CN105381810A - Preparation and applications of silver vanadate composite photocatalysis material - Google Patents

Preparation and applications of silver vanadate composite photocatalysis material Download PDF

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Publication number
CN105381810A
CN105381810A CN201410254922.5A CN201410254922A CN105381810A CN 105381810 A CN105381810 A CN 105381810A CN 201410254922 A CN201410254922 A CN 201410254922A CN 105381810 A CN105381810 A CN 105381810A
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powder
heat treatment
room temperature
distilled water
stirring
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史海峰
周长平
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Jiangnan University
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Jiangnan University
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Abstract

The present invention provides preparation of a silver vanadate composite photocatalysis material. The preparation method comprises: adding 2.5 mmol of an ammonium metavanadate precursor and 0.500 g of P123 to 30 mL of distilled water containing 2 mL of a 1 mol/L nitric acid (HNO3), stirring for 7 h at a room temperature, adding 2.5 mmol of silver nitrate, stirring for 1 h, transferring the obtained solution into an autoclave, carrying out a heat treatment for 24 h at a temperature of 150 DEG C, cooling the obtained product to a room temperature, grinding to obtain yellow AgVO3 powder, filtering the obtained precipitate, washing respectively with distilled water and acetone, drying for 12 h in an oven with a temperature of 70 DEG C, adding 10 g of melamine into a crucible having a cover, placing into the autoclave, carrying out a heat treatment for 4 h at a temperature of 520 DEG C at a heating rate of 20 DEG C/min, cooling the obtained product to a room temperature, grinding to obtain yellow powder g-C3N4, dissolving the g-C3N4 powder in a methanol solution, carrying out an ultrasonic treatment for 30 min, adding the prepared AgVO3 powder to the suspension, carrying out room temperature stirring for 24 h, collecting the product through centrifugation, washing with distilled water, drying for 24 h in an oven with a temperature of 70 DEG C, and carrying out a heat treatment for 1 h at a temperature of 250 DEG C in a muffle furnace.

Description

A kind of preparations and applicatio of silver vanadate composite photocatalyst material
Technical field
The present invention relates to composite semiconductor material Synthesis and applications field, especially a kind of preparations and applicatio of silver vanadate composite photocatalyst material.
Background technology
Along with room air pollution is more and more serious, many researchers start photocatalysis technology to be applied on depollution of environment field.Compared with traditional processing method, phase photo catalytic oxidation processes degrading organic pollutants has that energy consumption is low, easy and simple to handle, reaction condition is gentle and the advantage such as secondary pollution is less.No matter be that photochemical catalyzing prepares clean hydrogen energy source or photocatalysis degradation organic contaminant, its core technology is all the catalysis material that exploitation has high conversion quantum efficiency.Although, TiO 2main catalysis material, but due to TiO 2optical band gap be 3.2eV, only have and just have response to the light lower than 400nm wavelength, namely only to UV Absorption, visible ray is not absorbed.So solar energy utilization ratio is very low.Therefore, find the catalysis material with visible light-responded high conversion quantum efficiency, become the study hotspot of current photocatalysis field.
Ag 3vO 4valence band formed by the 4d track of Ag and the 2p orbital hybridization of O, and its conduction band is formed by the 5s track of Ag and the 3d orbital hybridization of V.The valence band structure of hydridization has the energy level more active than the 2p of single O, result in narrower energy gap.And pass through g-C 3n 4compounded g-C 3n 4/ AgVO 3material, further expands the response range to light, becomes the promising visible light responsive photocatalyst of another tool.
Summary of the invention
The object of this invention is to provide a kind of preparation method of silver vanadate composite photocatalyst material.
Technical scheme of the present invention is: a kind of silver vanadate composite photocatalyst material g-C 3n 4/ AgVO 3preparation method.Concrete steps are as follows:
(1) 2.5mmol metavanadic acid ammonia presoma and 0.500gP123 are added 30mL and comprise 2mL1mol/L nitric acid (HNO 3) distilled water in.
(2) stirred at ambient temperature 7h, adds 2.5mmol silver nitrate.
(3) after stirring 1h again, the solution obtained to be transferred in autoclave and at 150 DEG C heat treatment 24h, products therefrom is cooled to room temperature, and grinding can obtain yellow AgVO 3powder.
(4) sediment that obtains after filtering respectively with distilled water and acetone washing, and in the baking oven of 70 DEG C dry 12h.
(5) 10g melamine is put into crucible with cover, be placed in autoclave with 20 DEG C/min heating rate at 520 DEG C of heat treatment 4h, products therefrom is cooled to room temperature, and grinding can obtain yellow g-C 3n 4powder.
(6) by g-C 3n 4powder is dissolved in methanol solution, ultrasonic 30min.
(7) by prepared AgVO 3powder adds above-mentioned suspension, stirring at room temperature 24h.
(8) by product by collected by centrifugation, with distilled water washing, and in the baking oven of 70 DEG C dry 24h.
(9) by product 250 DEG C of heat treatment 1h in Muffle furnace.
Accompanying drawing explanation
Fig. 1 is the electron scanning micrograph of invention compound.
Detailed description of the invention
Detailed description of the invention one
2.5mmol metavanadic acid ammonia presoma and 0.500gP123 are added 30mL and comprises 2mL1mol/L nitric acid (HNO 3) distilled water in.Stirred at ambient temperature 7h, adds 2.5mmol silver nitrate.After stirring 1h again, the solution obtained to be transferred in autoclave and at 150 DEG C heat treatment 24h, products therefrom is cooled to room temperature, and grinding can obtain yellow AgVO 3powder.The sediment that obtained after filtering respectively with distilled water and acetone washing, and in the baking oven of 70 DEG C dry 12h.10g melamine is put into crucible with cover, and be placed in autoclave with 20 DEG C/min heating rate at 520 DEG C of heat treatment 4h, products therefrom is cooled to room temperature, and grinding can obtain yellow g-C 3n 4powder.By g-C 3n 4powder is dissolved in methanol solution, and ultrasonic 30min, by 0.04gAgVO 3nano wire powder joins in above-mentioned suspension, and constantly stirs 24 hours.By products therefrom by collected by centrifugation, and with distilled water washing, and at 70 DEG C, baking oven dry 24 hours.Finally, by product 250 DEG C of heat treatment 1 hour in Muffle furnace.Obtain the sample of 10%.
Detailed description of the invention two
Identical with mode one, unlike, by 0.08gAgVO 3nano wire powder joins in above-mentioned suspension, and constantly stirs 24 hours.By products therefrom by collected by centrifugation, and with distilled water washing, and at 70 DEG C, baking oven dry 24 hours.Finally, by product 250 DEG C of heat treatment 1 hour in Muffle furnace.Obtain the sample of 20%.
Detailed description of the invention two
Identical with mode one, unlike, by 0.12gAgVO 3nano wire powder joins in above-mentioned suspension, and constantly stirs 24 hours.By products therefrom by collected by centrifugation, and with distilled water washing, and at 70 DEG C, baking oven dry 24 hours.Finally, by product 250 DEG C of heat treatment 1 hour in Muffle furnace.Obtain the sample of 30%.

Claims (7)

1. a silver vanadate (Ag 3vO 4) preparation method of nano wire catalysis material, comprise following step:
(1) 2.5mmol metavanadic acid ammonia presoma and 0.500gP123 are added 30mL and comprise 2mL1mol/L nitric acid (HNO 3) distilled water in.
(2) stirred at ambient temperature 7h, adds 2.5mmol silver nitrate.
(3) after stirring 1h again, the solution obtained to be transferred in autoclave and at 150 DEG C heat treatment 24h, products therefrom is cooled to room temperature, and grinding can obtain yellow AgVO 3powder.
(4) sediment that obtains after filtering respectively with distilled water and acetone washing, and in the baking oven of 70 DEG C dry 12h.
(5) 10g melamine is put into crucible with cover, be placed in autoclave with 20 DEG C/min heating rate at 520 DEG C of heat treatment 4h, products therefrom is cooled to room temperature, and grinding can obtain yellow g-C 3n 4powder.
(6) by g-C 3n 4powder is dissolved in methanol solution, ultrasonic 30min.
(7) by prepared AgVO 3powder adds above-mentioned suspension, stirring at room temperature 24h.
(8) by product by collected by centrifugation, with distilled water washing, and in the baking oven of 70 DEG C dry 24h.
(9) by product 250 DEG C of heat treatment 1h in Muffle furnace.
2. the method for claim 1, it is characterized in that prepare silver vanadate used reactant be vanadic acid ammonia (NH 4vO 4) and silver nitrate (AgNO 3).And the molal quantity that ammonium vanadate, silver nitrate use is according to molecular formula Ag 3vO 4mol ratio.
3. the method for claim 1, is characterized in that stirred at ambient temperature 7h, adds 2.5mmol silver nitrate.
4. the method for claim 1, is characterized in that stirring after 1h, the solution obtained to transfer in autoclave and at 150 DEG C heat treatment 24h.
5. the method for claim 1, is characterized in that obtained sediment respectively with distilled water and acetone washing after filtering, and in the baking oven of 70 DEG C dry 12h.
6. the method for claim 1, is characterized in that g-C 3n 4powder is dissolved in methanol solution, and ultrasonic 30min, by AgVO 3powder adds suspension, stirring at room temperature 24h.
7. the method for claim 1, is characterized in that product 250 DEG C of heat treatment 1h in Muffle furnace.
CN201410254922.5A 2014-09-09 2014-09-09 Preparation and applications of silver vanadate composite photocatalysis material Pending CN105381810A (en)

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106268900A (en) * 2016-07-21 2017-01-04 吉林师范大学 A kind of g C3n4quantum dot sensitized AgVO3the preparation method of nano wire
CN106492865A (en) * 2016-09-06 2017-03-15 景德镇陶瓷大学 A kind of method that 2 composites of C3N4/CaTi2O4 (OH) are prepared using solvent-thermal method
CN108262054A (en) * 2018-03-06 2018-07-10 内蒙古大学 A kind of preparation method of silver vanadate/nitride porous carbon heterojunction composite photocatalyst
CN108479831A (en) * 2018-02-02 2018-09-04 常州大学 A kind of preparation method of photocatalytic degradation Microcystin composite material and application
CN108855191A (en) * 2018-07-12 2018-11-23 苏州大学 Visible light-responded hybrid aerogel and preparation method thereof and the application in exhaust-gas treatment
CN109225304A (en) * 2018-10-25 2019-01-18 聊城大学 A kind of visible light-responded Ag4V2O7/g-C3N4The preparation method of catalysis material
CN109765225A (en) * 2019-01-30 2019-05-17 扬州工业职业技术学院 A kind of g-C of load silver ion3N4Nano material and its application in the detection of kitchen abandoned oil
CN109999876A (en) * 2019-03-28 2019-07-12 江苏大学 AgVO3 QDs/rGO/g-C3N4The preparation method and its usage of-pDA@RC photocatalysis membrana
CN112642456A (en) * 2020-12-11 2021-04-13 内蒙古科技大学包头师范学院 Preparation method of composite photocatalyst
CN113731410A (en) * 2021-09-24 2021-12-03 太原理工大学 Ag2V4O11/g-C3N4Preparation method and application of composite photocatalyst

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102580736A (en) * 2012-02-09 2012-07-18 江苏大学 Grapheme / silver vanadium oxide nanometer composite visible light catalyst and preparation method thereof
CN103506116A (en) * 2012-06-29 2014-01-15 江南大学 Preparation and application of visible-light photocatalytic material of silver vanadate nanotube

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102580736A (en) * 2012-02-09 2012-07-18 江苏大学 Grapheme / silver vanadium oxide nanometer composite visible light catalyst and preparation method thereof
CN103506116A (en) * 2012-06-29 2014-01-15 江南大学 Preparation and application of visible-light photocatalytic material of silver vanadate nanotube

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106268900A (en) * 2016-07-21 2017-01-04 吉林师范大学 A kind of g C3n4quantum dot sensitized AgVO3the preparation method of nano wire
CN106492865A (en) * 2016-09-06 2017-03-15 景德镇陶瓷大学 A kind of method that 2 composites of C3N4/CaTi2O4 (OH) are prepared using solvent-thermal method
CN108479831A (en) * 2018-02-02 2018-09-04 常州大学 A kind of preparation method of photocatalytic degradation Microcystin composite material and application
CN108262054A (en) * 2018-03-06 2018-07-10 内蒙古大学 A kind of preparation method of silver vanadate/nitride porous carbon heterojunction composite photocatalyst
CN108855191A (en) * 2018-07-12 2018-11-23 苏州大学 Visible light-responded hybrid aerogel and preparation method thereof and the application in exhaust-gas treatment
CN109225304B (en) * 2018-10-25 2021-06-01 聊城大学 Ag with visible light response4V2O7/g-C3N4Preparation method of photocatalytic material
CN109225304A (en) * 2018-10-25 2019-01-18 聊城大学 A kind of visible light-responded Ag4V2O7/g-C3N4The preparation method of catalysis material
CN109765225A (en) * 2019-01-30 2019-05-17 扬州工业职业技术学院 A kind of g-C of load silver ion3N4Nano material and its application in the detection of kitchen abandoned oil
CN109999876A (en) * 2019-03-28 2019-07-12 江苏大学 AgVO3 QDs/rGO/g-C3N4The preparation method and its usage of-pDA@RC photocatalysis membrana
CN109999876B (en) * 2019-03-28 2021-06-22 江苏大学 AgVO3 QDs/rGO/g-C3N4Preparation method and application of (E) -pDA @ RC photocatalytic film
CN112642456A (en) * 2020-12-11 2021-04-13 内蒙古科技大学包头师范学院 Preparation method of composite photocatalyst
CN113731410A (en) * 2021-09-24 2021-12-03 太原理工大学 Ag2V4O11/g-C3N4Preparation method and application of composite photocatalyst
CN113731410B (en) * 2021-09-24 2024-03-15 太原理工大学 Ag (silver) alloy 2 V 4 O 11 /g-C 3 N 4 Preparation method and application of composite photocatalyst

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Application publication date: 20160309