CN106861678A - It is a kind of without surfactant and the flower-shaped Bi of template2MoO6The preparation method of catalysis material - Google Patents

It is a kind of without surfactant and the flower-shaped Bi of template2MoO6The preparation method of catalysis material Download PDF

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Publication number
CN106861678A
CN106861678A CN201611196884.8A CN201611196884A CN106861678A CN 106861678 A CN106861678 A CN 106861678A CN 201611196884 A CN201611196884 A CN 201611196884A CN 106861678 A CN106861678 A CN 106861678A
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China
Prior art keywords
solution
shaped
moo
flower
ammonium molybdate
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CN201611196884.8A
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Chinese (zh)
Inventor
谢宇
孙朝阳
张健
凌云
杨景心
李嘉昌
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Nanchang Hangkong University
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Nanchang Hangkong University
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Priority to CN201611196884.8A priority Critical patent/CN106861678A/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/16Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J23/24Chromium, molybdenum or tungsten
    • B01J23/31Chromium, molybdenum or tungsten combined with bismuth
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/002Mixed oxides other than spinels, e.g. perovskite
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00Catalysts, in general, characterised by their form or physical properties
    • B01J35/30
    • B01J35/39
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/30Treatment of water, waste water, or sewage by irradiation
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/38Organic compounds containing nitrogen
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2305/00Use of specific compounds during water treatment
    • C02F2305/10Photocatalysts
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W10/00Technologies for wastewater treatment
    • Y02W10/30Wastewater or sewage treatment systems using renewable energies
    • Y02W10/37Wastewater or sewage treatment systems using renewable energies using solar energy

Abstract

The invention discloses a kind of without surfactant and the flower-shaped Bi of template2MoO6The preparation method of catalysis material, the present invention prepares urea catalysis material as primary raw material with five nitric hydrate bismuths, Ammonium Molybdate Tetrahydrate, urea, concentrated nitric acid, sodium acid carbonate using the method that water-bath flows back.And the test of photocatalysis performance is carried out to the material prepared using simulated solar irradiation, the superior photocatalysis performance of the material is proved by degradation biological persistent organic pollutants rhodamine B.The method does not have any surfactant and template material of addition in preparation process, and preparation process is simply novel.The composite belongs to inorganic catalysis material, flower-shaped Bi2MoO6It is by a large amount of super-thin sheet-shaped Bi2MoO6Self assembly is formed, and photocatalytic activity is higher, there is good application prospect in terms of environmental protection.

Description

It is a kind of without surfactant and the flower-shaped Bi of template2MoO6The system of catalysis material Preparation Method
Technical field
The present invention relates to a kind of without surfactant and the flower-shaped Bi of template2MoO6The preparation method of catalysis material, Belong to optic catalytic composite material preparation field.
Background technology
In recent years, along with the development of China's rough formula of industry, problem of environmental pollution is also increasingly severe, water and air Pollution has seriously threatened the existence and procreation of the mankind.Contain substantial amounts of toxic organic pollutant in some chemical emissions, These pollutants can be enriched with the person, and the health to the mankind causes huge injury.In recent years, people always search for solution The certainly method of environmental pollution, the sight of correlative study person has gradually been placed on sight using this unlimited regenerative resource of solar energy Photocatalitic Technique of Semiconductor on.Can be by the efficient purifying water body of photocatalysis technology by sunshine.Traditional light Catalyst TiO2Have the advantages that photocatalytic activity is high, inexpensive nontoxic, anti-light burn into stable chemical nature photocatalysis technology research Active material.But TiO2Forbidden band energy gap be 3.2 eV, the ultraviolet light of short wavelength can only be absorbed and excited, and ultraviolet The energy of line only accounts for total 5 percent or so of sunlight, so TiO2Light utilization ratio is relatively low.
Bi2MoO6It is a kind of conductor photocatalysis material with visible light catalysis activity higher, it can be used in waste water The treatment of organic pollution, can decompose part in air harmful inorganic substances and almost all harmful organic substance Matter, very important effect is served to purify air environment purification.Bi2MoO6Maximum absorption wavelength is about 491nm, is a kind of There is the photochemical catalyst of response to visible ray well, it all shows excellent in terms of solar energy conversion and environmental pollution improvement Different visible light catalysis activity.Bi2MoO6Structure be simplest Aurivillius types oxide, its pattern, size etc. are The key factor of its chemical property is influenceed, therefore, study Bi2MoO6The controlledly synthesis of pattern and its visible light catalytic performance have There are most important theories meaning and practical value.
The content of the invention
It is an object of the invention to provide a kind of without surfactant and the flower-shaped Bi of template2MoO6Catalysis material system Preparation Method, is flowed back as primary raw material with five nitric hydrate bismuths, Ammonium Molybdate Tetrahydrate, urea, concentrated nitric acid, sodium acid carbonate using water-bath Method prepare urea catalysis material.And the survey of photocatalysis performance is carried out to the material prepared using simulated solar irradiation Examination, the superior photocatalysis performance of the material is proved by degradation biological persistent organic pollutants rhodamine B.The method is in system There is no addition any surfactant and template material during standby, preparation process is simply novel.The composite belongs to nothing Machine catalysis material, flower-shaped Bi2MoO6It is by a large amount of super-thin sheet-shaped Bi2MoO6Self assembly is formed, and photocatalytic activity is higher, in ring Border protection aspect has good application prospect.
It is a kind of without surfactant and the flower-shaped Bi of template2MoO6The preparation method of catalysis material, step is as follows:
Step one:
Two kinds of solids of five nitric hydrate bismuths and Ammonium Molybdate Tetrahydrate are weighed, the nitric acid that 15ml concentration is 2mol/L is dissolved in respectively molten In liquid, stirring makes it form five nitric hydrate bismuth solution and Ammonium Molybdate Tetrahydrate solution respectively;
Step 2:
Ammonium Molybdate Tetrahydrate solution is added drop-wise in five nitric hydrate bismuth solution, ultrasound 10min again after stirring 30min is mixed Close solution;
Step 3:
Sodium bicarbonate powder is added in the mixed solution obtained in step 2, and mixed solution is continued to monitor with pH meter PH, between the pH of mixed solution reaches 6-7;
Step 4:
The mixed solution that pH will be mixed up is transferred in round-bottomed flask, is centrifuged after the 18h that flowed back at 80 DEG C and is precipitated;
Step 5:
The precipitation deionized water and ethanol of acquisition are washed twice respectively, the product that will have been washed is put into 60 in vacuum drying chamber Degree dries 12 hours, obtains final products.
In described step one, the ratio between molal quantity of bismuth element and molybdenum element in five nitric hydrate bismuths and Ammonium Molybdate Tetrahydrate It is 2:1.
It is an advantage of the invention that:
The present invention relates to a kind of Bi with floriform appearance by super-thin sheet-shaped self assembly2MoO6The preparation of catalysis material Method, without any surfactant and template in preparation process, it is to avoid the trouble of removal additive, and addition Agent is possible to the problems such as removing unclean, and reduces synthesis cost.The plain mode that reaction is flowed back using water-bath, is a kind of Simple and effective synthetic method.50mg this products are in visible ray(λ>420nm)Lower degraded 50ml concentration is the rhodamine B of 10PPm Solution, degradation rate reaches 45% within 90 minutes.
Brief description of the drawings
Fig. 1 is to weigh the flower-shaped Bi of 50mg2MoO6Product is in visible ray(λ>420nm)Lower degraded 50ml concentration is sieve of 10PPm The degradation curve of red bright B solution.
Fig. 2 is the SEM scanning electron microscope (SEM) photographs of product.
Specific embodiment
Below by embodiment 1-3, the invention will be further described.
Embodiment 1
Step one:Two kinds of solids of the nitric hydrate bismuths of 1.2121g five and 0.2207g Ammonium Molybdate Tetrahydrates accurately are weighed, is dissolved respectively In 15ml concentration in the salpeter solution of 2mol/L, stirring forms it into five nitric hydrate bismuth solution and Ammonium Molybdate Tetrahydrate is molten Liquid;
Step 2:Ammonium Molybdate Tetrahydrate solution is added drop-wise in five nitric hydrate bismuth solution, ultrasound 10min again after stirring 30min, Obtain mixed solution;
Step 3:Sodium bicarbonate powder is added in the mixed solution obtained in step 2, and mixing is continued to monitor with pH meter The pH of solution, until the Ph of mixed solution reaches 6.5.
Step 4:The mixed solution that pH will be mixed up is transferred in round-bottomed flask, is centrifuged after the 18h that flowed back at 80 DEG C and obtained Precipitation.
Step 5:The precipitation deionized water and ethanol of acquisition are washed twice respectively.The product that will have been washed is put into very 12 hours of 60 degree of dryings in empty drying box, obtain final products.
Embodiment 2
Step one:Two kinds of solids of the nitric hydrate bismuths of 1.2121g five and 0.2207g Ammonium Molybdate Tetrahydrates accurately are weighed, is dissolved respectively In 15ml concentration in the salpeter solution of 2mol/L, stirring forms it into five nitric hydrate bismuth solution and Ammonium Molybdate Tetrahydrate is molten Liquid;
Step 2:Ammonium Molybdate Tetrahydrate solution is added drop-wise in five nitric hydrate bismuth solution, ultrasound 10min again after stirring 30min, Obtain mixed solution;
Step 3:Sodium bicarbonate powder is added in the mixed solution obtained in step 2, and mixing is continued to monitor with pH meter The pH of solution, until the pH of mixed solution reaches 7.
Step 4:The mixed solution that pH will be mixed up is transferred in round-bottomed flask, is centrifuged after the 18h that flowed back at 80 DEG C and obtained Precipitation.
Step 5:The precipitation deionized water and ethanol of acquisition are washed twice respectively.The product that will have been washed is put into very 12 hours of 60 degree of dryings in empty drying box, obtain final products.
Embodiment 3
Step one:Two kinds of solids of the nitric hydrate bismuths of 1.2121g five and 0.2207g Ammonium Molybdate Tetrahydrates accurately are weighed, is dissolved respectively In 15ml concentration in the salpeter solution of 2mol/L, stirring forms it into five nitric hydrate bismuth solution and Ammonium Molybdate Tetrahydrate is molten Liquid;
Step 2:Ammonium Molybdate Tetrahydrate solution is added drop-wise in five nitric hydrate bismuth solution, ultrasound 10min again after stirring 30min, Obtain mixed solution;
Step 3:Sodium bicarbonate powder is added in the mixed solution obtained in step 2, and mixing is continued to monitor with pH meter The pH of solution, until the pH of mixed solution reaches 6.7.
Step 4:The mixed solution that pH will be mixed up is transferred in round-bottomed flask, is centrifuged after the 18h that flowed back at 80 DEG C and obtained Precipitation.
Step 5:The precipitation deionized water and ethanol of acquisition are washed twice respectively.The product that will have been washed is put into very 12 hours of 60 degree of dryings in empty drying box, obtain final products.
By the flower-shaped Bi of final product2MoO650mg is under simulated solar irradiation for the rhodamine B solution of the 50ml 10PPm that degrade Refer to accompanying drawing 1.
Fig. 2 be embodiment 1-2 obtained by product scanning electron microscope (SEM) photograph, from the figure, it can be seen that with a process for preparing Flower-shaped Bi2MoO6It is by substantial amounts of super-thin sheet-shaped Bi2MoO6Self assembly is formed.

Claims (2)

1. a kind of without surfactant and the flower-shaped Bi of template2MoO6The preparation method of catalysis material, it is characterized by:Step It is rapid as follows:
Step one:
Two kinds of solids of five nitric hydrate bismuths and Ammonium Molybdate Tetrahydrate are weighed, the nitric acid that 15ml concentration is 2mol/L is dissolved in respectively molten In liquid, stirring makes it form five nitric hydrate bismuth solution and Ammonium Molybdate Tetrahydrate solution respectively;
Step 2:
Ammonium Molybdate Tetrahydrate solution is added drop-wise in five nitric hydrate bismuth solution, ultrasound 10min again after stirring 30min is mixed Close solution;
Step 3:
Sodium bicarbonate powder is added in the mixed solution obtained in step 2, and mixed solution is continued to monitor with pH meter PH, between the pH of mixed solution reaches 6-7;
Step 4:
The mixed solution that pH will be mixed up is transferred in round-bottomed flask, is centrifuged after the 18h that flowed back at 80 DEG C and is precipitated;
Step 5:
The precipitation deionized water and ethanol of acquisition are washed twice respectively, the product that will have been washed is put into 60 in vacuum drying chamber Degree dries 12 hours, obtains final products.
2. as claimed in claim 1 a kind of without surfactant and the flower-shaped Bi of template2MoO6The preparation of catalysis material Method, it is characterized by:In step one, the ratio between molal quantity of bismuth element and molybdenum element in five nitric hydrate bismuths and Ammonium Molybdate Tetrahydrate It is 2:1.
CN201611196884.8A 2016-12-22 2016-12-22 It is a kind of without surfactant and the flower-shaped Bi of template2MoO6The preparation method of catalysis material Pending CN106861678A (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101254463A (en) * 2008-04-11 2008-09-03 南京大学 Synthetic method of visible light catalyst Bi2MoO6
CN106076429A (en) * 2016-06-06 2016-11-09 东华大学 A kind of textile fabric/Graphene/Bi2moO6/ BiPO4the preparation method of combinational environment catalysis material

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101254463A (en) * 2008-04-11 2008-09-03 南京大学 Synthetic method of visible light catalyst Bi2MoO6
CN106076429A (en) * 2016-06-06 2016-11-09 东华大学 A kind of textile fabric/Graphene/Bi2moO6/ BiPO4the preparation method of combinational environment catalysis material

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
XUEMEI HOU, ET AL.: "Preparation and characterization of Fe3O4/SiO2/Bi2MoO6 composite as magnetically separable photocatalyst", 《JOURNAL OF ALLOYS AND COMPOUNDS》 *

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Application publication date: 20170620

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