CN105126821B - A kind of flower-shaped Bi2MoO6Preparation and its in photo catalytic reduction CO2In application - Google Patents
A kind of flower-shaped Bi2MoO6Preparation and its in photo catalytic reduction CO2In application Download PDFInfo
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- CN105126821B CN105126821B CN201510497285.9A CN201510497285A CN105126821B CN 105126821 B CN105126821 B CN 105126821B CN 201510497285 A CN201510497285 A CN 201510497285A CN 105126821 B CN105126821 B CN 105126821B
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- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
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- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/52—Improvements relating to the production of bulk chemicals using catalysts, e.g. selective catalysts
Abstract
The present invention relates to photocatalysis technology field, mainly provides a kind of flower-shaped Bi2MoO6Preparation and its in photo catalytic reduction CO2In application, it is characterised in that：Bi2MoO6For photochemical catalyst using bismuth nitrate, sodium molybdate as raw material, polyvinylpyrrolidone is pattern conditioning agent, is prepared by hydro-thermal method.In aqueous, the catalyst can be catalyzed reduction CO under visible light conditions2Prepare methanol and ethanol.It is an advantage of the invention that；The photochemical catalyst is to CO2Adsorption capacity it is strong, photo-quantum efficiency is high, is promoting CO2Emission reduction, the alternative energy source for developing fossil fuel and efficiently had broad application prospects using solar energy etc..
Description
Technical field
The present invention relates to photocatalysis technology field, mainly provides a kind of floriform appearance Bi2MoO6The preparation of catalysis material and
Its photo catalytic reduction CO2The method for preparing methanol and ethanol.
Background technology
The 80% of our times energy resource consumption still comes from the fossil energy based on oil, coal, natural gas.Continue to increase
Fossil energy consumption not only cause in air with CO2Based on greenhouse gas concentration sharply increase, more cause today's society
Energy crisis.But while as greenhouse gases, CO2And nontoxic, rich reserves C1 resources.Therefore if by CO2Effectively turn
Clean energy resource is turned to, is to solve current CO2Energy crisis has caused by caused greenhouse effects and fossil fuel consume excessively
Effect approach.Although current CO2It is a variety of dimethyl ether, carbonic ester, salicylic acid, urea, synthesis gas etc. can be converted into by chemical method
Basic chemical industry raw material and intermediate, but CO is activated in conversion process2The required big energy overwhelming majority still needs consumptionization
The stone energy provides.This just can not effectively realize CO2Emission reduction and alleviating energy crisis.
Sunshine is the energy cleaned the most on the earth, be cheap, enriched.Such as realized using solar energy to CO2Photocatalysis
Conversion, then can really realize CO2Emission reduction and synchronously completing of recycling of carbon resource, effectively alleviate greenhouse effects and carbon source danger
Machine.In recent years, people utilize photochemical catalyst such as TiO2、 CdS、ZnO、Cu2O、SiC、C3N4、WO3Deng can be successfully by CO2Conversion
For the high energy hydrocarbon such as methane, methanol, formic acid.Wherein TiO2Ground the most extensively because cheap, stable performance turns into
One of photochemical catalyst studied carefully.But the shortcomings that its is maximum is TiO2Only to accounting for ultraviolet light of the solar energy less than 5%（Wavelength< 400 nm）
There is effect, optoelectronic transformation efficiency is low in the case where accounting for the visible light conditions of solar energy 43%, catalytic effect is poor.Therefore, develop in visible striation
Effective photo catalytic reduction CO under part2Catalysis material turn into current people research emphasis.
As typical Aurivillius oxides, Bi2MoO6It is that one kind has narrow band gap（Eg = 2.63 eV）Half
Conductor, the visible ray for accounting for sunshine 50% can be directly absorbed, there are preferable absorbent properties to sunshine.In recent years
It is widely used as the catalysis material of light degradation organic dyestuff.But there has been no utilize Bi at present2MoO6As CO2Photo-reduction is catalyzed
The report of agent occurs.We utilize Bi first in the present invention2MoO6As photochemical catalyst, successfully water is situated between under visible light conditions
CO in matter2Photo catalytic reduction is methanol and ethanol.In addition, to effectively improve its photocatalytic activity, we are adjusted by pattern
The floriform appearance Bi for successfully synthesizing high-specific surface area and electric transmission efficiency is added in agent2MoO6。
The content of the invention
Present invention generally provides a kind of floriform appearance Bi2MoO6The preparation of catalysis material and its urged under visible light conditions
Change reduction CO2The method for preparing methanol and ethanol.
A kind of flower-shaped Bi of the present invention2MoO6Preparation method, it is characterised in that Bi2MoO6It is made using following steps：
（1）By bismuth nitrate, sodium molybdate, polyvinylpyrrolidone are dissolved separately in the HNO that isometric concentration is 1 M3Solution
In；Wherein, nitric acid bi concns are 0.2 M, and molybdic acid na concn is 0.1 M, and PVP addition is respectively 0-0.4g, and mixing is above-mentioned
Three kinds of solution are simultaneously transferred in autoclave, 180oHydro-thermal reaction 6-36 h under the conditions of C；
（2）Solid by filtration after hydro-thermal reaction is washed with deionized to neutrality after collecting, 80oDone under the conditions of C
Dry 8 h, that is, obtain Bi2MoO6Catalyst.
The addition of polyvinylpyrrolidone of the present invention is preferably 0.3 g.
The hydro-thermal reaction time of the present invention is preferably 24 h.
The Bi of the floriform appearance of synthesis of the present invention2MoO6Photocatalyst material, can be by aqueous medium under visible light conditions
In CO2Photo catalytic reduction is methanol and ethanol.
Photo catalytic reduction CO2Reaction condition be：By 50mg Bi2MoO6It is added in quartz reactor, holds with 50 mL water
Continuous stirring, reactor are placed in 4oIn C water-bath, 100 mL/min CO are continuously passed through after air in reactor is pumped2
After 30min, stable CO2Flow is 50 mL/min, with the W of power 300 xenon lamp under conditions of the nm of wavelength >=420 sub-irradiation
Dissipating has Bi2MoO6The aqueous solution, light application time is 1-4 hours, that is, methanol and ethanol is prepared.
The technical advantages of the present invention are that：
（1）The addition and control the hydro-thermal reaction time for adjusting polyvinylpyrrolidone can obtain having compared with Large ratio surface
Long-pending floriform appearance Bi2MoO6, this causes catalyst to have more rich active site, and to CO2There is stronger absorption
Ability, be advantageous to the progress of light-catalyzed reaction；
（2）Special crystal structure has stronger absorption to visible ray, and CO is reduced in visible light catalytic2Prepare methanol and second
There is higher yield in terms of alcohol, so as to realize CO2Effective utilization and recycling, while promote CO2Emission reduction；
（3）The present invention method can implement under visible optical drive and normal pressure, take it is short, cost is low, equipment is simply easy
Operation, and photochemical catalyst can be by filtering recycling, in CO2It is effective using with have in terms of recycling it is important potential
Using.
Brief description of the drawings
Fig. 1 be polyvinylpyrrolidone addition be 0.3g, the hydro-thermal reaction time be obtained Bi under 24 hs2MoO6
XRD.
Fig. 2 be polyvinylpyrrolidone addition be 0.3g, the hydro-thermal reaction time be obtained Bi under 24 hs2MoO6
UV-vis abosrption spectrograms.
Fig. 3 be polyvinylpyrrolidone addition be 0.3g, the hydro-thermal reaction time be obtained Bi under 24 hs2MoO6
SEM figure.
Fig. 4 be polyvinylpyrrolidone addition be 0.3g, the hydro-thermal reaction time be obtained Bi under 24 hs2MoO6
TEM figure.
Embodiment
Embodiment of the present invention and beneficial effect are described in detail below in conjunction with specific embodiment, to help reader to understand
The technical characteristic of the present invention and caused unexpected effect, but any limit can not be formed to the practical range of the present invention
It is fixed.
Embodiment 1
The present embodiment is floriform appearance Bi2MoO6Preparation method, mainly comprise the following steps：
Five nitric hydrate bismuths are weighed respectively（1.94 g）, sodium molybdate（0.484 g）Divide with the g of polyvinylpyrrolidone 0.3
The M of 20 mL 1 HNO is not dissolved in3In solution, the min of magnetic agitation 30, above-mentioned three kinds of solution is mixed, it is anti-to be transferred to 100 mL
Answer in kettle, 180oC maintains 24 h, and question response is cooled to room temperature after terminating；Solid after hydro-thermal reaction is first washed with deionized
To neutrality, the solid portion obtained after centrifugal filtration is 80oTaken out after drying 8 h in C baking oven, that is, obtain floriform appearance
Bi2MoO6Catalyst.
Embodiment 2
The present embodiment is prepared Bi under different condition2MoO6The performance evaluation of photochemical catalyst.
Visible light catalytic reduces CO2The reaction for preparing hydrocarbon is carried out in homemade seal quartz reactor,
Reactor carries cooling system, and temperature control is 4oC is with maintenance reaction temperature.50 mL ultra-pure waters and 50 are added in the reactor
mg Bi2MoO6Photochemical catalyst, CO is continuously passed through after air in reactor is pumped230min (flow velocity is 100 mL/min)
Obtain the CO of saturation2Solution, stable CO2Flow（50 mL/min）, magnetic agitation, open 300 W xenon lamp lamp sources, wavelength >=420
Nm, reaction stop illumination, after liquid product centrifuges, use gas chromatographic detection after 4 hours.Synthesis obtains under different condition
Bi2MoO6Photocatalysis performance is as shown in the table：
Embodiment 3
With embodiment 2, use polyvinylpyrrolidone addition for 0.3g, the hydro-thermal reaction time be under 24 hs it is made
It is photochemical catalyst to obtain Bi2MoO6, and light application time is respectively 1 and 3 hour, and photocatalysis performance is as shown in the table：
| Light application time（Hour） | Methanol yield（μmol/g-Cat） | Alcohol yied（μmol/g-Cat） |
| 1 | 10.1 | 9.8 |
| 3 | 20.8 | 17.5 |
Above example can prove, the Bi of floriform appearance involved in the present invention2MoO6Material reduces in visible light catalytic
CO2Prepare and higher photocatalytic activity is shown in the reaction of methanol and ethanol, this shows that invention achieves set invention mesh
's.
Claims (2)
- A kind of 1. flower-shaped Bi2MoO6In photo catalytic reduction CO2In application, it is characterised in that：The Bi of the floriform appearance of synthesis2MoO6 Photocatalyst material, by the CO in aqueous medium under visible light conditions2Photo catalytic reduction is methanol and ethanol；The flower-shaped Bi2MoO6It is made using following steps：（1）By bismuth nitrate, sodium molybdate, polyvinylpyrrolidone are dissolved separately in the HNO that isometric concentration is 1M3In solution；Its In, nitric acid bi concns are 0.2M, and molybdic acid na concn is 0.1M, and the addition of polyvinylpyrrolidone is 0.05-0.4g, in mixing State three kinds of solution and be transferred in autoclave, 180oHydro-thermal reaction 24-36h under the conditions of C；（2）Solid by filtration after hydro-thermal reaction is washed with deionized to neutrality after collecting, 80o8h is dried under the conditions of C, Obtain Bi2MoO6Catalyst.
- 2. flower-shaped Bi according to claim 12MoO6In photo catalytic reduction CO2In application, it is characterised in that：Photocatalysis Reduce CO2Reaction condition be：By 50mgBi2MoO6It is added to 50mL water in quartz reactor, lasting stirring, reactor is put In 4oIn C water-bath, 100mL/minCO is continuously passed through after air in reactor is pumped2After 30min, stable CO2Flow is 50mL/min, irradiated with power 300W xenon lamp under conditions of wavelength >=420nm and be dispersed with Bi2MoO6The aqueous solution, during illumination Between be 1-4 hours, that is, methanol and ethanol is prepared.
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| CN105709718B (en) * | 2016-01-22 | 2018-08-24 | 武汉工程大学 | A kind of preparation method of bismuth molybdate nanometer chip |
| CN107715865A (en) * | 2017-09-22 | 2018-02-23 | 浙江海洋大学 | A kind of Bi2MoO6The preparation method of/mussel shell composite micro-nano rice catalysis material |
| CN108097236B (en) * | 2017-12-07 | 2021-05-18 | 浙江海洋大学 | Biological photocatalyst for degrading phenol in industrial wastewater and preparation method thereof |
| CN113275003B (en) * | 2021-05-17 | 2023-01-06 | 南昌航空大学 | Molybdenum dioxide/bismuth photocatalyst and preparation method and application thereof |
| CN114939406B (en) * | 2022-03-24 | 2024-01-30 | 淮北师范大学 | Bi2MoO6 photocatalyst and preparation method and application thereof |
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| JPS5622636A (en) * | 1979-07-26 | 1981-03-03 | Natl Inst For Res In Inorg Mater | Synthesizing method for koechlinite type bi2moo6 |
| CN102923779B (en) * | 2012-11-14 | 2014-04-16 | 陕西科技大学 | Preparation method of flower-shaped spherical Bi2MoO6 microcrystal |
| CN104478656B (en) * | 2014-11-26 | 2016-02-10 | 广西大学 | A kind of method of carbon dioxide reduction |
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Non-Patent Citations (3)
| Title |
|---|
| Bi2MoO6粉体的制备工艺及性能研究;张婷;《中国优秀硕士学位论文全文数据库(工程科技I辑)》;20131215(第S2期);论文第14页最后1段 * |
| Photocatalytic reduction of CO2 into methanol and ethanol over conducting polymers modified Bi2WO6 microspheres under visible light;Weili Dai,et al;《Applied Surface Science》;20150811;第356卷;文章第175页2.3节，第177页3.5节，第178页Fig.9、Fig.10 * |
| γ-Bi2MoO6 nanoplates: Surfactant-assisted hydrothermal synthesis and optical properties;Chao Xu,et al;《Ceramics International》;20081209;第35卷(第5期);文章摘要，第2099页第2节，第2100页右栏第2段、Fig.2 * |
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