CN107537468A - A kind of preparation method for the bismuth tungstate based photocatalyst for loading graphite oxide - Google Patents
A kind of preparation method for the bismuth tungstate based photocatalyst for loading graphite oxide Download PDFInfo
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- CN107537468A CN107537468A CN201610480357.3A CN201610480357A CN107537468A CN 107537468 A CN107537468 A CN 107537468A CN 201610480357 A CN201610480357 A CN 201610480357A CN 107537468 A CN107537468 A CN 107537468A
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- mixed solution
- bismuth
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Abstract
This application discloses a kind of preparation method for the bismuth tungstate based photocatalyst for loading graphite oxide, including step：(1), by enuatrol, Bi (NO3)3·5H2O、Na2WO4·2H2O ultrasonic disperses obtain mixed solution in ethylene glycol solution；(2), graphene oxide is added into mixed solution to be stirred；(3), the mixed solution added with graphene oxide is reacted 22~24 hours in hydrothermal reaction kettle, 200~220 DEG C of reaction temperature；(4), supersound washing, drying and grind, obtain the bismuth tungstate/bismuth oxide photocatalyst for being loaded with graphene oxide, in the catalyst, the mass ratio of graphene oxide is 3~5%.Bismuth tungstate/bismuth oxide photocatalyst prepared by the present invention shows good photocatalytic activity, and under visible light illumination, its degradation rate to organic pollution reaches more than 99%, reaches more than 90% to RhB eliminating rate of absorption.
Description
Technical field
The application belongs to technical field of waste water processing, more particularly to a kind of bismuth tungstate base optic catalytic for loading graphite oxide
The preparation method of agent.
Background technology
China's medicinal industry produces substantial amounts of organic wastewater every year, wherein containing substantial amounts of antibiotic.Antibiotic is present in
In waste water, because it has extremely strong inhibitory action to microorganism, cause biochemical process performance poor, brought greatly to sewage disposal
Challenge, belongs to one of typical used water difficult to degradate.
Photocatalysis technology is widely closed in organic pollution processing in recent years as a kind of high-level oxidation technology
Note.Nano-photo catalytic be nano semiconductor material be under the irradiation of light, generation with extremely strong active hydroxyl oxygen radical (
OH), organic pollution materials are effectively decomposed or destroyed its difficult for biological degradation group by radical reaction, can be given birth to so as to improve it
Change degradability.The technology does not produce secondary pollution because its is simple to operate, and processing cost is low, be successfully applied to dyeing waste water and
The advanced treating of the waste water such as surfactant.
The content of the invention
It is an object of the invention to provide it is a kind of load graphite oxide bismuth tungstate based photocatalyst preparation method, with gram
Take deficiency of the prior art.
To achieve the above object, the present invention provides following technical scheme：
The embodiment of the present application discloses a kind of preparation method for the bismuth tungstate based photocatalyst for loading graphite oxide, including step
Suddenly：
(1), by enuatrol, Bi (NO3)3·5H2O、Na2WO4·2H2O ultrasonic disperses are mixed in ethylene glycol solution
Solution；
(2), graphene oxide is added into mixed solution to be stirred；
(3), the mixed solution added with graphene oxide is reacted 22~24 hours in hydrothermal reaction kettle, reaction temperature
200~220 DEG C；
(4), supersound washing, drying and grind, obtain the bismuth tungstate/bismuth oxide photocatalyst for being loaded with graphene oxide,
In the catalyst, the mass ratio of graphene oxide is 3~5%.
Preferably, in the preparation method of the bismuth tungstate based photocatalyst of above-mentioned load graphite oxide, in step (1),
Enuatrol, Bi (NO3)3·5H2O、Na2WO4·2H2O mol ratios are 1：(1~1.1)：(0.7~0.85).
Preferably, in the preparation method of the bismuth tungstate based photocatalyst of above-mentioned load graphite oxide, in step (1),
Bi(NO3)3·5H2O preparation method includes：
(1), by nonionic surface active agent: cosurfactant: organic solvent not soluble in water volume ratio (10~
14): (12~15): (50~70), be configured to mixed solution；
(2), addition concentration is 1.2~2.0mol/L bismuth nitrate solutions in mixed solution and concentration is 1.5~2.0mol/
L dilute alkaline solns, are stirred；And make reaction complete；
(3), products therefrom is centrifuged, washed and vacuum dried, obtains a nanometer bismuth nitrate.
Preferably, in the preparation method of the bismuth tungstate based photocatalyst of above-mentioned load graphite oxide, in step (1),
Na2WO4·2H2O purification process includes：Under conditions of 50~100 DEG C, adjusting the pH value of sodium tungstate solution precipitates silicon, obtains
To the first sodium tungstate mixed solution precipitated containing silicon；Magnesium salts is added into the first sodium tungstate mixed solution, obtains second
Sodium tungstate mixed solution；Under conditions of temperature is not less than 50 degrees Celsius, the second sodium tungstate mixed solution is stirred, is obtained containing heavy
The 3rd sodium tungstate mixed solution to form sediment；3rd sodium tungstate mixed solution is filtered, obtains filtrate；Filtrate is evaporated,
Dry, obtain pure sodium tungstate.
Preferably, in the preparation method of the bismuth tungstate based photocatalyst of above-mentioned load graphite oxide, in step (2),
The preparation method of graphene oxide：Graphite raw material, pro-oxidant are added aqueous slkali and be placed in closed container, uses replacement of oxygen
Gas in container and to be filled with oxygen to pressure be 1~20Mpa, in temperature, 101 DEG C~650 DEG C are reacted, and reaction takes after terminating
Go out reaction product separation of solid and liquid, gained solid phase is washed and dried, and obtains graphene oxide.
Compared with prior art, the advantage of the invention is that：Bismuth tungstate prepared by the present invention/bismuth oxide photocatalyst performance
Good photocatalytic activity is gone out, under visible light illumination, its degradation rate to organic pollution reaches more than 99%, to RhB
Eliminating rate of absorption reach more than 90%.
Embodiment
The present invention is described further by the following example：According to following embodiments, the present invention may be better understood.
However, as it will be easily appreciated by one skilled in the art that specific material ratio, process conditions and its result described by embodiment are only used
In the explanation present invention, without should be also without limitation on the present invention described in detail in claims.
The preparation method of bismuth nitrate：
1), by nonionic surface active agent: cosurfactant: organic solvent not soluble in water volume ratio (10~
14): (12~15): (50~70), be configured to mixed solution；
2), addition concentration is 1.2~2.0mol/L bismuth nitrate solutions in mixed solution and concentration is 1.5~2.0mol/L
Dilute alkaline soln, it is stirred；And make reaction complete；
3), products therefrom is centrifuged, washed and vacuum dried, obtains a nanometer bismuth nitrate.
The purification method of sodium tungstate
Under conditions of 50~100 DEG C, adjusting the pH value of sodium tungstate solution precipitates silicon, obtains first containing silicon precipitation
Sodium tungstate mixed solution；Magnesium salts is added into the first sodium tungstate mixed solution, obtains the second sodium tungstate mixed solution；In temperature
Degree is not less than under conditions of 50 degrees Celsius, stirs the second sodium tungstate mixed solution, obtains the 3rd sodium tungstate mixing containing precipitation
Solution；3rd sodium tungstate mixed solution is filtered, obtains filtrate；Filtrate is evaporated, dried, obtains pure wolframic acid
Sodium.
The preparation method of graphene oxide
Graphite raw material, pro-oxidant are added aqueous slkali and be placed in closed container, with replacement of oxygen gas in container simultaneously
It is 1~20Mpa to be filled with oxygen to pressure, and in temperature, 101 DEG C~650 DEG C are reacted, and reaction is taken out reaction product after terminating and consolidated
Liquid is separated, and gained solid phase is washed and dried, and obtains graphene oxide.
Load the preparation method of the bismuth tungstate based photocatalyst of graphite oxide
(1), by enuatrol, Bi (NO3)3·5H2O、Na2WO4·2H2O is according to mol ratio 1：(1~1.1)：(0.7~
0.85) ultrasonic disperse obtains mixed solution in ethylene glycol solution；
(2), graphene oxide is added into mixed solution to be stirred；
(3), the mixed solution added with graphene oxide is reacted 22~24 hours in hydrothermal reaction kettle, reaction temperature
200~220 DEG C；
(4), supersound washing, drying and grind, obtain the bismuth tungstate/bismuth oxide photocatalyst for being loaded with graphene oxide.
In the composite, the mass ratio of graphene oxide is 3~5%.
Bismuth tungstate/bismuth oxide photocatalyst of preparation shows good photocatalytic activity, under visible light illumination, its
More than 99% is reached to the degradation rate of organic pollution, more than 90% is reached to RhB eliminating rate of absorption.
Finally, it is to be noted that, term " comprising ", "comprising" or its any other variant be intended to it is non-exclusive
Property includes, so that process, method, article or equipment including a series of elements not only include those key elements, and
Also include the other element that is not expressly set out, or also include for this process, method, article or equipment inherently
Key element.
Claims (5)
1. a kind of preparation method for the bismuth tungstate based photocatalyst for loading graphite oxide, it is characterised in that including step：
(1), by enuatrol, Bi (NO3)3·5H2O、Na2WO4·2H2O ultrasonic disperses obtain mixing molten in ethylene glycol solution
Liquid；
(2), graphene oxide is added into mixed solution to be stirred；
(3), the mixed solution added with graphene oxide is reacted 22~24 hours in hydrothermal reaction kettle, reaction temperature 200
~220 DEG C；
(4), supersound washing, drying and grind, obtain the bismuth tungstate/bismuth oxide photocatalyst for being loaded with graphene oxide, this is urged
In agent, the mass ratio of graphene oxide is 3~5%.
2. the preparation method of the bismuth tungstate based photocatalyst of load graphite oxide according to claim 1, it is characterised in that：
In step (1), enuatrol, Bi (NO3)3·5H2O、Na2WO4·2H2O mol ratios are 1：(1~1.1)：(0.7~0.85).
3. the preparation method of the bismuth tungstate based photocatalyst of load graphite oxide according to claim 1, it is characterised in that：
In step (1), Bi (NO3)3·5H2O preparation method includes：
(1), by nonionic surface active agent: cosurfactant: the volume ratio (10~14) of organic solvent not soluble in water:
(12~15): (50~70), it is configured to mixed solution；
(2), addition concentration is 1.2~2.0mol/L bismuth nitrate solutions in mixed solution and concentration is 1.5~2.0mol/L dilute
Aqueous slkali, it is stirred；And make reaction complete；
(3), products therefrom is centrifuged, washed and vacuum dried, obtains a nanometer bismuth nitrate.
4. the preparation method of the bismuth tungstate based photocatalyst of load graphite oxide according to claim 1, it is characterised in that：
In step (1), Na2WO4·2H2O purification process includes：Under conditions of 50~100 DEG C, the pH value of sodium tungstate solution is adjusted
Silicon is precipitated, obtains the first sodium tungstate mixed solution containing silicon precipitation；Magnesium is added into the first sodium tungstate mixed solution
Salt, obtain the second sodium tungstate mixed solution；Under conditions of temperature is not less than 50 degrees Celsius, stirring the second sodium tungstate mixing is molten
Liquid, obtain the 3rd sodium tungstate mixed solution containing precipitation；3rd sodium tungstate mixed solution is filtered, obtains filtrate；It is right
Filtrate is evaporated, dried, and obtains pure sodium tungstate.
5. the preparation method of the bismuth tungstate based photocatalyst of load graphite oxide according to claim 1, it is characterised in that：
In step (2), the preparation method of graphene oxide：Graphite raw material, pro-oxidant are added aqueous slkali and are placed in closed container,
With replacement of oxygen gas in container and to be filled with oxygen to pressure be 1~20Mpa, and in temperature, 101 DEG C~650 DEG C are reacted, instead
Reaction product separation of solid and liquid is taken out after should terminating, gained solid phase is washed and dried, and obtains graphene oxide.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109939672A (en) * | 2019-03-06 | 2019-06-28 | 湘潭大学 | A kind of modified by graphene quantum dot Lacking oxygen bismuth tungstate composite photocatalyst and preparation method thereof |
| CN110180532A (en) * | 2019-05-07 | 2019-08-30 | 重庆工商大学 | A kind of carbon doping bismuth tungstate photocatalyst and preparation method thereof containing oxygen defect |
| CN112044430A (en) * | 2020-09-24 | 2020-12-08 | 哈尔滨理工大学 | Novel lignin carbon/bismuth tungstate composite material for photocatalytic degradation of methylene blue and preparation method thereof |
| CN113996318A (en) * | 2021-11-24 | 2022-02-01 | 白银新大孚科技化工有限公司 | Ternary compound Pr-Go-BiOX catalyst and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1587063A (en) * | 2004-07-22 | 2005-03-02 | 中国地质大学（武汉） | Process for preparing nano alkaline bismuth nitrate by micro emulsion |
| CN104722293A (en) * | 2015-02-02 | 2015-06-24 | 吉林大学 | Visible light responded load type Bi2WO6/Bi2O3 heterojunction photocatalyst and preparation method thereof |
| CN104973628A (en) * | 2015-06-30 | 2015-10-14 | 崇义章源钨业股份有限公司 | Method used for purifying sodium tungstate solution |
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2016
- 2016-06-27 CN CN201610480357.3A patent/CN107537468A/en not_active Withdrawn
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1587063A (en) * | 2004-07-22 | 2005-03-02 | 中国地质大学（武汉） | Process for preparing nano alkaline bismuth nitrate by micro emulsion |
| CN104722293A (en) * | 2015-02-02 | 2015-06-24 | 吉林大学 | Visible light responded load type Bi2WO6/Bi2O3 heterojunction photocatalyst and preparation method thereof |
| CN104973628A (en) * | 2015-06-30 | 2015-10-14 | 崇义章源钨业股份有限公司 | Method used for purifying sodium tungstate solution |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109939672A (en) * | 2019-03-06 | 2019-06-28 | 湘潭大学 | A kind of modified by graphene quantum dot Lacking oxygen bismuth tungstate composite photocatalyst and preparation method thereof |
| CN110180532A (en) * | 2019-05-07 | 2019-08-30 | 重庆工商大学 | A kind of carbon doping bismuth tungstate photocatalyst and preparation method thereof containing oxygen defect |
| CN112044430A (en) * | 2020-09-24 | 2020-12-08 | 哈尔滨理工大学 | Novel lignin carbon/bismuth tungstate composite material for photocatalytic degradation of methylene blue and preparation method thereof |
| CN113996318A (en) * | 2021-11-24 | 2022-02-01 | 白银新大孚科技化工有限公司 | Ternary compound Pr-Go-BiOX catalyst and preparation method thereof |
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