CN105879856A - Preparation method of carbon quantum dot/bismuth molybdate nano-sheet composite photocatalytic material - Google Patents
Preparation method of carbon quantum dot/bismuth molybdate nano-sheet composite photocatalytic material Download PDFInfo
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- CN105879856A CN105879856A CN201610344339.2A CN201610344339A CN105879856A CN 105879856 A CN105879856 A CN 105879856A CN 201610344339 A CN201610344339 A CN 201610344339A CN 105879856 A CN105879856 A CN 105879856A
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
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- B01J35/39—Photocatalytic properties
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts 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
- B01J23/24—Chromium, molybdenum or tungsten
- B01J23/31—Chromium, molybdenum or tungsten combined with bismuth
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Abstract
The invention discloses a preparation method of a carbon quantum dot/bismuth molybdate nano-sheet composite photocatalytic material. The carbon quantum dot/bismuth molybdate nano-sheet composite photocatalytic material is mainly prepared from glucose, bismuth acetate and ammonium molybdate through adopting a method of hydrothermal synthesis and calcining. The prepared material is subjected to a photocatalytic performance test by utilizing simulated sunlight and the excellent photocatalytic performances of the material are proved through degrading a non-biodegradable organic pollutant Rhodamine B. In view of a composite material, bismuth molybdate and carbon quantum dots are compounded together to prepare the composite photocatalytic material; and the material has relatively high photocatalytic performances, can stably degrade non-biodegradable toxic and organic pollutants including the Rhodamine B, methyl orange and the like under the simulated sunlight and has a wide application prospect in the aspect of environment protection.
Description
Technical field
The invention belongs to optic catalytic composite material preparation field, be specifically related to the preparation method of carbon quantum dot/bismuth molybdate nanometer sheet composite photocatalyst material.
Background technology
Nowadays, environmental pollution and energy shortage have become as the main obstruction of human social.Air pollutants and a large amount of discharges of water pollutant, the healthy existence of the mankind in serious threat, is more particularly difficult to the organic pollution being biodegradable, is difficult to be degraded in these pollutant emissions to environment, can be progressively enriched with in vivo, eventually become the Health Killer of the mankind.Therefore, the material studying novel effective degradation of contaminant becomes the key subjects that relevant academia divination by means of the milfoil is to be solved.
Bi2MoO6(bismuth molybdate) is a kind of well catalysis material, and it is under visible light, it is possible to rhodamine B degradation, methyl orange, methylene blue etc. are difficult to the toxic organic pollutants being biodegradable well.And bismuth molybdate has the environmental protection characteristic that entrance is nontoxic, the field that water processes therefore can be used in.Under the irradiation of visible ray, the electronics in bismuth molybdate valence band is excited on conduction band be formed electron-hole pair, causes reduction and oxidation reaction respectively.
Carbon quantum dot small-sized, can absorb visible ray, and send the wavelength short-wavelength light at 325-425nm, thus excites bismuth molybdate to form electron hole pair.Oxidant in electron hole pair and solution or reducing agent react generation living radical, thus degradating organic dye molecule.The more important thing is the carbon quantum dot surface at bismuth molybdate, the electronics in bismuth molybdate conduction band can be received, promote separation of charge, thus stop the compound of electric charge.Electronics can transmit along the conduction band network of carbon quantum dot, thus promotes the hole life of bismuth molybdate to extend the catalysis activity improving catalyst.Carbon quantum dot has wide absorbing band, chemical stability, luminescence generated by light, upper conversion and down-conversion fluorescent, accepts electronics and provide the character of electronics, and environmental sound.
A kind of aspect of design is widely used.
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of novel nano composite photocatalytic material, according to Bi2MoO6Both are combined by characteristic respective with carbon quantum dot, eliminate the organic pollution being difficult to be biodegradable and realize effectively degraded, eliminate organic pollution and be progressively enriched with in vivo, in order to solve the health problem of environmental conservation and the mankind.
The present invention is achieved through the following technical solutions above-mentioned purpose.The preparation method of carbon quantum dot/bismuth molybdate nanometer sheet composite photocatalyst material, preparation process is as follows:
Step one, the synthesis of bismuth molybdate:
1) accurately weigh bismuth acetate and two kinds of solids of Ammonium Molybdate Tetrahydrate, above two solid is dissolved in deionized water, uses magnetic stirrer 30min；
2) urea is joined in ethanol, after dissolving, joins above-mentioned steps 1) solution in；
3) by above-mentioned steps 2) mixture that formed through 150W supersound process 10min, form uniform solution；
4) by above-mentioned steps 3) solution be transferred in reactor, and be maintained under 160 DEG C of temperature conditionss reaction 10h；
5) after having reacted, form bismuth molybdate, bismuth molybdate is centrifuged under the centrifugal condition that rotating speed is 11000r/min 10min and collects precipitation, then wash twice respectively with deionized water and ethanol, the product washed is put in baking oven, 60 DEG C of temperature is dried 6h, forms bismuth molybdate product；
6) dried bismuth molybdate product is put into agate mortar grinds standby；
The synthesis of step 2, carbon quantum dot/bismuth molybdate nanometer sheet composite photocatalyst material:
1) weigh glucose and dissolve with deionized water, adding in the bismuth molybdate product that described step one is synthesized, forming mixture；
2) agitated 20min, after ultrasonic disperse 10min, then by above-mentioned steps 1) mixture that produces transfers in reactor, reacts 6h under 160 DEG C of hydrothermal conditions；
3) by above-mentioned steps 2) react rear products therefrom centrifugal 10min collect precipitation under the centrifugal condition that rotating speed is 11000r/min, then wash twice respectively with deionized water and ethanol, the product washed is put in baking oven, 60 DEG C of temperature are dried 6h；
4) putting in Muffle furnace by dried product, calcine 4h under conditions of 300 DEG C of temperature, heating rate is 2 DEG C/min；
5) product after calcining is put into after grinding in agate mortar and is stored for future use, and completes preparation.
Further, the described quality weighing glucose is respectively 0.05g, 0.1g, 0.15g.
Further, described reactor is 50ml inner liner polytetrafluoroethylene stainless steel cauldron.
The present invention is from the angle of composite; bismuth molybdate and carbon quantum dot are combined with each other; the composite photocatalyst material prepared; this material light catalysis activity is higher; rhodamine B degradation and methyl orange etc. can be stablized under simulated solar irradiation and be difficult to biodegradable toxic organic pollutant, in terms of environmental conservation, have the most wide application prospect.
Accompanying drawing explanation
Fig. 1 is that the present invention weighs the product that 40mg embodiment 1-3 prepares and degrades under simulated solar irradiation the degradation curve of rhodamine B solution that 40ml concentration is 10PPm.
Fig. 2 is the X-ray diffraction analysis figure of the product that embodiment of the present invention 1-3 prepares.
Fig. 3 is the tem analysis figure of the product that the embodiment of the present invention 2 prepares.
Detailed description of the invention
The invention will be further described with embodiment below in conjunction with the accompanying drawings.
Embodiment 1 :A kind of preparation method of carbon quantum dot/bismuth molybdate nanometer sheet composite photocatalyst material, preparation process is as follows:
Step one, the synthesis of bismuth molybdate:
1) accurately weighing bismuth acetate is 0.3861g and Ammonium Molybdate Tetrahydrate is 0.08828g, is dissolved in 20ml deionized water by the solid of both materials, uses magnetic stirrer 30min.
2) 0.3g urea is joined in 20ml ethanol, join after dissolving in solution produced by above-mentioned magnetic stirrer.
3) by step 2) mixture that produces is maintained at 150W supersound process 10 min, in order to form uniform solution.
4) solution that step 3) is formed is transferred in 50ml inner liner polytetrafluoroethylene stainless steel cauldron, is maintained at reaction 10h under the conditions of temperature is 160 DEG C.
5) after having reacted, the product centrifugal 10min under the centrifugal condition that rotating speed is 11000r/min that will be formed, regather precipitation, then wash twice respectively with deionized water and ethanol, the product washed is put in baking oven, under the conditions of temperature is 60 DEG C, is dried 6h, forms bismuth molybdate product.
6) dried bismuth molybdate product is put into agate mortar grinds standby.
The synthesis of step 2, carbon quantum dot/bismuth molybdate nanometer sheet composite photocatalyst material:
1) weigh 0.05g glucose 40ml deionized water dissolving, add in the bismuth molybdate product that 0.1g step one is synthesized, form mixture.
2) agitated 20min, after ultrasonic disperse 10min, then by above-mentioned steps 1) mixture that produces transfers in the reactor of 50ml, reacts 6h under 160 DEG C of hydrothermal conditions.
3), after having reacted, products therefrom it is centrifuged under the centrifugal condition that rotating speed is 11000r/min 10min and collects precipitation, then washing twice respectively with deionized water and ethanol, the product washed is put in baking oven, under the conditions of temperature is 60 DEG C, being dried 6h.
4) putting in Muffle furnace by dried product, calcine 4h under conditions of 300 DEG C of temperature, heating rate is 2 DEG C/min.
5) product after calcining is put into after grinding in agate mortar and is stored for future use, and completes preparation.
The product of gained is A0.1BO.O5.Taking this product of 40mg rhodamine B solution for the 40ml 10PPm that degrades under simulated solar irradiation, after 60min, degradation rate reaches 99.8%.
Embodiment 2:A kind of preparation method of carbon quantum dot/bismuth molybdate nanometer sheet composite photocatalyst material, preparation process is as follows:
Step one, same as in Example 1.
The synthesis of step 2, carbon quantum dot/bismuth molybdate nanometer sheet composite photocatalyst material:
1) weigh 0.1g glucose 40ml deionized water dissolving, add in the bismuth molybdate product being synthesized in 0.1g step one, form mixture.
2) agitated 20min, after ultrasonic disperse 10min, transfers to mixture, in the reactor of 50ml, react 6 h under 160 DEG C of hydrothermal conditions.
3), after having reacted, products therefrom it is centrifuged under the centrifugal condition that rotating speed is 11000r/min 10min and collects precipitation, then washing twice respectively with deionized water and ethanol, the product washed is put in baking oven, under the conditions of temperature is 60 DEG C, being dried 6h.
4) putting in Muffle furnace by dried product, calcine 4h under conditions of 300 DEG C of temperature, heating rate is 2 DEG C/min.
5) product after calcining is put into after grinding in agate mortar and is stored for future use, and completes preparation.
The product of gained is A0.1BO.1.Taking this product of 40mg rhodamine B solution for the 40ml 10PPm that degrades under simulated solar irradiation, after 60min, degradation rate reaches 98.34%.
Embodiment 3:A kind of preparation method of carbon quantum dot/bismuth molybdate nanometer sheet composite photocatalyst material, preparation process is as follows:
Step one, same as in Example 1.
The synthesis of step 2, carbon quantum dot/bismuth molybdate nanometer sheet composite photocatalyst material:
1) weigh 0.15g glucose 40ml deionized water dissolving, add in the bismuth molybdate product being synthesized in 0.1g step one, form mixture.
2) agitated 20min, after ultrasonic disperse 10min, transfers in the reactor of 50ml by mixture, at 160 DEG C of hydro-thermal reaction 6 h.
3), after having reacted, products therefrom it is centrifuged under the centrifugal condition that rotating speed is 11000r/min 10min and collects precipitation, then washing twice respectively with deionized water and ethanol, the product washed is put in baking oven, under the conditions of temperature is 60 DEG C, being dried 6h.
4) putting in Muffle furnace by dried product, calcine 4h under conditions of 300 DEG C of temperature, heating rate is 2 DEG C/min.
5) product after calcining is put into after grinding in agate mortar and is stored for future use, and completes preparation.
The product of gained is A0.1BO.15.Taking this product of 40mg rhodamine B solution for the 40ml 10PPm that degrades under simulated solar irradiation, after 60min, degradation rate reaches 95.7%.
Seeing Fig. 1, the complex AXBY that embodiment 1-3 prepares represents, A, B represent bismuth molybdate and glucose respectively.X, Y represent the quality of each of which respectively.
In embodiment 1-3, the product 40mg of gained compares for the degradation effect of the rhodamine B solution of the 40ml 10PPm that degrades under simulated solar irradiation, refers to accompanying drawing 1.From accompanying drawing 1, under simulated solar irradiation, the when that glucose addition being 0.05g, degradation effect is best, and along with load capacity continues to increase, degradation effect is worse and worse.
In embodiment 1-3, the X-ray diffraction analysis figure of products therefrom refers to accompanying drawing 2.By by accompanying drawing 2 and standard PDF picture check analysis, product is pure Bi2MoO6(PDF No.72-1524), and the load of carbon quantum dot does not change Bi2MoO6Architectural feature.
By the transmission electron microscope picture of product it can be seen that (see figure 3), more carbon quantum dot is loaded in bismuth molybdate nanometer sheet, the carbon quantum dot that size is less is easily reunited on sheet, and these carbon quantum dot are reunited in bismuth molybdate nanometer sheet, and the carbon quantum dot average-size after reunion is at about 40nm.
Claims (3)
1. the preparation method of carbon quantum dot/bismuth molybdate nanometer sheet composite photocatalyst material, preparation process is as follows:
Step one, the synthesis of bismuth molybdate:
1) accurately weigh bismuth acetate and two kinds of solids of Ammonium Molybdate Tetrahydrate, above two solid is dissolved in deionized water, uses magnetic stirrer 30min；
2) urea is joined in ethanol, after dissolving, joins above-mentioned steps 1) solution in；
3) by above-mentioned steps 2) mixture that formed through 150W supersound process 10min, form uniform solution；
4) by above-mentioned steps 3) solution be transferred in reactor, and be maintained under 160 DEG C of temperature conditionss reaction 10h；
5) after having reacted, form bismuth molybdate, bismuth molybdate is centrifuged under the centrifugal condition that rotating speed is 11000r/min 10min and collects precipitation, then wash twice respectively with deionized water and ethanol, the product washed is put in baking oven, 60 DEG C of temperature is dried 6h, forms bismuth molybdate product；
6) dried bismuth molybdate product is put into agate mortar grinds standby；
The synthesis of step 2, carbon quantum dot/bismuth molybdate nanometer sheet composite photocatalyst material:
1) weigh glucose and dissolve with deionized water, adding the bismuth molybdate product that described step one is synthesized, forming mixture；
2) agitated 20min, after ultrasonic disperse 10min, then by above-mentioned steps 1) mixture that produces transfers in reactor, reacts 6h under 160 DEG C of hydrothermal conditions；
3) by above-mentioned steps 2) react rear products therefrom centrifugal 10min collect precipitation under the centrifugal condition that rotating speed is 11000r/min, then wash twice respectively with deionized water and ethanol, the product washed is put in baking oven, 60 DEG C of temperature are dried 6h；
4) putting in Muffle furnace by dried product, calcine 4h under conditions of 300 DEG C of temperature, heating rate is 2 DEG C/min；
5) product after calcining is put into after grinding in agate mortar and is stored for future use, and completes preparation.
The preparation method of carbon quantum dot the most according to claim 1/bismuth molybdate composite photocatalyst material, it is characterised in that the quality weighing glucose in described step 2 is respectively 0.05g, 0.1g or 0.15g.
The preparation method of carbon quantum dot the most according to claim 1/bismuth molybdate nanometer sheet composite photocatalyst material, it is characterised in that described reactor is 50ml inner liner polytetrafluoroethylene stainless steel cauldron.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106902828A (en) * | 2017-03-14 | 2017-06-30 | 沃邦环保有限公司 | A kind of processing method of acetyl spiramycin antibiotic waste water |
| CN107029725A (en) * | 2017-03-14 | 2017-08-11 | 沃邦环保有限公司 | Carbon quantum dot nickel titanate compound degradation agent of degraded antibiotic and preparation method thereof |
| CN108097236A (en) * | 2017-12-07 | 2018-06-01 | 浙江海洋大学 | Biological photochemical catalyst for phenol in industrial wastewater of degrading and preparation method thereof |
| CN108477213A (en) * | 2018-04-17 | 2018-09-04 | 陕西科技大学 | Nano zine oxide@carbon quantum dot complex antimicrobials and its preparation method and application |
| CN108686705A (en) * | 2018-05-04 | 2018-10-23 | 大连理工大学 | A kind of carbon quantum dot-ZIF-67 absorption-photochemical catalyst and preparation method thereof |
| CN109449424A (en) * | 2018-11-14 | 2019-03-08 | 陕西科技大学 | A kind of compound carbon dots lithium ion battery anode material of cobalt molybdate and preparation method thereof |
| CN109713301A (en) * | 2019-03-04 | 2019-05-03 | 陕西科技大学 | A kind of preparation method of nickel molybdate doping carbon quantum dot lithium ion battery negative material |
| CN110354845A (en) * | 2019-06-28 | 2019-10-22 | 广东工业大学 | A kind of bismuth tungstate photocatalyst and its preparation method and application of carbon nano dot modification |
| CN110893340A (en) * | 2018-09-13 | 2020-03-20 | 江西理工大学 | Preparation method and application of carbon quantum dots and carbon nanofibers modified nanometer bismuth molybdate photocatalyst |
| CN115400387A (en) * | 2022-09-30 | 2022-11-29 | 陕西科技大学 | Degradable agricultural reflective film composite material and preparation method and use method thereof |
| CN116161647A (en) * | 2023-03-15 | 2023-05-26 | 云南师范大学 | Preparation method of sorbic acid carbon quantum dots |
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| CN106902828B (en) * | 2017-03-14 | 2019-11-19 | 沃邦环保有限公司 | A kind of processing method of acetyl spiramycin antibiotic waste water |
| CN107029725A (en) * | 2017-03-14 | 2017-08-11 | 沃邦环保有限公司 | Carbon quantum dot nickel titanate compound degradation agent of degraded antibiotic and preparation method thereof |
| CN106902828A (en) * | 2017-03-14 | 2017-06-30 | 沃邦环保有限公司 | A kind of processing method of acetyl spiramycin antibiotic waste water |
| CN107029725B (en) * | 2017-03-14 | 2019-11-19 | 沃邦环保有限公司 | Carbon quantum dot-nickel titanate compound degradation agent and preparation method thereof of degradation antibiotic |
| CN108097236A (en) * | 2017-12-07 | 2018-06-01 | 浙江海洋大学 | Biological photochemical catalyst for phenol in industrial wastewater of degrading and preparation method thereof |
| CN108097236B (en) * | 2017-12-07 | 2021-05-18 | 浙江海洋大学 | Biophotocatalyst for degrading phenol in industrial wastewater and preparation method thereof |
| CN108477213A (en) * | 2018-04-17 | 2018-09-04 | 陕西科技大学 | Nano zine oxide@carbon quantum dot complex antimicrobials and its preparation method and application |
| CN108686705A (en) * | 2018-05-04 | 2018-10-23 | 大连理工大学 | A kind of carbon quantum dot-ZIF-67 absorption-photochemical catalyst and preparation method thereof |
| CN110893340A (en) * | 2018-09-13 | 2020-03-20 | 江西理工大学 | Preparation method and application of carbon quantum dots and carbon nanofibers modified nanometer bismuth molybdate photocatalyst |
| CN109449424A (en) * | 2018-11-14 | 2019-03-08 | 陕西科技大学 | A kind of compound carbon dots lithium ion battery anode material of cobalt molybdate and preparation method thereof |
| CN109449424B (en) * | 2018-11-14 | 2021-09-28 | 陕西科技大学 | Cobalt molybdate composite carbon dot lithium ion battery anode material and preparation method thereof |
| CN109713301A (en) * | 2019-03-04 | 2019-05-03 | 陕西科技大学 | A kind of preparation method of nickel molybdate doping carbon quantum dot lithium ion battery negative material |
| CN110354845A (en) * | 2019-06-28 | 2019-10-22 | 广东工业大学 | A kind of bismuth tungstate photocatalyst and its preparation method and application of carbon nano dot modification |
| CN115400387A (en) * | 2022-09-30 | 2022-11-29 | 陕西科技大学 | Degradable agricultural reflective film composite material and preparation method and use method thereof |
| CN116161647A (en) * | 2023-03-15 | 2023-05-26 | 云南师范大学 | Preparation method of sorbic acid carbon quantum dots |
| CN116161647B (en) * | 2023-03-15 | 2024-05-14 | 云南师范大学 | A method for preparing sorbic acid carbon quantum dots |
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