CN107746077A - A kind of preparation method of flower ball-shaped silver vanadate - Google Patents
A kind of preparation method of flower ball-shaped silver vanadate Download PDFInfo
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- CN107746077A CN107746077A CN201710957597.2A CN201710957597A CN107746077A CN 107746077 A CN107746077 A CN 107746077A CN 201710957597 A CN201710957597 A CN 201710957597A CN 107746077 A CN107746077 A CN 107746077A
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- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G31/00—Compounds of vanadium
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- 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
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2004/30—Particle morphology extending in three dimensions
- C01P2004/32—Spheres
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- 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
- C02F2101/34—Organic compounds containing oxygen
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- 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
- C02F2101/36—Organic compounds containing halogen
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- 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
- C02F2101/38—Organic compounds containing nitrogen
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- 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
- C02F2101/40—Organic compounds containing sulfur
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- 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 a kind of preparation field of conductor photocatalysis material, more particularly to a kind of preparation method of flower ball-shaped silver vanadate, the invention provides a kind of without directed agents and the preparation method for preparing high-activity photocatalyst of acidity regulator, specifically include preparation silver salt solution, prepare vanadic salts ethanol solution, the polarity of appropriate acetone change reaction system will be added after both above-mentioned be well mixed, reacted by homogeneous reactor can obtain flower ball-shaped silver vanadate afterwards；The advantages of method provided by the invention has that technique is simple, cost is relatively low, energy consumption is minimum, product purity is high, and photocatalytic activity is good.
Description
Technical field
The application is related to a kind of preparation field of novel semiconductor material, and in particular to a kind of preparation of flower ball-shaped silver vanadate
Method.
Background technology
In recent years, as the horizontal of human being's production life improves constantly, continue to develop, in the situation that earth resource is limited
Under, the contradiction between material requisite and the limited resource especially energy that the mankind increasingly constantly expand is increasing, meanwhile, by
Development level difference in each department is larger, the utilization rate of resource is also not quite similar, these directly results in the existence of the mankind
Environment more deteriorates, on the other hand, rescue, protection, improvement environment are as the common recognition in the whole world.
The protection of water resource is an extremely important content in environmental protection, relative to traditional water technology, such as
UF membrane, absorption etc., there is great advantage using light-catalysed mode, it is light-catalysed according to the hole theory of classics, use
All organic matters for being difficult to separate, adsorbing can be almost decomposed into water and carbon dioxide by technology, and be made in this way
Simple and easy, the problem of cost is extremely low, non-secondary pollution.
Silver vanadate is as a kind of new semiconductor light-catalyst, due to its excellent photocatalysis performance, it has also become vast
Researcher falls over each other the hot subject of research.Huang et al. [Crystalline phase and photocatalytic
activities of hydrothermal synthesis Ag3VO4 and Ag4V2O7 under visible light
irradiation, Applied Catalysis A:General, 358 (2009), 164-172] disclose a kind of use
Hydro-thermal method prepares the method for silver vanadate, and has synthesized using CTAB as directed agents the silver vanadate of different-shape, by regulating and controlling water
The thermal response time and the silver vanadate of three kinds of crystalline phases is obtained using surfactant, Ag4V2O7, α-Ag3VO4 and both mixing
Phase；Its photolysis efficiency to isopropanol and benzene is substantially better than P25, and they think that being substantially improved for photocatalytic activity is primarily due to
Substantial amounts of hydroxyl group be present in the presence of mixed phase and surface, in addition, the hydro-thermal reaction time also have to photocatalysis effect it is very big
Influence.Chinese patent CN106191903A discloses a kind of preparation method of silver vanadate photochemical catalyst, uses the method system of electrolysis
For the silver vanadate of different-shape, specifically using silver strip as anode, using inert electrode as negative electrode, with sodium metavanadate and sodium nitrate water
Solution does anolyte, using hydrochloric acid solution or sodium chloride solution as catholyte, in the two-compartment cell that cation is film, uses
The mode of constant-current electrolysis, different structure and the vanadium of particle size are prepared by control electric current density, concentration of electrolyte and temperature
Sour silver.Chinese patent CN106179343A discloses a kind of method of Fast back-projection algorithm square Ag3VO4 photochemical catalysts, using heavy
Silver nitrate, is specifically added in citric acid and vanadic anhydride by shallow lake auxiliary microwave hydrothermal method method synthesis, after being well mixed, uses
Ammoniacal liquor adjusts pH value, then suitable temperature and hydro-thermal reaction is carried out under the time again, you can it is uniform to obtain a kind of composition, purity compared with
Height, there is the material of large specific surface area and photocatalytic activity.
The content of the invention
The present invention be directed to above-mentioned the deficiencies in the prior art, it is proposed that one kind without using materials such as directed agents, acidity regulators,
And the preparation method with higher active flower ball-shaped vanadic acid Argent grain is obtained, this method has processing step simple, and energy consumption is low,
The characteristics of product thing is mutually single, and the photocatalysis performance of product is good.
To realize above-mentioned experiment purpose, the present invention is to carry out by the following technical solutions, and the technical scheme is entered below
Row is discussed in detail.
A kind of preparation method of flower ball-shaped silver vanadate, is comprised the following steps that：
（1）Weigh 0.2-5.0g silver salt, solvent made using deionized water, under conditions of shading, be stirred continuously be configured to it is dense
Spend the silver salt solution for 0.02-0.25g/ml；
（2）0.5-10.0g vanadic salts is weighed, solvent is made using absolute ethyl alcohol, it is 0.1-1g/ml's to be stirred continuously and be configured to concentration
Vanadic salts ethanol solution；
（3）It is under conditions of being stirred continuously, the above-mentioned silver salt solution prepared and vanadic salts ethanol solution is same by proper ratio
When add homogeneous reaction kettle in, after certain time, then appropriate acetone soln is added into mixed liquor, continue stir 2-5 minutes；
（4）It is put into homogeneous reactor and is reacted after above-mentioned homogeneous reaction kettle is sealed, after certain time, question response terminates,
Room temperature is naturally cooled to, reactor is taken out, filtration product, washing, flower ball-shaped silver vanadate is both obtained after drying.
In the present invention, the step（1）In silver salt to include silver nitrate, silver sulfate, silver carbonate, silver perchlorate etc. water-soluble
One or more of combinations in property silver salt.
Step of the present invention（2）In vanadic salts refer to ammonium vanadate, vanadic anhydride, sodium metavanadate, potassium metavanadate, dichloro vanadyl
Etc. one or more of combinations in the vanadic salts for dissolving in ethanol.
Step of the present invention（3）In silver salt solution and vanadic salts ethanol solution refer to that the volume ratio of the two is by proper ratio
1：（0.5-1）, appropriate acetone soln refers to that volume is 0.5-3ml.
Step of the present invention（4）In reaction time be 4-12 hours, reaction temperature is 120-180 DEG C.
Beneficial effects of the present invention：
（1）The invention provides a kind of system for the flower ball-shaped silver vanadate that preparation method is simple, product purity is high, photocatalytic activity is good
Preparation Method；
（2）During the present invention prepares flower ball-shaped silver vanadate, it is not necessary to additionally introduce directed agents or acidity regulator；
（3）The invention introduces the larger polar solvent of this activity of acetone, due to the solvent activity difference in system
Larger, this nucleating growth process to crystal grain causes strong influence, has finally given a kind of vanadic acid ag material of flower ball-shaped；
（4）Flower ball-shaped silver vanadate in the present invention compared with prior art in vanadic acid ag material, there is more excellent photocatalysis
Performance, it can reach more than 98% to the percent of decolourization of methyl orange and rhodamine B.
Brief description of the drawings
The high power stereoscan photograph of flower ball-shaped silver vanadate prepared by Fig. 1 present invention；
The low power stereoscan photograph of flower ball-shaped silver vanadate prepared by Fig. 2 present invention；
Silver vanadate stereoscan photograph prepared by Fig. 3 comparative examples of the present invention.
Embodiment
Present disclosure is further illustrated below by embodiment.It should be noted that specific implementation is real
The scope that example is not intended to limit the invention, under conditions of being contributed without substantial technological content, the routine of those skilled in the art
Conversion be also considered as the present invention can practical range, in the protection domain of application claims.
Embodiment 1
0.2g silver nitrate is weighed, solvent is made using deionized water, under conditions of shading, is stirred continuously and is configured to concentration and is
0.02g/ml silver salt solution；0.5g ammonium vanadate is weighed, solvent is made using absolute ethyl alcohol, is stirred continuously and is configured to concentration and is
0.1g/ml vanadic salts ethanol solution；It is under conditions of being stirred continuously, the above-mentioned silver salt solution prepared and vanadic salts ethanol is molten
Liquid by volume 2：1 adds in homogeneous reaction kettle simultaneously, stir certain time after, then into mixed liquor add 0.5ml acetone
Solution, continue stirring 2 minutes；It is put into homogeneous reactor and is reacted after above-mentioned homogeneous reaction kettle is sealed, reaction temperature is
120 DEG C, the time is 4 hours, and question response terminates, and naturally cools to room temperature, takes out reactor, filtration product, washs, after drying both
Obtain flower ball-shaped silver vanadate.
Embodiment 2
5.0g silver nitrate is weighed, solvent is made using deionized water, under conditions of shading, is stirred continuously and is configured to concentration and is
0.25g/ml silver salt solution；10.0g ammonium vanadate is weighed, solvent is made using absolute ethyl alcohol, is stirred continuously and is configured to concentration and is
1g/ml vanadic salts ethanol solution；Under conditions of being stirred continuously, by the above-mentioned silver salt solution prepared and vanadic salts ethanol solution
By volume 2：1 adds in homogeneous reaction kettle simultaneously, stir certain time after, then into mixed liquor add 3ml acetone soln,
Continue stirring 5 minutes；It is put into homogeneous reactor and is reacted after above-mentioned homogeneous reaction kettle is sealed, reaction temperature is 160 DEG C,
Time is 8 hours, and question response terminates, and naturally cools to room temperature, takes out reactor, filtration product, washing, bouquet is both obtained after drying
Shape silver vanadate.
Embodiment 3
0.2g silver nitrate is weighed, solvent is made using deionized water, under conditions of shading, is stirred continuously and is configured to concentration and is
0.02g/ml silver salt solution；0.5g vanadic anhydrides are weighed, solvent is made using absolute ethyl alcohol, is stirred continuously and is configured to concentration
For 0.1g/ml vanadic salts ethanol solution；Under conditions of being stirred continuously, by the above-mentioned silver salt solution prepared and vanadic salts ethanol
Solution by volume 2：1 adds in homogeneous reaction kettle simultaneously, after stirring certain time, then the third of 0.5ml is added into mixed liquor
Ketone solution, continue stirring 2 minutes；It is put into homogeneous reactor and is reacted after above-mentioned homogeneous reaction kettle is sealed, reaction temperature
For 120 DEG C, the time is 4 hours, and question response terminates, and naturally cools to room temperature, takes out reactor, filtration product, washing, after drying
Both flower ball-shaped silver vanadate is obtained.
Embodiment 4
0.2g silver carbonate is weighed, solvent is made using deionized water, under conditions of shading, is stirred continuously and is configured to concentration and is
0.02g/ml silver salt solution；0.5g vanadic anhydrides are weighed, solvent is made using absolute ethyl alcohol, is stirred continuously and is configured to concentration
For 0.1g/ml vanadic salts ethanol solution；Under conditions of being stirred continuously, by the above-mentioned silver salt solution prepared and vanadic salts ethanol
Solution by volume 2：1 adds in homogeneous reaction kettle simultaneously, after stirring certain time, then the third of 0.5ml is added into mixed liquor
Ketone solution, continue stirring 2 minutes；It is put into homogeneous reactor and is reacted after above-mentioned homogeneous reaction kettle is sealed, reaction temperature
For 140 DEG C, the time is 6 hours, and question response terminates, and naturally cools to room temperature, takes out reactor, filtration product, washing, after drying
Both flower ball-shaped silver vanadate is obtained.
Embodiment 5
1.0g silver carbonate is weighed, solvent is made using deionized water, under conditions of shading, is stirred continuously and is configured to concentration and is
0.1g/ml silver salt solution；2.5g vanadic anhydrides are weighed, solvent is made using absolute ethyl alcohol, is stirred continuously and is configured to concentration
For 0.5g/ml vanadic salts ethanol solution；Under conditions of being stirred continuously, by the above-mentioned silver salt solution prepared and vanadic salts ethanol
Solution by volume 1：1 adds in homogeneous reaction kettle simultaneously, after stirring certain time, then the third of 0.5ml is added into mixed liquor
Ketone solution, continue stirring 2 minutes；It is put into homogeneous reactor and is reacted after above-mentioned homogeneous reaction kettle is sealed, reaction temperature
For 120 DEG C, the time is 6 hours, and question response terminates, and naturally cools to room temperature, takes out reactor, filtration product, washing, after drying
Both flower ball-shaped silver vanadate is obtained.
Comparative example 1
Experimentation is similar to Example 1, does not add acetone simply.
Claims (6)
- A kind of 1. preparation method of flower ball-shaped silver vanadate, it is characterised in that：Specifically include following steps：（1）Weigh 0.2-5.0g silver salt, solvent made using deionized water, under conditions of shading, be stirred continuously be configured to it is dense Spend the silver salt solution for 0.02-0.25g/ml；（2）0.5-10.0g vanadic salts is weighed, solvent is made using absolute ethyl alcohol, it is 0.1-1g/ml's to be stirred continuously and be configured to concentration Vanadic salts ethanol solution；（3）It is under conditions of being stirred continuously, the above-mentioned silver salt solution prepared and vanadic salts ethanol solution is same by proper ratio When add homogeneous reaction kettle in, after certain time, then appropriate acetone soln is added into mixed liquor, continue stir 2-5 minutes；（4）It is put into homogeneous reactor and is reacted after above-mentioned homogeneous reaction kettle is sealed, after certain time, question response terminates, Room temperature is naturally cooled to, reactor is taken out, filtration product, washing, flower ball-shaped silver vanadate is both obtained after drying.
- A kind of 2. preparation method of flower ball-shaped silver vanadate according to claim 1, it is characterised in that：The step（1）In Silver salt include one or more of combinations in the water soluble silver salt such as silver nitrate, silver sulfate, silver carbonate, silver perchlorate.
- A kind of 3. preparation method of flower ball-shaped silver vanadate according to claim 1, it is characterised in that：Step（2）In vanadium Salt refers to one kind that ammonium vanadate, vanadic anhydride, sodium metavanadate, potassium metavanadate, dichloro vanadyl etc. are dissolved in the vanadic salts of ethanol Or several combination.
- A kind of 4. preparation method of flower ball-shaped silver vanadate according to claim 1, it is characterised in that：Step（3）In silver Saline solution and vanadic salts ethanol solution refer to that the volume ratio of the two is 1 by proper ratio：（0.5-1）, appropriate acetone soln is Finger volume is 0.5-3ml.
- A kind of 5. preparation method of flower ball-shaped silver vanadate according to claim 1, it is characterised in that：Step（4）In it is anti- It is 4-12 hours between seasonable, reaction temperature is 120-180 DEG C.
- 6. flower ball-shaped silver vanadate prepared by a kind of preparation method of flower ball-shaped silver vanadate according to claim 1, its feature It is, it can reach more than 98% to the percent of decolourization of methyl orange and rhodamine B.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108774447A (en) * | 2018-06-05 | 2018-11-09 | 三峡大学 | A kind of carbon-silver microballoon/epoxy resin super-hydrophobic coat preparation method |
| CN111082003A (en) * | 2019-12-05 | 2020-04-28 | 华南理工大学 | Vanadate hydrate electrode material and preparation method and application thereof |
-
2017
- 2017-10-16 CN CN201710957597.2A patent/CN107746077A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108774447A (en) * | 2018-06-05 | 2018-11-09 | 三峡大学 | A kind of carbon-silver microballoon/epoxy resin super-hydrophobic coat preparation method |
| CN108774447B (en) * | 2018-06-05 | 2020-06-16 | 三峡大学 | Preparation method of carbon-silver microsphere/epoxy resin super-hydrophobic coating |
| CN111082003A (en) * | 2019-12-05 | 2020-04-28 | 华南理工大学 | Vanadate hydrate electrode material and preparation method and application thereof |
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