000007146 photocatalysis Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 229910052724 xenon Inorganic materials 0.000 description 4
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 4
- 230000003115 biocidal effect Effects 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 230000008021 deposition Effects 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 235000019441 ethanol Nutrition 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 230000008901 benefit Effects 0.000 description 2
- 238000001354 calcination Methods 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 229960004756 ethanol Drugs 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000011943 nanocatalyst Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 238000001338 self-assembly Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000005995 Aluminium silicate Substances 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 235000012211 aluminium silicate Nutrition 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
- -1 bismuthino Chemical group 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- GUJOJGAPFQRJSV-UHFFFAOYSA-N dialuminum;dioxosilane;oxygen(2-);hydrate Chemical compound O.[O-2].[O-2].[O-2].[Al+3].[Al+3].O=[Si]=O.O=[Si]=O.O=[Si]=O.O=[Si]=O GUJOJGAPFQRJSV-UHFFFAOYSA-N 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
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- MCPLVIGCWWTHFH-UHFFFAOYSA-L methyl blue Chemical compound [Na+].[Na+].C1=CC(S(=O)(=O)[O-])=CC=C1NC1=CC=C(C(=C2C=CC(C=C2)=[NH+]C=2C=CC(=CC=2)S([O-])(=O)=O)C=2C=CC(NC=3C=CC(=CC=3)S([O-])(=O)=O)=CC=2)C=C1 MCPLVIGCWWTHFH-UHFFFAOYSA-L 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 235000010755 mineral Nutrition 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052901 montmorillonite Inorganic materials 0.000 description 1
- 230000000877 morphologic effect Effects 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000007781 pre-processing Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 239000011435 rock Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000007962 solid dispersion Substances 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 229910052905 tridymite Inorganic materials 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
-
- 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
-
- 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 present invention relates to the synthesis and application of a kind of high dispersive BiOCl/ diatomite photochemical catalyst, belong to catalysis material water-treatment technology field, and in particular to a kind of synthesis and application of novel, efficient, organic pollutant in the environment that can be used for degrading photochemical catalyst BiOCl/ diatomite.For the present invention to purify smart diatomite as carrier, five water bismuth nitrates, potassium chloride are presoma, prepare the agent of BiOCl/ diatomite composite photocatalytic in the in the mixed solvent of ethylene glycol and water with an one-step hydrolysis sedimentation, obtain finished product after filtration, washing and drying.BiOCl of the invention is successfully loaded and is uniformly dispersed on diatomite rotary strainer, sufficiently exposes reactivity site, successfully solve the disadvantage that BiOCl powder photocatalyst is easy to reunite, difficult recycling, when diatomite content is greater than 30%, the hole of diatomite gradually reveals, the compound of photo-generated carrier can effectively be inhibited, the concerted catalysis effect for embodying diatomite, effectively improves the Ciprofloxacin of catalyst treatment difficult for biological degradation and the activity of dye, rhodamine B.
Description
Technical field
The present invention relates to the synthesis and application of a kind of high dispersive BiOCl/ diatomite photochemical catalyst, belong to catalysis material water
A kind of processing technology field, and in particular to novel, efficient, organic pollutant in the environment that can be used for degrading photochemical catalyst BiOCl/
The synthesis and application of diatomite.
Background technique
As a kind of novel green environmental protection technique, Photocatalytic Oxidation With Semiconductors technology turns in organic matter degradation and solar energy
Change aspect and shows great application prospect.A kind of semiconductor bismuthino photochemical catalyst of the BiOCl as indirect band gap, early in
Its photocatalysis performance is reported within 2006 under ultraviolet lighting than commerical grade TiO2Be higher by three times (Applied catalysis B:
Environmental, 2006,68:125-129), this is because BiOCl has anisotropic unique layer structure ([Bi2O2]
Layer and double Cl atomic layers) and electrical properties, electronics (e can be generated under illumination-) and hole (h+) and O2 -, OH isoreactivity
Free radical, these can play redox degradation to majority of organic pollutants in environment.But the BiOCl of preparation
That there are specific surface areas in degradation process is small for powdered photochemical catalyst, bad, easy to reunite, the difficult recycling of dispersibility and light induced electron are empty
A series of defects such as cave recombination rate height, so needing to improve the existing way of BiOCl to further increase its photocatalysis
Degradation property.
Some natural nonmetallic minerals such as diatomite, kaolin, montmorillonite and zeolite etc., can be used as photochemical catalyst
Ideal carrier, on the one hand solve the problems, such as reunion, the difficult recycling of nanocatalyst, on the other hand can also play synergistic effect and promote
Into the generation of redox reaction.Especially diatomite, it is a kind of biogenic deposit rock that ancient times diatom is formed, noncrystalline
SiO2For content up to 70% or more, diatom shell has the characteristics that acidproof, high temperature resistant, chemical inertness, and surface is a large amount of, ordered arrangement
Duct make it have high porosity, high-specific surface area and high absorption property, and it is rich reserves, cheap.Complete diatom
Range of soil cursting body (see Fig. 1 a) diameter at several microns to twenties microns.Stand in great numbers et al. in 80mL pure aquatic system with
2.8mmol Bi(NO3)·5H2O is as bismuth source, and 2.8mmol KX or NaX is as halogen source, after appropriate diatomite is added, under room temperature
One one-step hydrolysis deposition synthesis BiOX/ diatomite composite photocatalytic material, is found by rhodamine B degradation, 1.0g diatomite is added
Composite photo-catalyst illustrate preferable photocatalysis performance (patent application publication CN 107029757A), but pass through observation
The SEM of BiOX/ diatomite schemes, it is possible to find BiOX nanometer sheet is covered on diatomite surface, and BiOX nanometer sheet is mutually reunited one
It rises, has not only blocked the adsorption site of diatomite in this way, but also the reaction site of BiOX nanometer sheet can not also be completely exposed.Li et al.
People is loaded BiOI over celite by hydrolysis deposition in the system of pure water and ethyl alcohol, passes through rhodamine B degradation and Asia
Methyl blue discovery, the degradation effect of BiOI/7% diatomite preferably (Applied Surface Science 353 (2015)
1179-1185) it, can be found by observing the SEM figure of BiOI/ diatomite, due to the addition of ethyl alcohol, be loaded over celite
BiOI is to form flower ball-shaped by nanometer sheet self assembly, and sufficiently the active site of BiOI can be exposed for such pattern, but
Since diatomite content is less, BiOI can block most of adsorption site of diatomite.
For this purpose, we are intended to be formed a kind of Breakup of Liquid Ring of suitable particle growth using the performance and regulating strategy of solvent
Border, being prepared with the hydrolysis deposition of simple economy environmental protection can high dispersive, the active site of high exposure BiOCl, embodiment diatomite
The mesh of the organic pollutant quickly, in efficient degradation water is realized in the BiOCl/ diatomite composite photocatalytic agent of concerted catalysis performance
, therefore there is very big realistic meaning.
Summary of the invention
The present invention a kind of synthesis and application of high dispersive BiOCl/ diatomite photochemical catalyst, the purpose is to pass through adjusting solvent
The BiOCl/ diatomite photochemical catalyst of high degree of dispersion over celite is made in composition, so that it is in the group for solving nanocatalyst
The active site of catalyst and the concerted catalysis performance of diatomite are made full use of while poly-, difficult recycling problem, and then reaches drop
The effect of solving organic pollutant in environment.For the present invention to purify smart diatomite as carrier, five water bismuth nitrates, potassium chloride are forerunner
Body prepares the agent of BiOCl/ diatomite composite photocatalytic in the in the mixed solvent of ethylene glycol and water with an one-step hydrolysis sedimentation, passes through
Finished product is obtained after filter, washing, drying.
The present invention is achieved by the following technical solutions: a kind of synthesis side of high dispersive BiOCl/ diatomite photochemical catalyst
Method, comprising the following steps:
1) five water bismuth nitrates are weighed, are placed in ethylene glycol, ultrasonic 30min is denoted as solution A；Weigh again potassium chloride and
Smart diatomite, is placed in pure water, and ultrasonic 30min postscript is solution B；At room temperature, solution A is added dropwise to solution
In B, after stirring 1h, white suspension is obtained；
2) the white suspension of gained in step 1) is centrifuged with centrifuge, the precipitating of acquisition uses anhydrous second respectively
Alcohol after distilling water washing 3 times, is dried at 60 DEG C to get the agent of BiOCl/ diatomite composite photocatalytic is arrived.
In the present invention, regional high-grade diatomite is drying, super as raw material near a river using Jilin Province for the smart diatomite
Smart diatomite can be obtained after sound, water-bath acidleach, calcining.
As the further improvement of technical solution of the present invention, the molar ratio of five water bismuth nitrates and potassium chloride described in step 1)
For 1:1.
As the further improvement of technical solution of the present invention, the additional amount volume ratio of ethylene glycol described in step 1) and pure water
For 0.7-1.1:1.Experiments have shown that: it is entirely ethylene glycol according to solvent, BiOCl nanometer sheet has self assembly trend, keeps BiOCl brilliant
Body exists with spherical shape, is unfavorable for loading；It is entirely water according to solvent, BiOCl crystal is overlapped mutually with nanometer sheet form, nothing
BiOCl reactivity site is completely exposed in method.
As the further improvement of technical solution of the present invention, the concentration of five water bismuth nitrates is 0.0161g/ in the solution A
mL-0.4851g/mL。
As the further improvement of technical solution of the present invention, the concentration of potassium chloride is 0.0025g/mL- in the solution B
0.0746g/mL。
It is obtained invention further provides a kind of synthetic method of high dispersive BiOCl/ diatomite photochemical catalyst
Application of the BiOCl/ diatomite composite photocatalytic agent in degradable organic pollutant.
As the further improvement of application technology scheme of the present invention, the organic pollutant is Ciprofloxacin, dyestuff Luo Dan
Bright B.
As the further improvement of application technology scheme of the present invention, the reaction condition of the application are as follows:, will under normal temperature and pressure
BiOCl/ diatomite composite photocatalytic agent is placed in the solution containing Ciprofloxacin or/and dye, rhodamine B, light source irradiation, cyclopropyl
Degradation reaction occurs for husky star or/and dye, rhodamine B.
As the further improvement of application technology scheme of the present invention, the light source is simulated solar irradiation.When it is implemented, can
Using xenon lamp simulated solar irradiation.
The present invention a kind of synthesis and application method advantage of high dispersive BiOCl/ diatomite photochemical catalyst are as follows:
1) raw materials used cheap and easy to get, method therefor is simple and easy, economic and environment-friendly, does not generate poisonous and harmful by-product, behaviour
Make condition normal temperature and pressure, it is easy to accomplish industrialized production；
2) present invention prepares dispersion degree using the Morphological control effect of ethylene glycol and the solid dispersion effect of diatomite
BiOCl/ diatomite photochemical catalyst high, more than active site.The compound of photo-generated carrier can be effectively suppressed in this catalyst, urges light
The activity of agent is greatly improved, and is one of catalyst most excellent at present；
3) it is compared to traditional BiOCl powder photocatalyst, the made BiOCl/ diatomite photochemical catalyst of the present invention is same
Etc. good photocatalytic activity is shown in the case where dosages, and performance is stable, is easily recycled, this is to promoting the sun
The practical application of energy photocatalytic advanced oxidation technology is of great significance.
4) BiOCl nanometer sheet of the invention is successfully loaded and is uniformly dispersed on diatomite rotary strainer, sufficiently exposes reaction
Active site successfully solves the disadvantage that BiOCl powder photocatalyst is easy to reunite, difficult recycling, when diatomite content is greater than
When 30%, the hole of diatomite is gradually revealed, and can effectively inhibit the compound of photo-generated carrier, and the collaboration for embodying diatomite is urged
Change effect, effectively improves the Ciprofloxacin of catalyst treatment difficult for biological degradation and the activity of dye, rhodamine B.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention for those of ordinary skill in the art without creative efforts, can be with
It obtains other drawings based on these drawings.
Fig. 1 is made smart diatomite, BiOCl (comparative example 1), BiOCl/30% (embodiment 1), BiOCl/50% (implementation
Example 2) diatomite catalyst SEM spectrum.A is made smart diatomite in figure, and b BiOCl, c are that BiOCl/30% diatomite is urged
Agent, d are BiOCl/50% diatomite catalyst.
Fig. 2 is made smart diatomite, BiOCl (comparative example 1), BiOCl/30% (embodiment 1), BiOCl/50% (implementation
Example 2) diatomite catalyst XRD spectrum.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, technical solution of the present invention will be carried out below
Detailed description.Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Base
Embodiment in the present invention, those of ordinary skill in the art are obtained all without making creative work
Other embodiment belongs to the range that the present invention is protected.
Technical solution of the present invention is described in detail with reference to the accompanying drawing.
Raw material pre-processing
Smart diatomite the preparation method comprises the following steps: regional high-grade diatomite is first dried at 110 DEG C as raw material near a river using Jilin Province
12h is placed in case；28wt% sulfuric acid ultrasound 10min is added with the liquid-solid ratio (6mL liquid corresponds to 1g solid) of 6:1；In 100 DEG C of water
4h is heated in bath, is diluted and (is diluted using 28wt% sulfuric acid) by 15:1 liquid-solid ratio and continues 100 DEG C of heating 1h afterwards, filter, wash,
It is dry；With 500 DEG C of calcining 2h in Muffle furnace, both smart diatomite.
High-grade diatomite of the present invention is provided by Bei Feng diatomite Co., Ltd near a river.
Comparative example 1
Five water bismuth nitrate of 2.4255g is weighed, is placed in 20mL ethylene glycol, ultrasonic 30min is denoted as solution A；Claim again
0.3730g potassium chloride is taken to be placed in 20mL pure water, ultrasonic 30min postscript is solution B；At room temperature, dropwise by solution A
It is added in solution B, after stirring 1h, obtains white suspension.With centrifuge by the white suspension of gained in step 1) carry out from
Heart separation, gained precipitating with after dehydrated alcohol, distillation water washing 3 times, are dried at 60 DEG C to get BiOCl photocatalysis is arrived respectively
Agent powder.
The application method of the photochemical catalyst BiOCl synthesized in aforementioned manners, it is characterised in that difficult biology drop in the water
The antibiotic ciprofloxacin and dye, rhodamine B of solution, reaction condition are as follows: normal temperature and pressure, catalyst amount be respectively 0.05g (or
0.025g) and 0.02g (or 0.01g), the treating capacity of Ciprofloxacin and rhodamine B is 100mL, 10mgL-1, light source used
For xenon lamp, power 300W is used up apart from reaction interface 15cm as simulated solar irradiation.
Embodiment 1
Five water bismuth nitrate of 0.9720g is weighed, is placed in 10mL ethylene glycol, ultrasonic 30min is denoted as solution A；Claim again
0.1490g potassium chloride and 0.2270g essence diatomite are taken, is placed in 10mL pure water, ultrasonic 30min postscript is solution B；?
At room temperature, solution A is added dropwise in solution B, after stirring 1h, obtains white suspension.With centrifuge by institute in step 1)
White suspension is obtained to be centrifuged, gained precipitating with after dehydrated alcohol, distillation water washing 3 times, is dried at 60 DEG C respectively,
Obtain BiOCl/30% diatomite photocatalyst powder (the smart diatomite containing 30%).
The application method of the photochemical catalyst BiOCl/30% diatomite synthesized in aforementioned manners, it is characterised in that the water
The antibiotic ciprofloxacin and dye, rhodamine B of middle difficult for biological degradation, reaction condition are as follows: normal temperature and pressure, catalyst amount are
The treating capacity of 0.05g and 0.02g, Ciprofloxacin and rhodamine B is 100mL, 10mgL-1, light source used is xenon lamp, power
It uses up for 300W apart from reaction interface 15cm as simulated solar irradiation.
Embodiment 2
Five water bismuth nitrate of 2.4255g is weighed, is placed in 20mL ethylene glycol, ultrasonic 30min is denoted as solution A；Claim again
0.3730g potassium chloride and 1.3020g essence diatomite are taken, is placed in 20mL pure water, ultrasonic 30min postscript is solution B；?
At room temperature, solution A is added dropwise in solution B, after stirring 1h, obtains white suspension.With centrifuge by institute in step 1)
White suspension is obtained to be centrifuged, gained precipitating with after dehydrated alcohol, distillation water washing 3 times, is dried at 60 DEG C respectively,
Obtain BiOCl/50% diatomite photocatalyst powder (the smart diatomite containing 50%).
The application method of the photochemical catalyst BiOCl/50% diatomite synthesized in aforementioned manners, difficult biology drop in the water
The antibiotic ciprofloxacin and dye, rhodamine B of solution, reaction condition are as follows: normal temperature and pressure, catalyst amount are 0.05g and 0.02g,
The treating capacity of Ciprofloxacin and rhodamine B is 100mL, 10mgL-1, light source used is xenon lamp, and power 300W, distance is instead
Interface 15cm is answered, is used up as simulated solar irradiation.
Comparative example 1 to each catalyst of embodiment 2 performance referring to Tables 1 and 2.
1 different catalysts of table are under simulated solar irradiation to the degradation rate of Ciprofloxacin
2 different catalysts of table are under simulated solar irradiation to the degradation rate of rhodamine B
By Tables 1 and 2 it can be seen that the effect of catalyzing and degrading pollutant obviously mentions after BiOCl is carried on diatomite
It rises.
Embodiment 3
Five water bismuth nitrate of 2.4255g is weighed, is placed in 5mL ethylene glycol, ultrasonic 30min is denoted as solution A；It weighs again
0.5222g potassium chloride and 1.2030g essence diatomite, are placed in 7mL pure water, and ultrasonic 30min postscript is solution B；In room
Under temperature, solution A is added dropwise in solution B, after stirring 1h, obtains white suspension.With centrifuge by gained in step 1)
White suspension is centrifuged, and gained precipitating with after dehydrated alcohol, distillation water washing 3 times, is dried, i.e., at 60 DEG C respectively
Obtain BiOCl/ diatomite photocatalyst powder.
Embodiment 4
Five water bismuth nitrate of 0.4851g is weighed, is placed in 33mL ethylene glycol, ultrasonic 30min is denoted as solution A；Claim again
0.0750g potassium chloride and 1.3020g essence diatomite are taken, is placed in 30mL pure water, ultrasonic 30min postscript is solution B；?
At room temperature, solution A is added dropwise in solution B, after stirring 1h, obtains white suspension.With centrifuge by institute in step 1)
White suspension is obtained to be centrifuged, gained precipitating with after dehydrated alcohol, distillation water washing 3 times, is dried at 60 DEG C respectively,
Obtain BiOCl/ diatomite photocatalyst powder.
The above description is merely a specific embodiment, but scope of protection of the present invention is not limited thereto, any
Those familiar with the art in the technical scope disclosed by the present invention, can easily think of the change or the replacement, and should all contain
Lid is within protection scope of the present invention.Therefore, protection scope of the present invention should be based on the protection scope of the described claims.
Claims (9)
1. a kind of synthetic method of high dispersive BiOCl/ diatomite photochemical catalyst, which comprises the following steps:
1) five water bismuth nitrates are weighed, are placed in ethylene glycol, 30 min of ultrasound are denoted as solution A；Potassium chloride and essence are weighed again
Diatomite is placed in pure water, and ultrasonic 30 min postscripts are solution B；At room temperature, solution A is added dropwise to solution B
In, after stirring 1 h, obtain white suspension；
2) the white suspension of gained in step 1) is centrifuged with centrifuge, the precipitating of acquisition uses anhydrous second respectively
Alcohol after distilling water washing 3 times, is dried at 60 DEG C to get the agent of BiOCl/ diatomite composite photocatalytic is arrived.
2. a kind of synthetic method of high dispersive BiOCl/ diatomite photochemical catalyst according to claim 1, which is characterized in that
The molar ratio of five water bismuth nitrates and potassium chloride described in step 1) is 1:1.
3. a kind of synthetic method of high dispersive BiOCl/ diatomite photochemical catalyst according to claim 2, which is characterized in that
The additional amount volume ratio of ethylene glycol described in step 1) and pure water is 0.7-1.1:1.
4. a kind of synthetic method of high dispersive BiOCl/ diatomite photochemical catalyst according to claim 3, which is characterized in that
The concentration of five water bismuth nitrates is 0.0161g/mL-0.4851g/mL in the solution A.
5. a kind of synthetic method of high dispersive BiOCl/ diatomite photochemical catalyst according to claim 4, which is characterized in that
The concentration of potassium chloride is 0.0025 g/mL-0.0746g/mL in the solution B.
6. a kind of synthetic method acquisition of high dispersive BiOCl/ diatomite photochemical catalyst described in claims 1 or 2 or 3 or 4 or 5
Application of the BiOCl/ diatomite composite photocatalytic agent in degradable organic pollutant.
7. application according to claim 6, which is characterized in that the organic pollutant is Ciprofloxacin, dye, rhodamine
B。
8. application according to claim 7, which is characterized in that the reaction condition of the application are as follows:, will under normal temperature and pressure
BiOCl/ diatomite composite photocatalytic agent is placed in the solution containing Ciprofloxacin or/and dye, rhodamine B, light source irradiation, cyclopropyl
Degradation reaction occurs for husky star or/and dye, rhodamine B.
9. application according to claim 8, which is characterized in that the light source is simulated solar irradiation.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811499453.8A CN109331845A (en) | 2018-12-09 | 2018-12-09 | A kind of synthesis and application of high dispersive BiOCl/ diatomite photochemical catalyst |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811499453.8A CN109331845A (en) | 2018-12-09 | 2018-12-09 | A kind of synthesis and application of high dispersive BiOCl/ diatomite photochemical catalyst |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109331845A true CN109331845A (en) | 2019-02-15 |
Family
ID=65303079
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811499453.8A Pending CN109331845A (en) | 2018-12-09 | 2018-12-09 | A kind of synthesis and application of high dispersive BiOCl/ diatomite photochemical catalyst |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109331845A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN110743578A (en) * | 2019-11-21 | 2020-02-04 | 中国地质大学（北京） | Tourmaline-loaded BiOI photocatalyst and preparation method thereof |
| CN112871187A (en) * | 2021-01-18 | 2021-06-01 | 武汉梓强生态科技有限公司 | Modified diatomite-loaded BiVO4-BiOCl heterojunction composite material and application |
| 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 |
| CN115228488A (en) * | 2022-07-21 | 2022-10-25 | 上海力巢新材料科技有限公司 | Preparation method and application of nano diatomite composite decorative material |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101879455A (en) * | 2010-07-07 | 2010-11-10 | 太原理工大学 | Preparation and application of bismuth oxychloride as photocatalyst |
| WO2013098428A1 (en) * | 2011-12-30 | 2013-07-04 | Inael Electrical Systems, S.A. | Mechanochemical method for synthesizing doped anatase-phase titanium-dioxide particles |
| CN105854906A (en) * | 2016-04-27 | 2016-08-17 | 中国矿业大学(北京) | BiOCl-TiO2/diatomite photocatalyst and preparation method thereof |
| CN107029757A (en) * | 2017-05-22 | 2017-08-11 | 湖南城市学院 | A kind of preparation method of BiOX diatomite composite photocatalytic agent |
| CN107837813A (en) * | 2017-11-21 | 2018-03-27 | 长治学院 | Chlorine oxygen bismuth/modified montmorillonoid composite photo-catalyst and its preparation method and application |
-
2018
- 2018-12-09 CN CN201811499453.8A patent/CN109331845A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101879455A (en) * | 2010-07-07 | 2010-11-10 | 太原理工大学 | Preparation and application of bismuth oxychloride as photocatalyst |
| WO2013098428A1 (en) * | 2011-12-30 | 2013-07-04 | Inael Electrical Systems, S.A. | Mechanochemical method for synthesizing doped anatase-phase titanium-dioxide particles |
| CN105854906A (en) * | 2016-04-27 | 2016-08-17 | 中国矿业大学(北京) | BiOCl-TiO2/diatomite photocatalyst and preparation method thereof |
| CN107029757A (en) * | 2017-05-22 | 2017-08-11 | 湖南城市学院 | A kind of preparation method of BiOX diatomite composite photocatalytic agent |
| CN107837813A (en) * | 2017-11-21 | 2018-03-27 | 长治学院 | Chlorine oxygen bismuth/modified montmorillonoid composite photo-catalyst and its preparation method and application |
Non-Patent Citations (2)
| Title |
|---|
| HAILI LIN ET AL.，: ""Ethylene glycol-assisted synthesis, photoelectrochemical and photocatalytic properties of BiOI microflowers"", 《MATERIALS CHEMISTRY》 * |
| 贾泽慧等，: ""临江高品位硅藻土的物理化学提纯"", 《人工晶体学报》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN112871187A (en) * | 2021-01-18 | 2021-06-01 | 武汉梓强生态科技有限公司 | Modified diatomite-loaded BiVO4-BiOCl heterojunction composite material and application |
| 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 |
| CN115228488A (en) * | 2022-07-21 | 2022-10-25 | 上海力巢新材料科技有限公司 | Preparation method and application of nano diatomite composite decorative material |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109331845A (en) | A kind of synthesis and application of high dispersive BiOCl/ diatomite photochemical catalyst | |
| Yuan et al. | Multi-component design and in-situ synthesis of visible-light-driven SnO2/g-C3N4/diatomite composite for high-efficient photoreduction of Cr (VI) with the aid of citric acid | |
| Wei et al. | Novel pn heterojunction photocatalyst fabricated by flower-like BiVO4 and Ag2S nanoparticles: Simple synthesis and excellent photocatalytic performance | |
| Cai et al. | Controllable location of Au nanoparticles as cocatalyst onto TiO2@ CeO2 nanocomposite hollow spheres for enhancing photocatalytic activity | |
| CN110918126B (en) | Preparation method of flower-shaped molybdenum disulfide combined UiO-66 photocatalyst | |
| Zhang et al. | Synthesis of BiOCl/TiO2–zeolite composite with enhanced visible light photoactivity | |
| CN108273564B (en) | Composite visible light photocatalyst Ag2CO3/TiO2/UiO-66-(COOH)2Preparation method and application thereof | |
| CN106492849B (en) | A kind of preparation method of BiOCl ultrathin nanometer piece photochemical catalyst | |
| CN104707542B (en) | A kind of photochemical catalyst/SiO2aerogel composite and preparation method thereof | |
| CN103172030A (en) | Oxide powder and preparation method thereof as well as catalyst and carrier thereof | |
| Parida et al. | Visible light response photocatalytic water splitting over CdS-pillared zirconium–titanium phosphate (ZTP) | |
| CN102580714A (en) | Graphene oxide/silver phosphate composite visible light catalyst and preparation method thereof | |
| Zhu et al. | Efficient photocatalytic water splitting through titanium silicalite stabilized CoO nanodots | |
| CN102674451A (en) | Preparation method of {001} face exposed titanium dioxide nanocrystals | |
| Liu et al. | A novel amorphous CoS x/NH 2-MIL-125 composite for photocatalytic degradation of rhodamine B under visible light | |
| He et al. | Biogenic C-doped titania templated by cyanobacteria for visible-light photocatalytic degradation of Rhodamine B | |
| Pandey et al. | Synthesis of novel tetranuclear Ni complex incorporated mesoporous silica for improved photocatalytic degradation of methylene blue in presence of visible light | |
| CN109647437B (en) | CuS doped nano TiO2Photocatalyst, preparation method and application thereof | |
| CN109876804A (en) | A kind of titanium dioxide loaded ruthenium catalyst and preparation method thereof adding hydrogen cyclohexene for benzene selective | |
| CN108160121B (en) | Composite visible light photocatalyst Ag2CO3/TiO2/UIO-66-(COOH)2And application of organic matter degradation | |
| Chen et al. | Highly enhanced photocatalytic degradation of dye rhodamine B on the biogenic hierarchical porous TiO 2/SiO 2 with 1D/3D-chain | |
| CN108393083A (en) | A kind of bismuth vanadate photocatalyst and preparation method for sewage disposal | |
| CN101676031B (en) | Photocatalyst with core-shell structure and applications thereof | |
| CN114082448B (en) | Tb-MOF/P-TiO 2 Heterojunction photocatalyst, preparation and application thereof | |
| CN109126829A (en) | A kind of 3-D heterojunction structure CdS-MoS2The preparation method of composite granule |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |