CN106994356A - The preparation method of photochemical catalyst CdS NiS nano composite materials - Google Patents
The preparation method of photochemical catalyst CdS NiS nano composite materials Download PDFInfo
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- CN106994356A CN106994356A CN201710406910.3A CN201710406910A CN106994356A CN 106994356 A CN106994356 A CN 106994356A CN 201710406910 A CN201710406910 A CN 201710406910A CN 106994356 A CN106994356 A CN 106994356A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000003054 catalyst Substances 0.000 title claims abstract description 22
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 21
- 239000000463 material Substances 0.000 title claims abstract description 20
- 239000000047 product Substances 0.000 claims abstract description 31
- 238000005119 centrifugation Methods 0.000 claims abstract description 24
- 229910052976 metal sulfide Inorganic materials 0.000 claims abstract description 22
- 229910052793 cadmium Inorganic materials 0.000 claims abstract description 21
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000005406 washing Methods 0.000 claims abstract description 20
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000000203 mixture Substances 0.000 claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 10
- 238000009835 boiling Methods 0.000 claims abstract description 9
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 9
- 229910052979 sodium sulfide Inorganic materials 0.000 claims abstract description 9
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000012265 solid product Substances 0.000 claims abstract description 9
- 239000007788 liquid Substances 0.000 claims abstract description 7
- 239000003960 organic solvent Substances 0.000 claims abstract description 7
- 238000005979 thermal decomposition reaction Methods 0.000 claims abstract description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 239000008236 heating water Substances 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 5
- 238000009938 salting Methods 0.000 claims abstract description 5
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 12
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical group Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 12
- 238000000354 decomposition reaction Methods 0.000 claims description 7
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 6
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 6
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 6
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 6
- 239000005642 Oleic acid Substances 0.000 claims description 6
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 6
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid group Chemical group C(CCCCCCC\C=C/CCCCCCCC)(=O)O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 6
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 claims description 4
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 229940078494 nickel acetate Drugs 0.000 claims description 3
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 3
- 150000002815 nickel Chemical class 0.000 claims description 2
- 239000011941 photocatalyst Substances 0.000 claims 1
- 230000035484 reaction time Effects 0.000 claims 1
- 230000015556 catabolic process Effects 0.000 abstract description 5
- 238000006731 degradation reaction Methods 0.000 abstract description 5
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 abstract description 5
- 229940043267 rhodamine b Drugs 0.000 abstract description 5
- 230000002045 lasting effect Effects 0.000 abstract description 4
- 229960000907 methylthioninium chloride Drugs 0.000 abstract description 2
- 238000012876 topography Methods 0.000 abstract description 2
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 abstract 1
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 abstract 1
- 229940012189 methyl orange Drugs 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 20
- 238000006243 chemical reaction Methods 0.000 description 8
- 239000007787 solid Substances 0.000 description 8
- -1 benzo thiophenes Azoles Chemical class 0.000 description 5
- 238000000034 method Methods 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000003643 water by type Substances 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- IOJUPLGTWVMSFF-UHFFFAOYSA-N benzothiazole Chemical compound C1=CC=C2SC=NC2=C1 IOJUPLGTWVMSFF-UHFFFAOYSA-N 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000001699 photocatalysis Effects 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- CXKWCBBOMKCUKX-UHFFFAOYSA-M methylene blue Chemical compound [Cl-].C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 CXKWCBBOMKCUKX-UHFFFAOYSA-M 0.000 description 1
- 238000000593 microemulsion method Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 230000001052 transient effect Effects 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
- B01J27/04—Sulfides
- B01J27/043—Sulfides with iron group metals or platinum group metals
-
- B01J35/39—
-
- 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
-
- 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
- C02F1/32—Treatment of water, waste water, or sewage by irradiation with ultraviolet light
-
- 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
-
- 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 invention discloses the preparation method of photochemical catalyst CdS NiS nano composite materials, 0.8 2g mercaptobenzothiazolers conjunction cadmium is put into 50 100 mL high boiling organic solvent, heating for dissolving obtains uniform solution, continuous heating to make mercaptobenzothiazoler close cadmium thermal decomposition, cooling, solid product is obtained after washing centrifugation；Products therefrom is added in 20 80 mL saturation sodium sulfide solutions, heating water bath simultaneously continues stirring, then removes unnecessary sulphion and centrifugation with absolute ethyl alcohol to product, obtains centrifuging product；The centrifugation product obtained is distributed in water, is then mixed with soluble nickel salting liquid, and lasting stirring makes after it fully reacts, and centrifuge washing, drying obtains composition metal sulfide CdS NiS.The sample topography that the present invention is obtained is regular, size uniformity, can effectively absorb ultraviolet light and visible ray, and to organic pollution thing rhodamine B, methylene blue, methyl orange has significant degradation.
Description
Technical field
The invention belongs to technical field of nano material, more particularly to a kind of photochemical catalyst CdS-NiS nano composite materials
Preparation method.
Background technology
Photocatalysis technology is due to its application in terms of solar energy is converted into Hydrogen Energy and photocatalytic degradation organic compound
Increasingly paid close attention to by people.With TiO2For representative conventional oxide photochemical catalyst because its band gap wide (3.2 eV) it is narrow,
Ultraviolet and near ultraviolet ray can only be responded, the utilization rate to solar energy is low (about 5%), greatly constrains its marketing development,
Therefore more research sight have turned to transient metal sulfide instantly.
Metal sulfide is ideal for the absorption performance of visible ray, but single metal sulfide is unstable under light illumination
It is fixed, easily occur photoetch and the phenomenon such as photo-generate electron-hole is compound, its photocatalytic activity is declined rapidly.In order to solve these
Problem, people are modified using multiple means to metal sulfide, such as：Metal ion mixing, metal-modified and semiconductor are multiple
Close etc..
The preparation method of current metal sulfide mainly has solid phase decomposition method, hydro-thermal method, microemulsion method, solvent-thermal process
Method, sol-gel process and template etc..These methods more or less all have a little defect, as required by hydro-thermal method
The equipment requirement of every reaction condition pair is higher；The raw material that sol-gel process is used costly and reaction the time required to compared with
It is long；The corresponding preparation process such as template is relatively complicated；Problems result in photochemical catalyst and can not mass produce, be applied to
In real life.
Therefore, it is very necessary to seek a kind of new, simplicity, effective composition metal sulfide preparation method.
The content of the invention
The present invention provides a kind of preparation method of photochemical catalyst CdS-NiS nano composite materials, to solve in the prior art
The problem of.
To achieve the above object, the technical solution adopted by the present invention is：
A kind of preparation method of photochemical catalyst CdS-NiS nano composite materials, comprises the following steps：
Step（1）, by 0.8-2g mercaptobenzothiazolers conjunction cadmium be put into 50-100 mL high boiling organic solvent, dissolve by heating
Uniform solution is obtained, continuous heating is to making mercaptobenzothiazoler close cadmium thermal decomposition, and cooling obtains solid product after washing centrifugation,
It is then CdS；
Step（2）, by step（1）Middle products therefrom is added in 20-80 mL saturation sodium sulfide solutions, and heating water bath simultaneously continues
Stirring, then removes unnecessary sulphion and centrifugation to product with absolute ethyl alcohol, obtains centrifuging product；
Step（3）, take step（2）Obtained centrifugation product is distributed in water, is then mixed, is persistently stirred with soluble nickel salting liquid
Mixing makes after it fully reacts, and centrifuge washing, drying obtains composition metal sulfide CdS-NiS.
Further, the step（1）Middle mercaptobenzothiazoler closes solution temperature of the cadmium in high boiling organic solvent
100-140℃。
Further, the step（1）In, high boiling organic solvent is oleic acid or oleyl amine, and its boiling point is higher than sulfydryl benzo
Thiazole closes the decomposition temperature of cadmium.
Further, the step（1）In, the decomposition reaction temperature that mercaptobenzothiazoler closes cadmium is 270 DEG C -300 DEG C, instead
It is 5-60 min between seasonable.
Further, the step（1）In, chilling temperature is to 20-40 DEG C after decomposition reaction.
Further, the step（2）In, bath temperature is 60-70 DEG C.
Further, the step（3）In, carried out at a temperature of being blended in 60 DEG C -70 DEG C with soluble nickel salting liquid.
Further, the step（3）Middle soluble nickel salt is nickel chloride, nickel acetate or nickel nitrate.
Further, the step（3）In, drying temperature is 40-60 DEG C.
Compared with prior art, the invention has the advantages that：
The preparation method of the NEW TYPE OF COMPOSITE metal sulfide provided is invented, obtained sample topography is regular, size uniformity, Neng Gouyou
The absorption ultraviolet light and visible ray of effect, to organic pollution thing rhodamine B, methylene blue has significant degradation, in 30min
Within, to the degradation efficiency of rhodamine B up to more than 99%.
Brief description of the drawings
Fig. 1 is the XRD of product prepared by the embodiment of the present invention 4；
Fig. 2 is the SEM figures of product prepared by the embodiment of the present invention 4；
Fig. 3 is the SEM figures of product rhodamine B degradation prepared by the embodiment of the present invention 4.
Embodiment
The present invention is further described with reference to embodiment.
Embodiment 1
A kind of preparation method of photochemical catalyst CdS-NiS nano composite materials, comprises the following steps：By 1.5 g sulfydryl benzo thiophenes
Azoles closes cadmium and is added in the three-necked flask for 250 mL for filling 80 mL oleic acid, and being persistently stirred and heated to 100 DEG C makes solid dissolving
Afterwards, continuing to be heated to 240 DEG C of isothermal reactions makes complex thermal decomposition complete for 5 minutes.Solid product washing centrifugation is taken after cooling, is taken
Go out undesired impurities, be added in 50 mL saturation sodium sulfide solutions, heated 5 minutes in 65 DEG C of waters bath with thermostatic control, washing is centrifuged off many
Remaining sulphion, then solid product is dissolved in water, in 65 DEG C of water bath with thermostatic control heating, and 50 mL concentration ratios are slowly added dropwise for 0.15 g
:50 mL nickel chloride aqueous solution, is added dropwise completely follow-up continuous reaction and stops heating in 5 minutes, take gained solid to be washed with deionization
Centrifugation is washed, the composition metal sulfide CdS-NiS of 10%Ni doping is obtained.
Embodiment 2
It is identical with terms and conditions in embodiment 1, the nickel chloride solution concentration ratio of dropwise addition is changed to 0.3 g:50 mL, obtain 20%
The composition metal sulfide CdS-NiS of Ni doping.
Embodiment 3
It is identical with terms and conditions in embodiment 1, the nickel chloride solution concentration ratio of dropwise addition is changed to 0.45 g:50 mL, obtain 30%
The composition metal sulfide CdS-NiS of Ni doping.
Embodiment 4
It is identical with terms and conditions in embodiment 1, the nickel chloride solution concentration ratio of dropwise addition is changed to 0.6 g:50 mL, obtain 40%Ni
The composition metal sulfide CdS-NiS of doping；As shown in figure 3, within 30min, to the degradation efficiency of rhodamine B up to 99% with
On.
Embodiment 5
It is identical with terms and conditions in embodiment 1, the nickel chloride solution concentration ratio of dropwise addition is changed to 0.75 g:50 mL, obtain 50%
The composition metal sulfide CdS-NiS of Ni doping.
Embodiment 6
It is identical with terms and conditions in embodiment 1, the nickel chloride solution concentration ratio of dropwise addition is changed to 1.05 g:50 mL, are obtained
The composition metal sulfide CdS-NiS of 70%Ni doping.
Embodiment 7
It is identical with terms and conditions in embodiment 1, the nickel chloride solution concentration ratio of dropwise addition is changed to 1.35 g:50 mL, are obtained
The composition metal sulfide CdS-NiS of 90%Ni doping.
Embodiment 8
A kind of preparation method of photochemical catalyst CdS-NiS nano composite materials, comprises the following steps：By 1.5 g sulfydryl benzo thiophenes
Azoles closes cadmium and is added in the three-necked flask for 250 mL for filling 80 mL oleic acid, and being persistently stirred and heated to 100 DEG C makes solid dissolving
Afterwards, continuing to be heated to 240 DEG C of isothermal reactions makes complex thermal decomposition complete for 15 minutes.Solid product washing centrifugation is taken after cooling,
Undesired impurities are taken out, are added in 50 mL saturation sodium sulfide solutions, are heated 5 minutes in 65 DEG C of waters bath with thermostatic control, washing is centrifuged off
Redundant sulfide ions, then solid product is dissolved in water, in 65 DEG C of water bath with thermostatic control heating, and it is 0.75 that 50 mL concentration ratios, which are slowly added dropwise,
g :50 mL nickel chloride aqueous solution, is added dropwise completely follow-up continuous reaction and stops heating in 5 minutes, take gained solid with deionized water
Washing centrifugation, obtains product composition metal sulfide CdS-NiS.
Embodiment 9
A kind of preparation method of photochemical catalyst CdS-NiS nano composite materials, comprises the following steps：By 1.5 g sulfydryl benzo thiophenes
Azoles closes cadmium and is added in the three-necked flask for 250 mL for filling 80 mL oleic acid, and being persistently stirred and heated to 100 DEG C makes solid dissolving
Afterwards, continuing to be heated to 240 DEG C of isothermal reactions makes complex thermal decomposition complete for 25 minutes.Solid product washing centrifugation is taken after cooling,
Undesired impurities are taken out, are added in 50 mL saturation sodium sulfide solutions, are heated 5 minutes in 65 DEG C of waters bath with thermostatic control, washing is centrifuged off
Redundant sulfide ions, then solid product is dissolved in water, in 65 DEG C of water bath with thermostatic control heating, and it is 0.75 that 50 mL concentration ratios, which are slowly added dropwise,
g :50 mL nickel chloride aqueous solution, is added dropwise completely follow-up continuous reaction and stops heating in 5 minutes, take gained solid with deionized water
Washing centrifugation, obtains product composition metal sulfide CdS-NiS.
Embodiment 10
A kind of preparation method of photochemical catalyst CdS-NiS nano composite materials, comprises the following steps：
Step（1）, by 0.8g mercaptobenzothiazolers conjunction cadmium be put into 50mL oleyl amine, be heated to 100 DEG C of dissolvings and obtain homogeneous molten
Liquid, continuous heating makes mercaptobenzothiazoler close cadmium thermal decomposition 5min to 270 DEG C, is cooled to 20 DEG C, solid is obtained after washing centrifugation
Product, then be CdS；
Step（2）, by step（1）Middle products therefrom is added in 20 mL saturation sodium sulfide solutions, in 60 DEG C of heating water baths and is held
Continuous stirring, then removes unnecessary sulphion and centrifugation to product with absolute ethyl alcohol, obtains centrifuging product；
Step（3）, take step（2）Obtained centrifugation product is distributed in water, then at a temperature of 60 DEG C with soluble nickel chloride
Solution is mixed, and lasting stirring makes after it fully reacts, and centrifuge washing is dried at 40 DEG C, obtains composition metal sulfide CdS-
NiS。
Embodiment 11
A kind of preparation method of photochemical catalyst CdS-NiS nano composite materials, comprises the following steps：
Step（1）, by 1.5g mercaptobenzothiazolers conjunction cadmium be put into 80 mL oleyl amine, be heated to 130 DEG C of dissolvings and obtain homogeneous molten
Liquid, continuous heating makes mercaptobenzothiazoler close cadmium to thermally decompose 30 min, be cooled to 30 DEG C, after washing centrifugation consolidated to 280 DEG C
Body product, then be CdS；
Step（2）, by step（1）Middle products therefrom is added in 70 mL saturation sodium sulfide solutions, in 62 DEG C of heating water baths and is held
Continuous stirring, then removes unnecessary sulphion and centrifugation to product with absolute ethyl alcohol, obtains centrifuging product；
Step（3）, take step（2）Obtained centrifugation product is distributed in water, then at a temperature of 65 DEG C with soluble nickel acetate
Solution is mixed, and lasting stirring makes after it fully reacts, and centrifuge washing is dried at 40-60 DEG C, obtains composition metal sulfide
CdS-NiS。
Embodiment 12
A kind of preparation method of photochemical catalyst CdS-NiS nano composite materials, comprises the following steps：
Step（1）, by 2g mercaptobenzothiazolers conjunction cadmium be put into 100 mL oleic acid, be heated to 140 DEG C of dissolvings and obtain uniform solution,
Continuous heating makes mercaptobenzothiazoler close cadmium to thermally decompose 60 min, be cooled to 40 DEG C, solid production is obtained after washing centrifugation to 300 DEG C
Thing, then be CdS；
Step（2）, by step（1）Middle products therefrom is added in 20-80 mL saturation sodium sulfide solutions, in 70 DEG C of heating water baths
And continue stirring, unnecessary sulphion and centrifugation then are removed with absolute ethyl alcohol to product, obtain centrifuging product；
Step（3）, take step（2）Obtained centrifugation product is distributed in water, then at a temperature of 70 DEG C with soluble nickel nitrate
Solution is mixed, and lasting stirring makes after it fully reacts, and centrifuge washing is dried at 60 DEG C, obtains composition metal sulfide CdS-
NiS。
Described above is only the preferred embodiment of the present invention, it should be pointed out that：For the ordinary skill people of the art
For member, under the premise without departing from the principles of the invention, some improvements and modifications can also be made, these improvements and modifications also should
It is considered as protection scope of the present invention.
Claims (9)
1. a kind of preparation method of photochemical catalyst CdS-NiS nano composite materials, it is characterised in that comprise the following steps：
Step（1）, by 0.8-2g mercaptobenzothiazolers conjunction cadmium be put into 50-100 mL high boiling organic solvent, dissolve by heating
Uniform solution is obtained, continuous heating is to making mercaptobenzothiazoler close cadmium thermal decomposition, and cooling obtains solid product after washing centrifugation,
It is then CdS；
Step（2）, by step（1）Middle products therefrom is added in 20-80 mL saturation sodium sulfide solutions, and heating water bath simultaneously continues
Stirring, then removes unnecessary sulphion and centrifugation to product with absolute ethyl alcohol, obtains centrifuging product；
Step（3）, take step（2）Obtained centrifugation product is distributed in water, is then mixed, is persistently stirred with soluble nickel salting liquid
Mixing makes after it fully reacts, and centrifuge washing, drying obtains composition metal sulfide CdS-NiS.
2. the preparation method of photochemical catalyst CdS-NiS nano composite materials according to claim 1, it is characterised in that：Institute
State step（1）It is 100-140 DEG C that middle mercaptobenzothiazoler, which closes solution temperature of the cadmium in high boiling organic solvent,.
3. the preparation method of photochemical catalyst CdS-NiS nano composite materials according to claim 1, it is characterised in that：Institute
State step（1）In, high boiling organic solvent is oleic acid or oleyl amine, and its boiling point closes the decomposition temperature of cadmium higher than mercaptobenzothiazoler.
4. the preparation method of photochemical catalyst CdS-NiS nano composite materials according to claim 1, it is characterised in that：Institute
State step（1）In, the decomposition reaction temperature that mercaptobenzothiazoler closes cadmium is 270 DEG C -300 DEG C, and the reaction time is 5-60 min.
5. the preparation method of photochemical catalyst CdS-NiS nano composite materials according to claim 1, it is characterised in that：Institute
State step（1）In, chilling temperature is to 20-40 DEG C after decomposition reaction.
6. the preparation method of photochemical catalyst CdS-NiS nano composite materials according to claim 1, it is characterised in that：Institute
State step（2）In, bath temperature is 60-70 DEG C.
7. the preparation method of photochemical catalyst CdS-NiS nano composite materials according to claim 1, it is characterised in that：Institute
State step（3）In, carried out at a temperature of being blended in 60 DEG C -70 DEG C with soluble nickel salting liquid.
8. the preparation method of CdS-CuS nano composite photo-catalysts according to claim 1, it is characterised in that：The step
Suddenly（3）Middle soluble nickel salt is nickel chloride, nickel acetate or nickel nitrate.
9. the preparation method of photochemical catalyst CdS-NiS nano composite materials according to claim 1, it is characterised in that：Institute
State step（3）In, drying temperature is 40-60 DEG C.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107349938A (en) * | 2017-09-06 | 2017-11-17 | 北京邮电大学 | A kind of nickel sulfide cadmium sulfide nano wires heterojunction structure and preparation method thereof |
| CN110302814A (en) * | 2019-08-02 | 2019-10-08 | 谢明财 | A kind of compound assemble method of CdS Semiconductor Nanometer Particles |
| CN112958118A (en) * | 2021-03-15 | 2021-06-15 | 北京化工大学 | Double-sulfide composite material and preparation method and application thereof |
| CN114634746A (en) * | 2022-02-14 | 2022-06-17 | 烟台大学 | Fluorescent self-warning, corrosion-inhibition and self-repairing nano anticorrosive coating and preparation method thereof |
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| CN107349938A (en) * | 2017-09-06 | 2017-11-17 | 北京邮电大学 | A kind of nickel sulfide cadmium sulfide nano wires heterojunction structure and preparation method thereof |
| CN107349938B (en) * | 2017-09-06 | 2019-11-12 | 北京邮电大学 | A kind of nickel sulfide-cadmium sulfide nano wires heterojunction structure and preparation method thereof |
| CN110302814A (en) * | 2019-08-02 | 2019-10-08 | 谢明财 | A kind of compound assemble method of CdS Semiconductor Nanometer Particles |
| CN112958118A (en) * | 2021-03-15 | 2021-06-15 | 北京化工大学 | Double-sulfide composite material and preparation method and application thereof |
| CN112958118B (en) * | 2021-03-15 | 2023-07-25 | 北京化工大学 | Double sulfide composite material and preparation method and application thereof |
| CN114634746A (en) * | 2022-02-14 | 2022-06-17 | 烟台大学 | Fluorescent self-warning, corrosion-inhibition and self-repairing nano anticorrosive coating and preparation method thereof |
| CN114634746B (en) * | 2022-02-14 | 2022-10-25 | 烟台大学 | Fluorescent self-warning, corrosion-inhibition and self-repairing nano anticorrosive coating and preparation method thereof |
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