CN107572585A - A kind of bismuth oxybromide visible light catalyst and preparation method thereof - Google Patents
A kind of bismuth oxybromide visible light catalyst and preparation method thereof Download PDFInfo
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- CN107572585A CN107572585A CN201710807109.XA CN201710807109A CN107572585A CN 107572585 A CN107572585 A CN 107572585A CN 201710807109 A CN201710807109 A CN 201710807109A CN 107572585 A CN107572585 A CN 107572585A
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Abstract
The invention discloses a kind of Bi24Br10O31The preparation method of visible light catalyst, using ethylene glycol and glucose as complexant and reducing agent, the two-step method combined by microwave with calcining is easy to operate, is easy to large-scale production, obtained micro-nano flower-shaped Bi24Br10O31Visible light catalyst purity is good, crystallinity is high, with high photoproduction carrier separation efficiency, high visible light catalytic activity, high stability, phenmethylol can be converted into benzaldehyde with high selectivity, react 2.5 hours conversion ratios with selectivity up to 99%, there is boundless application prospect.
Description
Technical field：
The present invention relates to novel semi-conductor catalysis material technical field, and in particular to a kind of Bi24Br10O31Visible ray is urged
Agent and its preparation method and application.
Background technology：
Industrial or agricultural continues to develop and brings that living standard is also faced with environmental pollution while increasing substantially and the energy is short
The problem of lacking getting worse.And Photocatalitic Technique of Semiconductor has the characteristics of efficient, energy-conservation, environment-friendly, it is considered to be solve
One of effective way of environmental pollution and energy shortage.Current photocatalysis technology is mainly used in light degradation organic pollution, light
Water hydrogen manufacturing, nitrogen and the fixation of carbon dioxide and the conversion of organic matter are solved, the selective catalysis conversion of wherein organic matter is near
The study hotspot risen over year.Benzaldehyde has active carbonyl, be fine chemistry industry production in staple product and intermediate,
It is a kind of important organic matter and intermediate for synthetic dyestuffs, agricultural chemicals, spices and medicine etc..Synthesized in traditional organic reaction
Not only severe reaction conditions, selectivity be not high and more serious pollution can be produced to environment for the method that benzaldehyde uses.And utilize
Photocatalysis technology is selectively oxidized phenmethylol and obtains this synthesis path of benzaldehyde, reaction condition it is gentle (normal temperature and pressure,
Without needing special installation), avoid using poisonous or strong corrosivity oxidant, and efficient energy-saving, be a kind of green to have
The approach of machine synthesizing benzaldehyde.
High-performance optical catalyst is the core of photocatalysis technology, and novel photocatalyst bismuth oxybromide (BiOBr) is one
Kind ternary metal oxyhalide semiconductor, it has special layer structure, can efficiently separate photo-generated carrier, improves light and urges
Change efficiency.The bismuth oxybromide (O and Br atom number ratio are more than 1) of rich oxygen type is such as Bi24Br10O31、Bi3O4Br、Bi12O17Br2、
Bi4O5Br2Deng oxygen-enriched degree is bigger, and band gap is narrower, and catalyst can be made to have bigger visible light-responded scope.Wherein
Bi24Br10O31Stability is good and its band structure can meet that oxidation conversion phenmethylol is wanted to benzaldehyde under visible light conditions
Ask.But current synthesis Bi24Br10O31Method it is more complicated, operation is whard to control.
The content of the invention：
It is an object of the invention to provide a kind of Bi24Br10O31The preparation method of visible light catalyst, this method is with ethylene glycol
With glucose as complexant and reducing agent, the two-step method combined by microwave with calcining is easy to operate, is easy to scale metaplasia
Production, obtained micro-nano flower-shaped Bi24Br10O31Visible light catalyst purity is good, crystallinity is high, has high photo-generated carrier point
From efficiency, high visible light catalysis activity, high stability, phenmethylol can be converted into benzaldehyde with high selectivity.
The present invention is achieved by the following technical programs：
A kind of Bi24Br10O31The preparation method of visible light catalyst, this method are used as complexant using ethylene glycol and glucose
And reducing agent, combined, comprised the following steps by microwave and calcining：
1) preparation of presoma：Glucose, bismuth nitrate and KBr are added sequentially to be stirred dissolving in ethylene glycol
Obtain solution, the mol ratio of bismuth nitrate and KBr is 2：1, the mol ratio of glucose and bismuth nitrate is 3~12：1, then will be molten
Liquid, which is transferred in microwave reactor, carries out microwave reaction, and reaction is centrifugally separating to obtain precipitation after terminating, with deionized water and anhydrous
40~100 DEG C of dryings 8~24 hours, obtain presoma after ethanol washing；
2) calcine：The precursor that step 1) is obtained is placed in Muffle furnace 400~500 DEG C and calcined, and soaking time 2~
4 hours, obtain Bi24Br10O31Photochemical catalyst.
Step 1) mixing time is 6-48 hours；Microwave power is 200~800W in microwave reaction, the reaction time is 3~
10min。
The present invention also protects the Bi that above-mentioned preparation method obtains24Br10O31The application of visible light catalyst, the catalyst
Catalytic conversion phenmethylol is the application of benzaldehyde under visible light.
Beneficial effects of the present invention are as follows：
The present invention is using ethylene glycol and glucose as complexant and reducing agent, the two-step method combined by microwave with calcining,
It is easy to operate, it is easy to large-scale production, obtained micro-nano popped rice Bi24Br10O31Visible light catalyst purity is good, crystallinity is high, tool
There are high photoproduction carrier separation efficiency, high visible light catalytic activity, high stability, phenmethylol can be converted into benzene with high selectivity
Formaldehyde, 2.5 hours conversion ratios are reacted with selectivity up to 99%, there is boundless application prospect.
Brief description of the drawings：
Fig. 1 is Bi prepared by the embodiment of the present invention 124Br10O31XRD spectrum.
Fig. 2 is Bi prepared by the embodiment of the present invention 124Br10O31SEM spectrum.
Fig. 3 is Bi prepared by the embodiment of the present invention 124Br10O31Visible light catalytic conversion phenmethylol is benzaldehyde activity.
Embodiment：
It is to further explanation of the invention, rather than limitation of the present invention below.
Embodiment 1：
1.2g glucose is added in 50mL ethylene glycol 15min is stirred at room temperature, then add 0.485g Bi
(NO3)3.5H2O continues to stir, and 0.06g KBr are added after stirring, and continues to stir 12h formation settled solutions.
Above-mentioned mixed solution is subjected to microwave reaction, microwave power 400W, reaction time 4min, sallow is obtained after reaction
The precipitation of color, is centrifuged, and is washed respectively 3 times with deionized water and absolute ethyl alcohol, and obtained solid is placed in into 60 DEG C
Dried 12 hours in baking oven, you can obtain presoma.
Weigh 300mg presomas to calcine 2 hours in 450 DEG C of Muffle furnace, you can obtain Bi24Br10O31Photochemical catalyst.
Its XRD spectrum is as shown in figure 1, Bi24Br10O31Diffraction maximum it is consistent with standard card, purity is high, better crystallinity degree.Bi24Br10O31
SEM spectrum as shown in Fig. 2 be in nanometer flower ball-shaped, part caves in broken after firing.Use the embodiment of the present invention
Bi24Br10O31Benzaldehyde experiment is catalytically conveted to phenmethylol under visible light illumination, as a result as shown in Figure 3.React 150min
The selectivity that phenmethylol is converted into benzaldehyde reaches 99%, while conversion ratio also reaches 99%, shows the active non-of the catalyst
Chang Gao.
Embodiment 2
2.4g glucose is added in 100mL ethylene glycol 15min is stirred at room temperature, then add 0.485gBi
(NO3)3.5H2O continues to stir, and 0.06g KBr are added after stirring, and continues to stir 48h formation settled solutions.
Above-mentioned mixed solution is subjected to microwave reaction, microwave power 800W, reaction time 3min, sallow is obtained after reaction
The precipitation of color, is centrifuged, and is washed respectively 3 times with deionized water and absolute ethyl alcohol, and obtained solid is placed in into 60 DEG C
Dried 12 hours in baking oven, you can obtain presoma.
Weigh 300mg presomas to calcine 4 hours in 400 DEG C of Muffle furnace, you can obtain Bi24Br10O31Photochemical catalyst.
Use the Bi of the embodiment of the present invention24Br10O31Benzaldehyde reality is catalytically conveted to phenmethylol under visible light illumination
Test, the selectivity that reaction 150min phenmethylols are converted into benzaldehyde reaches 99%, while conversion ratio reaches 90%.
Embodiment 3
0.6g glucose is added in 100mL ethylene glycol 15min is stirred at room temperature, then add 0.485gBi
(NO3)3.5H2O continues to stir, and 0.06g KBr are added after stirring, and continues to stir 6h formation settled solutions.
Above-mentioned mixed solution is subjected to microwave reaction, microwave power 200W, reaction time 10min, ash is obtained after reaction
The precipitation of yellow, is centrifuged, and is washed respectively 3 times with deionized water and absolute ethyl alcohol, and obtained solid is placed in into 60 DEG C
Baking oven in dry 12 hours, you can obtain presoma.
Weigh 300mg presomas to calcine 2 hours in 500 DEG C of Muffle furnace, you can obtain Bi24Br10O31Photochemical catalyst.
Use the Bi of the embodiment of the present invention24Br10O31Benzaldehyde reality is catalytically conveted to phenmethylol under visible light illumination
Test, the selectivity that reaction 150min phenmethylols are converted into benzaldehyde reaches 99%, while conversion ratio reaches 87%.
Finally it should be noted that the above embodiments are merely illustrative of the technical solutions of the present invention rather than the present invention is protected
The limitation of scope, it will be understood by those within the art that, technical scheme can be modified or waited
With replacing, without departing from the spirit and scope of technical solution of the present invention.
Claims (4)
- A kind of 1. Bi24Br10O31The preparation method of visible light catalyst, it is characterised in that this method is made with ethylene glycol and glucose For complexant and reducing agent, combined by microwave and calcining, this method comprises the following steps：1) glucose, bismuth nitrate and KBr are added sequentially to be stirred dissolving in ethylene glycol and obtain solution, bismuth nitrate and The mol ratio of KBr is 2：1, the mol ratio of glucose and bismuth nitrate is 3~12：1, then transfer the solution into microwave reaction Microwave reaction is carried out in device, reaction is centrifugally separating to obtain precipitation after terminating, 40~100 after being washed with deionized water and absolute ethyl alcohol DEG C dry 8~24 hours, obtain presoma；2) precursor for obtaining step 1) is placed in Muffle furnace 400~500 DEG C and calcined, and soaking time 2~4 hours, obtains To Bi24Br10O31Photochemical catalyst.
- 2. Bi according to claim 124Br10O31The preparation method of visible light catalyst, it is characterised in that step 1) is stirred It is 6-48 hours to mix the time；Microwave power is 200~800W in microwave reaction, and the reaction time is 3~10min.
- A kind of 3. Bi24Br10O31Visible light catalyst, it is characterised in that the Bi24Br10O31Visible light catalyst is according to right It is required that the preparation method in 1-2 described in any one claim obtains.
- 4. the Bi described in claim 324Br10O31The application of visible light catalyst, it is characterised in that the catalyst is visible Catalytic conversion phenmethylol is benzaldehyde under light.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108187699A (en) * | 2018-01-31 | 2018-06-22 | 安徽师范大学 | BiOX-Bi4O5X2Hetero-junctions and its preparation method and application |
| CN111482186A (en) * | 2020-04-15 | 2020-08-04 | 重庆科技学院 | Bi for treating oil field waste liquid organic matter3O4Preparation method of Br photocatalyst |
| CN113813971A (en) * | 2021-10-14 | 2021-12-21 | 内蒙古农业大学 | Preparation method and application of necklace-shaped bismuth oxybromide and sodium titanate heterojunction composite catalyst |
| CN114011403A (en) * | 2021-12-16 | 2022-02-08 | 广东工业大学 | Preparation method and application of amorphous bismuth tungstate photocatalytic material |
-
2017
- 2017-09-08 CN CN201710807109.XA patent/CN107572585B/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108187699A (en) * | 2018-01-31 | 2018-06-22 | 安徽师范大学 | BiOX-Bi4O5X2Hetero-junctions and its preparation method and application |
| CN111482186A (en) * | 2020-04-15 | 2020-08-04 | 重庆科技学院 | Bi for treating oil field waste liquid organic matter3O4Preparation method of Br photocatalyst |
| CN111482186B (en) * | 2020-04-15 | 2022-04-01 | 重庆科技学院 | Bi for treating oil field waste liquid organic matter3O4Preparation method of Br photocatalyst |
| CN113813971A (en) * | 2021-10-14 | 2021-12-21 | 内蒙古农业大学 | Preparation method and application of necklace-shaped bismuth oxybromide and sodium titanate heterojunction composite catalyst |
| CN113813971B (en) * | 2021-10-14 | 2023-08-22 | 内蒙古农业大学 | Preparation method and application of necklace-shaped bismuth oxybromide and sodium titanate heterojunction composite catalyst |
| CN114011403A (en) * | 2021-12-16 | 2022-02-08 | 广东工业大学 | Preparation method and application of amorphous bismuth tungstate photocatalytic material |
| CN114011403B (en) * | 2021-12-16 | 2022-07-12 | 广东工业大学 | Preparation method and application of amorphous bismuth tungstate photocatalytic material |
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