CN109364958A - A kind of Bi4O5BrxI2-xThe preparation method of mischcrystal photocatalyst - Google Patents
A kind of Bi4O5BrxI2-xThe preparation method of mischcrystal photocatalyst Download PDFInfo
- Publication number
- CN109364958A CN109364958A CN201811510441.0A CN201811510441A CN109364958A CN 109364958 A CN109364958 A CN 109364958A CN 201811510441 A CN201811510441 A CN 201811510441A CN 109364958 A CN109364958 A CN 109364958A
- Authority
- CN
- China
- Prior art keywords
- preparation
- mischcrystal photocatalyst
- iodide
- bromide
- mischcrystal
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 30
- 239000000243 solution Substances 0.000 claims abstract description 20
- 230000001699 photocatalysis Effects 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 16
- 238000007146 photocatalysis Methods 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 16
- CPELXLSAUQHCOX-UHFFFAOYSA-M Bromide Chemical compound [Br-] CPELXLSAUQHCOX-UHFFFAOYSA-M 0.000 claims abstract description 13
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 claims abstract description 13
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000012046 mixed solvent Substances 0.000 claims abstract description 9
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 6
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 6
- FVAUCKIRQBBSSJ-UHFFFAOYSA-M sodium iodide Chemical compound [Na+].[I-] FVAUCKIRQBBSSJ-UHFFFAOYSA-M 0.000 claims description 30
- IOLCXVTUBQKXJR-UHFFFAOYSA-M potassium bromide Chemical compound [K+].[Br-] IOLCXVTUBQKXJR-UHFFFAOYSA-M 0.000 claims description 20
- 238000003756 stirring Methods 0.000 claims description 16
- 235000009518 sodium iodide Nutrition 0.000 claims description 10
- 239000000725 suspension Substances 0.000 claims description 8
- 239000011259 mixed solution Substances 0.000 claims description 7
- NLKNQRATVPKPDG-UHFFFAOYSA-M potassium iodide Chemical compound [K+].[I-] NLKNQRATVPKPDG-UHFFFAOYSA-M 0.000 claims description 6
- 238000000926 separation method Methods 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 5
- 238000005303 weighing Methods 0.000 claims description 5
- 238000006243 chemical reaction Methods 0.000 claims description 4
- 229940068918 polyethylene glycol 400 Drugs 0.000 claims description 4
- JHJLBTNAGRQEKS-UHFFFAOYSA-M sodium bromide Chemical compound [Na+].[Br-] JHJLBTNAGRQEKS-UHFFFAOYSA-M 0.000 claims description 4
- 239000003513 alkali Substances 0.000 claims description 3
- 229940113115 polyethylene glycol 200 Drugs 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 2
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 abstract description 24
- 239000006104 solid solution Substances 0.000 abstract description 17
- 239000008367 deionised water Substances 0.000 abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 abstract description 8
- 238000010189 synthetic method Methods 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 4
- 229910052797 bismuth Inorganic materials 0.000 abstract description 3
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 abstract description 3
- 238000006555 catalytic reaction Methods 0.000 abstract description 3
- 230000001276 controlling effect Effects 0.000 abstract description 3
- 239000002904 solvent Substances 0.000 abstract description 3
- 230000003197 catalytic effect Effects 0.000 abstract description 2
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 2
- 230000001105 regulatory effect Effects 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract 2
- 229910052736 halogen Inorganic materials 0.000 abstract 1
- 150000002367 halogens Chemical class 0.000 abstract 1
- 238000001027 hydrothermal synthesis Methods 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 239000003054 catalyst Substances 0.000 description 8
- 238000013019 agitation Methods 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 229910001220 stainless steel Inorganic materials 0.000 description 6
- 239000010935 stainless steel Substances 0.000 description 6
- 238000002441 X-ray diffraction Methods 0.000 description 5
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 4
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 235000011187 glycerol Nutrition 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 238000007539 photo-oxidation reaction Methods 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241000790917 Dioxys <bee> Species 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 1
- 239000005977 Ethylene Substances 0.000 description 1
- 238000002835 absorbance Methods 0.000 description 1
- 230000032900 absorption of visible light Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/06—Halogens; Compounds thereof
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Catalysts (AREA)
Abstract
The invention discloses a kind of Bi4O5BrxI2‑xThe preparation method of mischcrystal photocatalyst, belongs to photocatalysis field.The method comprise the steps that, by regulating and controlling the molar ratio of bromide and iodide, having obtained a series of Bi of different proportions using a step solvent-thermal method in a certain proportion of in the mixed solvent4O5BrxI2‑xSolid solution catalysis material, and show excellent visible light catalytic organic pollutant activity.Preparation step are as follows: using polyethylene glycol and deionized water as solvent, using bismuth nitrate, bromide and iodide as raw material, and with sodium hydroxide solution adjust solution pH value, control the input amount of halogen, rich bismuth Bi obtained by simple one step hydro thermal method4O5BrxI2‑xMischcrystal photocatalyst.This method simple process avoids the lengthy and jumbled of multi-step synthetic methods, Bi low in cost, prepared4O5BrxI2‑xMischcrystal photocatalyst visible light catalysis activity with higher.
Description
Technical field
The present invention relates to a kind of Bi4O5BrxI2-xThe preparation method of mischcrystal photocatalyst, belongs to photocatalysis field.
Background technique
Since people excessively pursue the rate of economic development without strong environmental consciousness therefore lead to non-renewable energy
A large amount of consumption and environmental pollution in source.Solar energy is as a kind of sustainable energy of green non-pollution, in this resource phase now
To capturing consequence under deficient overall background.Photocatalysis technology can be converted natural light and artificial light to due to it
Organic matter in contaminated water can also be resolved into water and dioxy under illumination condition by the chemical energy that can be utilized by people
Change the inorganic molecules such as carbon to degrade to pollutant, thus causes the extensive concern of people.
Photochemical catalyst BiOX is received significant attention because of its special layer structure in photocatalysis field.However BiOX light is urged
It is limited to the absorption of visible light to change material, photo-generate electron-hole is easy in conjunction with causing photocatalysis efficiency lower.BiOX's leads
Band bottom (CB) is mainly made of Bi 6p track, therefore raising Bi content can make the edge CB increase and reduce band-gap energy
(Eg), thus absorption of the enhancing to visible bloom;Solid solution strategy can also be adjusted compared with accuracy controlling band gap and bandedge placement
Separation and the transport property of carrier are controlled, so as to improve the photocatalysis performance of material.Rich bismuth and solid solution strategy combine, and both make
Band gap narrows, and enhances absorption of the catalysis material to visible light, while increase valence band location again, improves photooxidation energy
Power.But it is reported at present about Bi4O5BrxI2-xThe synthetic method of solid solution is complex, and two steps or multistep processes is mostly used to close
At.Wherein, the method that two-step method largely uses solvent heat or hydro-thermal first prepares Bi4O5BrxI2-xThen presoma passes through water again
The method of solution obtains pure phase Bi4O5BrxI2-xThe shortcomings that solid solution, the method, is that the precursor construction and composition to be formed is difficult to really
Fixed, this will cause final Bi4O5BrxI2-xThe content of middle Br and I is difficult to control.
It is, thus, sought for a kind of simpler, efficient synthetic method prepares Bi4O5BrxI2-xSolid solution.
Summary of the invention
For current preparation Bi4O5BrxI2-xThe step of method of solid solution complexity problem, the invention solves technology
Problem is to simplify preparation Bi4O5BrxI2-xThe processing step of solid solution simultaneously obtains solid solution pure phase.
In order to solve the above technical problems, present invention provide the technical scheme that being rubbed by regulation bromide and iodide
That ratio, prepares a series of Bi using simple step solvent-thermal method4O5BrxI2-xMischcrystal photocatalyst, the photochemical catalyst band
Gap is adjustable, under visible light can efficient degradable organic pollutant, and the method for the present invention simple process, low in cost, synthesis
Different Br/I molar ratios photochemical catalyst photocatalysis have different photocatalysis performances.
Further, a kind of Bi provided by the invention4O5BrxI2-xThe preparation method of mischcrystal photocatalyst, including it is following
Step:
(1) by water and polyethylene glycol with volume ratio (0~1): 1 preparation obtains mixed solvent, and bismuth nitrate, stirring 0.5 is added
~3h;
(2) bromide and iodide for weighing different mol ratio are dissolved in above-mentioned mixed solution, continue 0.5~3h of stirring;
(3) it is 10~11 that alkali, which is added, and adjusts solution ph, continues stirring until forming uniform suspension;
(4) above-mentioned suspension is transferred in reaction kettle, 12~18h is reacted at 120~180 DEG C, product is separated by solid-liquid separation,
It is dry, a series of Bi of different proportions can be prepared4O5BrxI2-xMischcrystal photocatalyst, wherein x meets: 0≤x≤2.
In one embodiment of the invention, the polyethylene glycol is polyethylene glycol 200, one in polyethylene glycol 400
Kind.
In one embodiment of the invention, final concentration of 0.03~0.1mol/L of the bismuth nitrate.
In one embodiment of the invention, the bromide is one of potassium bromide, sodium bromide.
In one embodiment of the invention, the iodide are one of potassium iodide, sodium iodide.
In one embodiment of the invention, the molar ratio of the bromide and iodide is unlimited, preferably 1:1.
In one embodiment of the invention, the molar ratio of the bismuth nitrate and bromide and iodide summation is 1:1.
In one embodiment of the invention, the alkali is sodium hydroxide solution.
In one embodiment of the invention, the concentration of the sodium hydroxide solution is 1~3molL-1。
In one embodiment of the invention, the reaction kettle is the stainless steel reaction under high pressure containing polytetrafluoroethylliner liner
Kettle.
In one embodiment of the invention, the drying is dry 6~12h at 50~80 DEG C.
In one embodiment of the invention, the water is preferably deionized water.
Compared with prior art, the present invention having a significant advantage that
(1) present invention uses simple step solvent-thermal method, by the in the mixed solvent being made of polyethylene glycol and water,
The molar ratio for regulating and controlling bromide and iodide, has obtained a series of Bi of difference Br/I ratios4O5BrxI2-xSolid solution photocatalysis
Agent, the synthetic method craft is simple, easy to operate, avoids the lengthy and jumbled of two steps or multi-step synthetic methods, low in cost.
(2) Bi prepared by the present invention4O5BrxI2-xMischcrystal photocatalyst band gap is adjustable, effectively accelerates moving for carrier
Rate is moved, rich bismuth and solid solution strategy combine and not only enhance to visible absorption but also improve photooxidation ability, and different
Br/I molar ratio solid solution shows different photocatalytic activities.
Detailed description of the invention
Figure 1B i4O5BrxI2-xThe X-ray diffraction style of mischcrystal photocatalyst;
Fig. 2 Bi4O5Br2、Bi4O5BrI、Bi4O5I2The electron scanning micrograph of mischcrystal photocatalyst, wherein (a)
Bi4O5Br2;(b)Bi4O5BrI;(c)Bi4O5I2;
Fig. 3 Bi4O5BrxI2-xThe photocatalysis performance of mischcrystal photocatalyst compares;
Fig. 4 is using deionized water as Bi prepared by solvent4O5The X-ray diffraction style of BrI photochemical catalyst;
Fig. 5 is using glycerine and deionized water as Bi prepared by mixed solvent4O5The X-ray diffraction style of BrI photochemical catalyst.
Specific embodiment
In order to better understand the present invention, below with reference to the example content that the present invention is furture elucidated, but it is of the invention interior
Appearance is not limited to example given below.
Embodiment 1
A kind of Bi4O5BrxI2-xThe preparation method of mischcrystal photocatalyst, preparation process are as follows:
The ratio of polyethylene glycol 400 that total volume is 30mL and deionized water 1:0.2 by volume are measured as in beaker,
The bismuth nitrate for weighing 2mmol is dissolved in above-mentioned in the mixed solvent, magnetic agitation 0.5h;Then the difference that total amount is 2mmol is weighed
The potassium bromide and sodium iodide of molar ratio (2:0,1.5:0.5,1:1,0.5:1.5,0:2) are dissolved in above-mentioned mixed solution, continue to stir
1h;Sodium hydroxide solution (the 1molL of 5.5mL is added-1) solution ph is adjusted to 10.5, continue stirring until being formed uniform
Then suspension is transferred in stainless steel autoclave of the 50mL containing polytetrafluoroethylliner liner, reacts 16h at 160 DEG C, by institute
Product centrifuge separation is obtained, and dry at 60 DEG C, obtains a series of Bi of different proportions4O5BrxI2-xMischcrystal photocatalyst.
To the Bi being prepared4O5BrxI2-xMischcrystal photocatalyst has carried out X-ray diffraction characterization, as shown in Figure 1, working as
When potassium bromide and the molar ratio of sodium iodide are 2:0, obtained sample is Bi4O5Br2, diffraction maximum and standard card (JCPDS
No.97-041-2591) match, when potassium bromide and the molar ratio of sodium iodide are 0:2, obtained sample is pure phase Bi4O5I2;
When potassium bromide and the molar ratio of sodium iodide are 1.5:0.5,1:1,0.5:1.5, Bi4O5BrxI2-xDiffraction maximum between Bi4O5Br2
And Bi4O5I2Between.The result shows that successfully having obtained Bi using synthetic method of the present invention4O5BrxI2-xSolid solution.
Using scanning electron microscope to Bi4O5BrxI2-xThe pattern of solid solution is characterized, as shown in Figure 2, wherein
Wherein (a) is Bi4O5Br2;It (b) is Bi4O5BrI;It (c) is Bi4O5I2.As it can be seen that three samples show regular two-dimensional nano
Chip architecture, wherein Bi4O5Br2Surface is smooth, thinner thickness;Bi4O5The thickness and Bi of BrI4O5Br2It is similar;And Bi4O5I2Thickness
It is thicker.
Bi4O5BrxI2-xThe photocatalysis performance of solid solution is degradation of phenol under the radiation of visible light provided by 300W xenon lamp
For solution come what is measured, specific experimentation is as follows: it is molten to weigh the 100mL phenol that 50mg photochemical catalyst addition concentration is 10mg/L
In liquid, the solution prepared is placed in dark place magnetic agitation 30min and reaches adsorption equilibrium, so that it is carried out photocatalysis anti-
It answers, takes the solution of about 4mL every 10min, by being centrifugated out photochemical catalyst, measure supernatant using ultraviolet specrophotometer
Absorbance.Bi4O5BrxI2-xThe photocatalysis performance of solid solution is as shown in figure 3, work as x=1, i.e., when the molar ratio of Br/I is 1:1
When, the photocatalysis performance of sample is best, complete catalytic elimination phenol can be somebody's turn to do as x=0.5 in 50min
Bi4O5Br0.5I1.5Solid solution catalyst can also remove 90% or more phenol in 50min, it is seen then that the present invention is prepared
Bi4O5BrxI2-xMischcrystal photocatalyst has good photocatalysis performance.
Embodiment 2
A kind of Bi4O5BrxI2-xThe preparation method of mischcrystal photocatalyst, preparation process are as follows:
The ratio of polyethylene glycol 400 that total volume is 30mL and deionized water 1:1 by volume are measured as in beaker, is claimed
The bismuth nitrate of 2mmol is taken to be dissolved in above-mentioned in the mixed solvent, magnetic agitation 0.5h;Then the difference that total amount is 2mmol is weighed to rub
You are dissolved in above-mentioned mixed solution at the potassium bromide and sodium iodide than (2:0,1.5:0.5,1:1,0.5:1.5,0:2), continue to stir 1h;
Sodium hydroxide solution (the 1molL of 5.5mL is added-1) solution ph is adjusted to 10.5, continue stirring until forming uniform hang
Then supernatant liquid is transferred in stainless steel autoclave of the 50mL containing polytetrafluoroethylliner liner, 18h is reacted at 120 DEG C, by gained
Product centrifuge separation, and it is dry at 80 DEG C, obtain a series of Bi of different proportions4O5BrxI2-xMischcrystal photocatalyst.
Embodiment 3
A kind of Bi4O5BrxI2-xThe preparation method of mischcrystal photocatalyst, preparation process are as follows:
It measures the polyethylene glycol 200 that total volume is 30mL and is dissolved in poly- second two as the bismuth nitrate in beaker, weighing 2mmol
In alcohol 200, magnetic agitation 0.5h;Then weigh total amount be 2mmol different mol ratio (2:0,1.5:0.5,1:1,0.5:1.5,
Potassium bromide and sodium iodide 0:2) is dissolved in above-mentioned mixed solution, continues to stir 1h;The sodium hydroxide solution of 5.5mL is added
(1mol·L-1) solution ph is adjusted to 11, continue stirring until forming uniform suspension, is then transferred to 50mL containing polytetrafluoro
In the stainless steel autoclave of ethylene liner, 12h is reacted at 180 DEG C, products therefrom is centrifugated, and done at 50 DEG C
It is dry, obtain a series of Bi of different proportions4O5BrxI2-xMischcrystal photocatalyst.
Comparative example 1
A kind of Bi4O5The preparation method of BrI mischcrystal photocatalyst, preparation process are as follows:
Measuring total volume is 30mL deionized water in beaker, and the bismuth nitrate for weighing 2mmol is dissolved in above-mentioned mixed solvent
In, magnetic agitation 0.5h;Then the different mol ratio (2:0,1.5:0.5,1:1,0.5:1.5,0:2) that total amount is 2mmol is weighed
Potassium bromide and sodium iodide be dissolved in above-mentioned mixed solution, continue stir 1h;Sodium hydroxide solution (the 1molL of 5.5mL is added-1)
Solution ph is adjusted to 10.5, continues stirring until forming uniform suspension, is then transferred to 50mL containing polytetrafluoroethylliner liner
Stainless steel autoclave in, react 16h at 160 DEG C, products therefrom be centrifugated, and is dry at 60 DEG C, obtain
Bi4O5BrI mischcrystal photocatalyst.The Bi being prepared4O5BrI passes through XRD analysis it is found that being non-pure phase structure, containing unknown
Impurity diffraction maximum, as shown in Figure 4.
Comparative example 2
A kind of Bi4O5The preparation method of BrI mischcrystal photocatalyst, preparation process are as follows:
The ratio of glycerine and deionized water 1:0.2 by volume that total volume is 30mL is measured as in beaker, is weighed
The bismuth nitrate of 2mmol is dissolved in above-mentioned in the mixed solvent, magnetic agitation 0.5h;Then different moles that total amount is 2mmol are weighed
Potassium bromide and sodium iodide than (2:0,1.5:0.5,1:1,0.5:1.5,0:2) are dissolved in above-mentioned mixed solution, continue to stir 1h;Add
Enter the sodium hydroxide solution (1molL of 5.5mL-1) solution ph is adjusted to 10.5, continue stirring until forming uniform suspension
Then liquid is transferred in stainless steel autoclave of the 50mL containing polytetrafluoroethylliner liner, reacts 16h at 160 DEG C, gained is produced
Object centrifuge separation, and it is dry at 60 DEG C, obtain Bi4O5BrI mischcrystal photocatalyst.Obtained Bi4O5The XRD of BrI sample
As a result as shown in Figure 5, it can be seen that product is not pure phase Bi4O5BrI structure contains impurity diffraction maximum.
Although the present invention has been described by way of example and in terms of the preferred embodiments, it is not intended to limit the invention, any to be familiar with this skill
The people of art can do various change and modification, therefore protection model of the invention without departing from the spirit and scope of the present invention
Enclosing subject to the definition of the claims.
Claims (10)
1. a kind of Bi4O5BrxI2-xThe preparation method of mischcrystal photocatalyst, which is characterized in that the described method comprises the following steps:
(1) by water and polyethylene glycol with volume ratio (0~1): 1 preparation obtains mixed solvent, and bismuth nitrate is added, and stirs 0.5~3h;
(2) bromide and iodide for weighing different mol ratio are dissolved in above-mentioned mixed solution, continue 0.5~3h of stirring;
(3) it is 10~11 that alkali, which is added, and adjusts solution ph, continues stirring until forming uniform suspension;
(4) above-mentioned suspension is transferred in reaction kettle, 12~18h is reacted at 120~180 DEG C, product is separated by solid-liquid separation, done
It is dry, a series of Bi of different proportions can be prepared4O5BrxI2-xMischcrystal photocatalyst, wherein x meets: 0≤x≤2.
2. a kind of Bi according to claim 14O5BrxI2-xThe preparation method of mischcrystal photocatalyst, which is characterized in that institute
Stating polyethylene glycol is one of polyethylene glycol 200, polyethylene glycol 400.
3. a kind of Bi according to claim 1 or 24O5BrxI2-xThe preparation method of mischcrystal photocatalyst, feature exist
In final concentration of 0.03~0.1mol/L of the bismuth nitrate.
4. any a kind of Bi according to claim 1~34O5BrxI2-xThe preparation method of mischcrystal photocatalyst, feature
It is, the bromide is one of potassium bromide, sodium bromide.
5. a kind of Bi according to any one of claims 1 to 44O5BrxI2-xThe preparation method of mischcrystal photocatalyst, feature
It is, the iodide are one of potassium iodide, sodium iodide.
6. any a kind of Bi according to claim 1~54O5BrxI2-xThe preparation method of mischcrystal photocatalyst, feature
It is, the molar ratio of the bromide and iodide is unlimited.
7. a kind of Bi according to claim 64O5BrxI2-xThe preparation method of mischcrystal photocatalyst, which is characterized in that institute
The molar ratio for stating bromide and iodide is 1:1.
8. any a kind of Bi according to claim 1~74O5BrxI2-xThe preparation method of mischcrystal photocatalyst, feature
It is, the bismuth nitrate is 1:1 with the molar ratio of bromide and iodide summation.
9. any a kind of Bi according to claim 1~84O5BrxI2-xThe preparation method of mischcrystal photocatalyst, feature
It is, the drying is dry 6~12h at 50~80 DEG C.
10. a kind of any Bi of claim 1~94O5BrxI2-xThe preparation method of mischcrystal photocatalyst is led in photocatalysis
Application in domain or water treatment field.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201811510441.0A CN109364958A (en) | 2018-12-11 | 2018-12-11 | A kind of Bi4O5BrxI2-xThe preparation method of mischcrystal photocatalyst |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201811510441.0A CN109364958A (en) | 2018-12-11 | 2018-12-11 | A kind of Bi4O5BrxI2-xThe preparation method of mischcrystal photocatalyst |
Publications (1)
Publication Number | Publication Date |
---|---|
CN109364958A true CN109364958A (en) | 2019-02-22 |
Family
ID=65373138
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201811510441.0A Pending CN109364958A (en) | 2018-12-11 | 2018-12-11 | A kind of Bi4O5BrxI2-xThe preparation method of mischcrystal photocatalyst |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN109364958A (en) |
Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110508320A (en) * | 2019-08-22 | 2019-11-29 | 南京理工大学 | BiO(HCOO)xIyBr1-x-yThe solid-phase grinding preparation method of mischcrystal photocatalyst |
CN111097454A (en) * | 2019-12-13 | 2020-05-05 | 江南大学 | Two-dimensional heterostructure CuO/Bi4O5BrxI2-xComposite photocatalyst and preparation method thereof |
CN111604065A (en) * | 2020-05-14 | 2020-09-01 | 延安大学 | Preparation method of bismuth-rich two-dimensional nano bismuth oxyhalide-based photocatalyst |
CN111617786A (en) * | 2020-04-17 | 2020-09-04 | 延安大学 | Transition metal phosphide/bismuth oxyhalide photocatalyst and preparation method and application thereof |
CN111632610A (en) * | 2019-03-01 | 2020-09-08 | 南开大学 | BiOI capable of efficiently degrading perfluorinated compounds1-xFxSolid solution photocatalytic material and preparation method thereof |
CN111744507A (en) * | 2020-07-16 | 2020-10-09 | 南京信息工程大学 | Novel application of iodine-doped bismuth oxybromide photocatalyst in aspect of nitrogen fixation |
CN112517030A (en) * | 2020-12-15 | 2021-03-19 | 陕西科技大学 | Preparation method of BSO-BiOXmYn composite photocatalyst replaced by layer |
Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
KR100816424B1 (en) * | 2006-12-22 | 2008-03-25 | 인하대학교 산학협력단 | Photocatalyst having bismuthoxide-bismuthoxyhalide junction structure and preparation method thereof |
CN102553619A (en) * | 2011-12-22 | 2012-07-11 | 华中师范大学 | Visible-light catalyst Bi3O4Br and preparation method thereof |
CN104226339A (en) * | 2014-09-18 | 2014-12-24 | 玉林师范学院 | Visible-light-induced photocatalyst Bi4O5Br2 and preparation method thereof |
-
2018
- 2018-12-11 CN CN201811510441.0A patent/CN109364958A/en active Pending
Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
KR100816424B1 (en) * | 2006-12-22 | 2008-03-25 | 인하대학교 산학협력단 | Photocatalyst having bismuthoxide-bismuthoxyhalide junction structure and preparation method thereof |
CN102553619A (en) * | 2011-12-22 | 2012-07-11 | 华中师范大学 | Visible-light catalyst Bi3O4Br and preparation method thereof |
CN104226339A (en) * | 2014-09-18 | 2014-12-24 | 玉林师范学院 | Visible-light-induced photocatalyst Bi4O5Br2 and preparation method thereof |
Non-Patent Citations (2)
Title |
---|
乔玉洁: ""基于形貌调控的卤氧化铋及复合物的合成及其光催化性能"", 《中国优秀硕士学位论文全文数据库 程科技Ⅰ辑》 * |
王燕琴: ""卤氧化铋光催化剂的研究进展"", 《化工进展》 * |
Cited By (9)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111632610A (en) * | 2019-03-01 | 2020-09-08 | 南开大学 | BiOI capable of efficiently degrading perfluorinated compounds1-xFxSolid solution photocatalytic material and preparation method thereof |
CN110508320A (en) * | 2019-08-22 | 2019-11-29 | 南京理工大学 | BiO(HCOO)xIyBr1-x-yThe solid-phase grinding preparation method of mischcrystal photocatalyst |
CN111097454A (en) * | 2019-12-13 | 2020-05-05 | 江南大学 | Two-dimensional heterostructure CuO/Bi4O5BrxI2-xComposite photocatalyst and preparation method thereof |
CN111097454B (en) * | 2019-12-13 | 2023-07-04 | 江南大学 | Two-dimensional heterostructure CuO/Bi 4 O 5 Br x I 2-x Composite photocatalyst and preparation method thereof |
CN111617786A (en) * | 2020-04-17 | 2020-09-04 | 延安大学 | Transition metal phosphide/bismuth oxyhalide photocatalyst and preparation method and application thereof |
CN111617786B (en) * | 2020-04-17 | 2022-12-23 | 延安大学 | Transition metal phosphide/bismuth oxyhalide photocatalyst and preparation method and application thereof |
CN111604065A (en) * | 2020-05-14 | 2020-09-01 | 延安大学 | Preparation method of bismuth-rich two-dimensional nano bismuth oxyhalide-based photocatalyst |
CN111744507A (en) * | 2020-07-16 | 2020-10-09 | 南京信息工程大学 | Novel application of iodine-doped bismuth oxybromide photocatalyst in aspect of nitrogen fixation |
CN112517030A (en) * | 2020-12-15 | 2021-03-19 | 陕西科技大学 | Preparation method of BSO-BiOXmYn composite photocatalyst replaced by layer |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN109364958A (en) | A kind of Bi4O5BrxI2-xThe preparation method of mischcrystal photocatalyst | |
CN106076421B (en) | A kind of MIL-53 (Fe)/g-C3N4The preparation method of nanometer sheet composite photocatalyst material | |
CN106582765B (en) | A kind of the natrium doping graphite phase carbon nitride and its application of one-step synthesis preparation | |
CN107029770B (en) | A kind of preparation method of metastable phase bismuth oxide and its application in photocatalysis degradation organic contaminant | |
CN102249395B (en) | Water ozonization treatment method by taking cerium oxide nanomaterial as catalyst | |
CN107649168B (en) | Method for degrading bisphenol A in water through photocatalysis and catalyst used by method | |
CN106552651B (en) | Bi12O17Br2Synthesis and application method of photocatalyst | |
CN110639620A (en) | Composite photocatalyst for degrading tetracycline and preparation method and application thereof | |
CN106391086A (en) | Preparation method of C3N4/SiO2 heterojunction photocatalyst | |
CN110180565B (en) | Photocatalyst Bi5O7Synthetic method of Br and application thereof | |
CN110465318A (en) | Hollow nitride porous carbon ball composite photo-catalyst of a kind of carbon quantum dot load and its preparation method and application | |
CN106166495B (en) | A kind of sulfur doping oxygen-starved TiO2The preparation method of photochemical catalyst | |
CN108554407A (en) | Nano-copper base catalyst and preparation method thereof | |
CN107744814A (en) | A kind of preparation method and application of composite photo-catalyst | |
CN110339854A (en) | A kind of p-n homojunction carbonitride@cube argentum nano composite material and preparation method thereof of cyano modulation | |
CN103447033B (en) | Method for preparing mesoporous AgGaO2 photocatalytic material | |
CN108246306B (en) | One-pot synthesis of photocatalyst CuBi with visible light response2O4/Bi2WO6Nanosphere and application thereof | |
CN116351438A (en) | Cerium oxide indium sulfide photocatalytic material and preparation method and application thereof | |
CN113769726B (en) | Preparation method and application of rare earth vanadate quantum dot/biochar nanosheet composite photocatalytic material | |
CN107597155B (en) | One-pot synthesis of visible-light-responsive photocatalyst BiPO4/WO3Preparation method of nanosheet | |
CN111793218B (en) | Preparation method and application of Schiff base dicarboxylic acid ligand Zn and Cu metal organic framework material | |
CN115010101A (en) | Preparation method and application of carbon nitride nanosheet with wide spectral response and high crystallinity | |
CN114433132A (en) | Method for synthesizing Z-type heterojunction catalytic material by ultrasonic-assisted method | |
CN113908862A (en) | Preparation method of BiOCl-GO visible light photocatalyst | |
CN107737598A (en) | A kind of Cu1.8Se/CuAgSe composite photocatalyst materials and preparation method thereof |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190222 |
|
RJ01 | Rejection of invention patent application after publication |