CN107519898A - The preparation method of cadmium selenide-bismuth tungstate composite photocatalyst - Google Patents
The preparation method of cadmium selenide-bismuth tungstate composite photocatalyst Download PDFInfo
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- CN107519898A CN107519898A CN201610458295.6A CN201610458295A CN107519898A CN 107519898 A CN107519898 A CN 107519898A CN 201610458295 A CN201610458295 A CN 201610458295A CN 107519898 A CN107519898 A CN 107519898A
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- solution
- bismuth
- preparation
- cadmium selenide
- composite photocatalyst
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- PBYZMCDFOULPGH-UHFFFAOYSA-N tungstate Chemical compound [O-][W]([O-])(=O)=O PBYZMCDFOULPGH-UHFFFAOYSA-N 0.000 title claims abstract description 40
- LPCKVWBOWUPESZ-UHFFFAOYSA-N bismuth cadmium(2+) selenium(2-) Chemical compound [Bi+3].[Se-2].[Cd+2] LPCKVWBOWUPESZ-UHFFFAOYSA-N 0.000 title claims abstract description 26
- 239000002131 composite material Substances 0.000 title claims abstract description 25
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000000243 solution Substances 0.000 claims abstract description 40
- 239000011259 mixed solution Substances 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- UHYPYGJEEGLRJD-UHFFFAOYSA-N cadmium(2+);selenium(2-) Chemical class [Se-2].[Cd+2] UHYPYGJEEGLRJD-UHFFFAOYSA-N 0.000 claims abstract description 15
- 229910052797 bismuth Inorganic materials 0.000 claims abstract description 14
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000008367 deionised water Substances 0.000 claims abstract description 13
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 13
- BUGBHKTXTAQXES-UHFFFAOYSA-N Selenium Chemical compound [Se] BUGBHKTXTAQXES-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000005984 hydrogenation reaction Methods 0.000 claims abstract description 9
- 229910052711 selenium Inorganic materials 0.000 claims abstract description 9
- 239000011669 selenium Substances 0.000 claims abstract description 9
- OISMQLUZKQIKII-UHFFFAOYSA-L dichlorocadmium;hydrate Chemical compound O.[Cl-].[Cl-].[Cd+2] OISMQLUZKQIKII-UHFFFAOYSA-L 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 5
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 claims description 23
- 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 description 20
- 239000002243 precursor Substances 0.000 claims description 14
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 7
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 7
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- DKIDEFUBRARXTE-UHFFFAOYSA-N 3-mercaptopropanoic acid Chemical class OC(=O)CCS DKIDEFUBRARXTE-UHFFFAOYSA-N 0.000 claims description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- 238000005406 washing Methods 0.000 claims description 4
- 235000011121 sodium hydroxide Nutrition 0.000 claims description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 2
- 238000002242 deionisation method Methods 0.000 claims description 2
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 2
- -1 polyethylene Pyrrolidones Polymers 0.000 claims description 2
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 2
- 239000012279 sodium borohydride Substances 0.000 claims description 2
- 230000003197 catalytic effect Effects 0.000 abstract description 3
- PMNLUUOXGOOLSP-UHFFFAOYSA-N 2-mercaptopropanoic acid Chemical class CC(S)C(O)=O PMNLUUOXGOOLSP-UHFFFAOYSA-N 0.000 abstract 1
- 238000000034 method Methods 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 239000003381 stabilizer Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 1
- 229910000238 buergerite Inorganic materials 0.000 description 1
- 229910052793 cadmium Inorganic materials 0.000 description 1
- RDVQTQJAUFDLFA-UHFFFAOYSA-N cadmium Chemical compound [Cd][Cd][Cd][Cd][Cd][Cd][Cd][Cd][Cd] RDVQTQJAUFDLFA-UHFFFAOYSA-N 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- WGPCGCOKHWGKJJ-UHFFFAOYSA-N sulfanylidenezinc Chemical compound [Zn]=S WGPCGCOKHWGKJJ-UHFFFAOYSA-N 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 229910052984 zinc sulfide Inorganic materials 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
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/057—Selenium or tellurium; Compounds thereof
- B01J27/0573—Selenium; 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Catalysts (AREA)
Abstract
This application discloses a kind of preparation method of cadmium selenide bismuth tungstate composite photocatalyst, including step：(1), by chloride hydrate cadmium, 3 mercaptopropionic acids according to 1:(1.5~1.7) mol ratio dissolves in deionized water, forms mixed solution, regulation pH value of solution to 7~8；Selenium hydrogenation is added in mixed solution and receives presoma, react 30~35 minutes at 160~170 DEG C, acquisition CdSe quantum dots；(2), by CdSe quantum dots and bismuth tungstate dissolving in deionized water, flowed back 20~25 hours at 80~90 DEG C, centrifugal drying obtains cadmium selenide bismuth tungstate composite photocatalyst.The cadmium selenide bismuth tungstate composite photocatalyst that the present invention obtains has good catalytic activity, stability height.
Description
Technical field
The application belongs to technical field of waste water processing, is urged more particularly to a kind of cadmium selenide-bismuth tungstate complex light
The preparation method of agent.
Background technology
Cadmium selenide is the direct band-gap semicondictor material that energy gap is 1.7eV, has cubic zinc blende and six
Square two kinds of crystal structures of buergerite, wherein cube phase structure is metastable state, can be only present in lower temperature,
It is changed into hexagonal phase structure during high temperature.Cadmium selenide at normal temperatures can simultaneously exist cube and six sides, two kinds of crystalline phases.
Cadmium selenide nano-crystal is to be studied in semiconductor nano most extensively, the best a kind of II-VI group of application prospect half
Conductor is nanocrystalline, because it has important nonlinear optical property, luminosity and other physical chemistry
Characteristic and enjoy attracting attention for common people.As a kind of very important semi-conducting material, various luminous
Device, laser and infrared detector, the neck such as infrared window and nonlinear optical material and light sensor
The wide application prospect of domain views.Particularly cadmium selenide can absorb visible ray well, thus it is light
The preferred material of chemical catalyst.
Cadmium selenide easily photoetch, photostability is poor, and the light absorbs threshold value of titanium dioxide is confined to ultraviolet light
Go, sun utilization rate is low, and these deficiencies strongly limit the performance of their performances.
The content of the invention
It is an object of the invention to provide a kind of preparation method of cadmium selenide-bismuth tungstate composite photocatalyst, with
Overcome 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 of cadmium selenide-bismuth tungstate composite photocatalyst, including step
Suddenly：
(1), by chloride hydrate cadmium, 3- mercaptopropionic acids according to 1:(1.5~1.7) mol ratio is dissolved in deionization
In water, mixed solution, regulation pH value of solution to 7~8 are formed；Selenium hydrogenation is added in mixed solution and receives forerunner
Body, reacted 30~35 minutes at 160~170 DEG C, obtain CdSe quantum dots；
(2), by CdSe quantum dots and bismuth tungstate dissolving in deionized water, in 80~90 DEG C of backflows 20~25
Hour, centrifugal drying obtains cadmium selenide-bismuth tungstate composite photocatalyst.
Preferably, in the preparation method of above-mentioned cadmium selenide-bismuth tungstate composite photocatalyst, step (1)
In, the preparation method of bismuth tungstate：It is first (3~5) according to the mass ratio between bismuth nitrate and nitric acid: 1
Ratio adds bismuth nitrate in the salpeter solution that concentration is (1~4) mol/L, obtains bismuth nitrate solution, then
It is (30~50) according to the mass ratio between sodium tungstate and deionized water: sodium tungstate is added and gone by 1 ratio
Stirred in ionized water, obtain sodium tungstate solution, then, polyvinylpyrrolidone is first added into wolframic acid
Stirred in sodium solution, obtain mixed solution, then bismuth nitrate solution is added in mixed solution, obtained
Precursor solution, then, 20~24h, cooling are incubated at being 160~180 DEG C in temperature by precursor solution
To room temperature, the processing through centrifuging, washing and dry, bismuth tungstate is obtained.
Preferably, in the preparation method of above-mentioned cadmium selenide-bismuth tungstate composite photocatalyst, mixed solution
In sodium tungstate and polyvinylpyrrolidone between mass ratio be (1.8~2.2)：1.
Preferably, in the preparation method of above-mentioned cadmium selenide-bismuth tungstate composite photocatalyst, precursor is molten
The mass ratio between bismuth nitrate and sodium tungstate in liquid is (2.8~3.2):1.
Preferably, in the preparation method of above-mentioned cadmium selenide-bismuth tungstate composite photocatalyst, hydroxide is used
Sodium adjusts pH value of solution to 7~8.
Preferably, in the preparation method of above-mentioned cadmium selenide-bismuth tungstate composite photocatalyst, selenium hydrogenation is received
The preparation method of presoma：By sodium borohydride and selenium powder according to 1:(7~8) mol ratio is dissolved in deionized water
In, mixed under logical condition of nitrogen gas, obtain selenium hydrogenation and receive precursor solution.
Compared with prior art, the advantage of the invention is that：Cadmium selenide-bismuth tungstate that the present invention obtains is compound
Photochemical catalyst has good catalytic activity, stability height.
Embodiment
The present invention is described further by the following example：, can be more preferably geographical according to following embodiments
The solution present invention.However, as it will be easily appreciated by one skilled in the art that specific material described by embodiment
The present invention is merely to illustrate than, process conditions and its result, without should be also without limitation on claims
In the described in detail present invention.
Embodiment 1
The preparation method of cadmium selenide-bismuth tungstate composite photocatalyst
(1), the preparation of bismuth tungstate
It is by bismuth nitrate addition concentration according to the ratio that the mass ratio between bismuth nitrate and nitric acid is 5: 1 first
At least 30min is stirred in 4mol/L salpeter solution, obtains bismuth nitrate solution, according still further to sodium tungstate with going
The ratio that mass ratio between ionized water is 50: 1, which adds sodium tungstate in deionized water, to stir, and obtains
To sodium tungstate solution, then, first polyvinylpyrrolidone is added in sodium tungstate solution and stirred, is obtained
To mixed solution, wherein, the mass ratio between sodium tungstate and polyvinylpyrrolidone in mixed solution is
1.8：1, then bismuth nitrate solution is added in mixed solution, precursor solution is obtained, wherein, precursor is molten
The mass ratio between bismuth nitrate and sodium tungstate in liquid is 2.8:1, then, first precursor solution is placed in close
Closed state, it is to be incubated 20h at 160 DEG C in temperature, then after it naturally cools to room temperature, through centrifuging,
Washing and the processing dried, obtain bismuth tungstate powder；
(2), by chloride hydrate cadmium, 3- mercaptopropionic acids (stabilizer) according to 1:1.55 mol ratios are dissolved in
In ionized water, mixed solution is formed, with sodium hydrate regulator solution pH to 7~8；Add in mixed solution
Enter selenium hydrogenation and receive presoma, react 30 minutes at 160 DEG C, acquisition CdSe quantum dots；
(3), by CdSe quantum dots and bismuth tungstate dissolving in deionized water, after stirring 10 minutes,
100 DEG C are flowed back 24 hours, and centrifugal drying obtains cadmium selenide-bismuth tungstate composite photocatalyst.
Cadmium selenide-bismuth tungstate composite photocatalyst of acquisition has good catalytic activity, stability height.
Embodiment 2
The preparation method of cadmium selenide-bismuth tungstate composite photocatalyst
(1), the preparation of bismuth tungstate
It is by bismuth nitrate addition concentration according to the ratio that the mass ratio between bismuth nitrate and nitric acid is 4: 1 first
At least 30min is stirred in 2mol/L salpeter solution, obtains bismuth nitrate solution, according still further to sodium tungstate with going
The ratio that mass ratio between ionized water is 50: 1, which adds sodium tungstate in deionized water, to stir, and obtains
To sodium tungstate solution, then, first polyvinylpyrrolidone is added in sodium tungstate solution and stirred, is obtained
To mixed solution, wherein, the mass ratio between sodium tungstate and polyvinylpyrrolidone in mixed solution is 2：
1, then bismuth nitrate solution is added in mixed solution, precursor solution is obtained, wherein, precursor solution
In bismuth nitrate and sodium tungstate between mass ratio be 3:1, then, first precursor solution is placed in closed
State, it is to be incubated 22h at 170 DEG C in temperature, then after it naturally cools to room temperature, through centrifuging, washing
The processing washed and dried, obtain bismuth tungstate powder；
(2), by chloride hydrate cadmium, 3- mercaptopropionic acids (stabilizer) according to 1:1.66 mol ratios are dissolved in
In ionized water, mixed solution is formed, with sodium hydrate regulator solution pH to 7；Added in mixed solution
Presoma is received in selenium hydrogenation, react 30 minutes at 160 DEG C, acquisition CdSe quantum dots；
(3), by CdSe quantum dots and bismuth tungstate dissolving in deionized water, after stirring 10 minutes,
100 DEG C are flowed back 22 hours, and centrifugal drying obtains cadmium selenide-bismuth tungstate composite photocatalyst.
Finally, it is to be noted that, term " comprising ", "comprising" or its any other variant are intended to
Nonexcludability includes, so that process, method, article or equipment including a series of elements are not
Only include those key elements, but also the other element including being not expressly set out, or it is this also to include
Kind of process, method, article or the intrinsic key element of equipment.
Claims (6)
1. a kind of preparation method of cadmium selenide-bismuth tungstate composite photocatalyst, it is characterised in that including step：
(1), by chloride hydrate cadmium, 3- mercaptopropionic acids according to 1:(1.5~1.7) mol ratio is dissolved in deionization
In water, mixed solution, regulation pH value of solution to 7~8 are formed；Selenium hydrogenation is added in mixed solution and receives forerunner
Body, reacted 30~35 minutes at 160~170 DEG C, obtain CdSe quantum dots；
(2), by CdSe quantum dots and bismuth tungstate dissolving in deionized water, in 80~90 DEG C of backflows 20~25
Hour, centrifugal drying obtains cadmium selenide-bismuth tungstate composite photocatalyst.
2. the preparation method of cadmium selenide-bismuth tungstate composite photocatalyst according to claim 1, it is special
Sign is：In step (1), the preparation method of bismuth tungstate：First according to the quality between bismuth nitrate and nitric acid
Than for (3~5): bismuth nitrate addition concentration is in (1~4) mol/L salpeter solution by 1 ratio, is obtained
It is (30~50): 1 ratio according still further to the mass ratio between sodium tungstate and deionized water to bismuth nitrate solution
Sodium tungstate is added in deionized water and stirred by example, sodium tungstate solution is obtained, then, first by polyethylene
Pyrrolidones is added in sodium tungstate solution and stirred, and obtains mixed solution, then bismuth nitrate solution is added
In mixed solution, precursor solution is obtained, then, is protected at being 160~180 DEG C in temperature by precursor solution
20~24h of temperature, after being cooled to room temperature, the processing through centrifuging, washing and dry, obtains bismuth tungstate.
3. the preparation method of cadmium selenide-bismuth tungstate composite photocatalyst according to claim 2, it is special
Sign is：The mass ratio between sodium tungstate and polyvinylpyrrolidone in mixed solution is (1.8~2.2)：
1。
4. the preparation method of cadmium selenide-bismuth tungstate composite photocatalyst according to claim 2, it is special
Sign is：The mass ratio between bismuth nitrate and sodium tungstate in precursor solution is (2.8~3.2):1.
5. the preparation method of cadmium selenide-bismuth tungstate composite photocatalyst according to claim 1, it is special
Sign is：With sodium hydrate regulator solution pH to 7~8.
6. the preparation method of cadmium selenide-bismuth tungstate composite photocatalyst according to claim 1, it is special
Sign is：The preparation method of presoma is received in selenium hydrogenation：By sodium borohydride and selenium powder according to 1:(7~8) mole
Than dissolving in deionized water, mixed under logical condition of nitrogen gas, obtain selenium hydrogenation and receive precursor solution.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610458295.6A CN107519898A (en) | 2016-06-22 | 2016-06-22 | The preparation method of cadmium selenide-bismuth tungstate composite photocatalyst |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610458295.6A CN107519898A (en) | 2016-06-22 | 2016-06-22 | The preparation method of cadmium selenide-bismuth tungstate composite photocatalyst |
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| CN201610458295.6A Withdrawn CN107519898A (en) | 2016-06-22 | 2016-06-22 | The preparation method of cadmium selenide-bismuth tungstate composite photocatalyst |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108568302A (en) * | 2018-04-08 | 2018-09-25 | 辽宁大学 | A kind of just symmetrical double Z shaped system sound catalyst SnO2–CdSe–Bi2O3And its preparation method and application |
| CN114632528A (en) * | 2022-03-30 | 2022-06-17 | 青岛科技大学 | Cadmium selenide/calcium molybdate photocatalyst and preparation method and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103623847A (en) * | 2013-11-22 | 2014-03-12 | 江苏大学 | Method for preparing CdSe-Bi2WO6 photocatalyst |
-
2016
- 2016-06-22 CN CN201610458295.6A patent/CN107519898A/en not_active Withdrawn
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103623847A (en) * | 2013-11-22 | 2014-03-12 | 江苏大学 | Method for preparing CdSe-Bi2WO6 photocatalyst |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108568302A (en) * | 2018-04-08 | 2018-09-25 | 辽宁大学 | A kind of just symmetrical double Z shaped system sound catalyst SnO2–CdSe–Bi2O3And its preparation method and application |
| CN114632528A (en) * | 2022-03-30 | 2022-06-17 | 青岛科技大学 | Cadmium selenide/calcium molybdate photocatalyst and preparation method and application thereof |
| CN114632528B (en) * | 2022-03-30 | 2023-07-25 | 青岛科技大学 | Cadmium selenide/calcium molybdate photocatalyst and preparation method and application thereof |
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Application publication date: 20171229 |