CN109622015A - A kind of preparation method of cadmium doped zinc sulphide/carbonitride - Google Patents
A kind of preparation method of cadmium doped zinc sulphide/carbonitride Download PDFInfo
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- CN109622015A CN109622015A CN201811529968.8A CN201811529968A CN109622015A CN 109622015 A CN109622015 A CN 109622015A CN 201811529968 A CN201811529968 A CN 201811529968A CN 109622015 A CN109622015 A CN 109622015A
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- carbonitride
- doped zinc
- zinc sulphide
- cadmium doped
- ultrasonic disperse
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- 239000005083 Zinc sulfide Substances 0.000 title claims abstract description 21
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 229910052793 cadmium Inorganic materials 0.000 title claims abstract description 20
- BDOSMKKIYDKNTQ-UHFFFAOYSA-N cadmium atom Chemical compound [Cd] BDOSMKKIYDKNTQ-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 27
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 22
- 230000001699 photocatalysis Effects 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 11
- 229920000877 Melamine resin Polymers 0.000 claims abstract description 9
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 claims abstract description 9
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000004246 zinc acetate Substances 0.000 claims abstract description 7
- 239000004570 mortar (masonry) Substances 0.000 claims description 16
- 239000000843 powder Substances 0.000 claims description 16
- 238000007146 photocatalysis Methods 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 8
- 230000001376 precipitating effect Effects 0.000 claims description 8
- 239000003643 water by type Substances 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims 2
- 238000001354 calcination Methods 0.000 claims 1
- 229910052799 carbon Inorganic materials 0.000 claims 1
- 239000000203 mixture Substances 0.000 claims 1
- 229910052757 nitrogen Inorganic materials 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 11
- 238000006243 chemical reaction Methods 0.000 abstract description 7
- 239000011701 zinc Substances 0.000 abstract description 5
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 abstract description 2
- 239000003795 chemical substances by application Substances 0.000 abstract description 2
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 238000007654 immersion Methods 0.000 abstract 2
- 238000000975 co-precipitation Methods 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 8
- 239000003054 catalyst Substances 0.000 description 6
- 238000006555 catalytic reaction Methods 0.000 description 6
- 238000005303 weighing Methods 0.000 description 6
- 235000013904 zinc acetate Nutrition 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 238000005215 recombination Methods 0.000 description 5
- 230000006798 recombination Effects 0.000 description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 239000008367 deionised water Substances 0.000 description 2
- 229910021641 deionized water Inorganic materials 0.000 description 2
- 239000000975 dye Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000005012 migration Effects 0.000 description 2
- 238000013508 migration Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 239000006104 solid solution Substances 0.000 description 2
- DJWUNCQRNNEAKC-UHFFFAOYSA-L zinc acetate Chemical class [Zn+2].CC([O-])=O.CC([O-])=O DJWUNCQRNNEAKC-UHFFFAOYSA-L 0.000 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 description 1
- 241001062009 Indigofera Species 0.000 description 1
- 230000032900 absorption of visible light Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001311 chemical methods and process Methods 0.000 description 1
- 239000003426 co-catalyst Substances 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000004042 decolorization Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 125000000325 methylidene group Chemical group [H]C([H])=* 0.000 description 1
- 229960000907 methylthioninium chloride Drugs 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 238000000103 photoluminescence spectrum Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 238000007086 side reaction Methods 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000002604 ultrasonography 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
- 229910052725 zinc Inorganic materials 0.000 description 1
Classifications
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- 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
- B01J27/24—Nitrogen compounds
-
- B01J35/39—
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/343—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of ultrasonic wave energy
-
- 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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Toxicology (AREA)
- Health & Medical Sciences (AREA)
- Materials Engineering (AREA)
- Physics & Mathematics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Plasma & Fusion (AREA)
- Optics & Photonics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Catalysts (AREA)
Abstract
Cadmium doped zinc sulphide/carbonitride method is prepared the invention discloses a kind of.For the present invention using zinc acetate, caddy and melamine as raw material, thiocarbamide is dressing agent, is prepared for different proportion Zn using coprecipitation and immersion method2+With Cd2+The g-C of sulfide nanocrystalline doping3N4, pH to 13 or so is adjusted using sodium hydroxide, in logical N2Under the conditions of using immersion method be made cadmium doped zinc sulphide/carbonitride (ZnxCd1‑xS/g‑C3N4).Cadmium doped zinc sulphide prepared by the present invention/carbon nitride material photocatalytic activity is high, and preparation method of the invention has the characteristics that reaction process is easily manipulated, preparation cost is low, high conversion rate, green and pollution-free.
Description
Technical field
The invention belongs to field of functional materials, are related to a kind of preparation method of cadmium doped zinc sulphide/carbonitride.
Background technique
In recent years, in the various technologies of response environment pollution, photocatalysis technology has become most promising skill
One of art.Photocatalysis technology is to carry out some important optical electro-chemistry reactions by directly absorbing the energy in sunlight, make too
Sun can directly decompose the pollutant in water or become efficient chemical energy source, can effectively alleviate and even solve environment danger
Machine, this point, the extensive concern by researcher and government department in worldwide.
Photo-generate electron-hole is migrated to the number that catalyst surface carries out redox reaction and is determined in light-catalyzed reaction
The photocatalysis efficiency of material.This is that is, catalysis material catalytic activity depends primarily on the following: (1) electronics-sky
The recombination rate in cave pair.The recombination rate of electron-hole pair determines the height of photocatalytic activity, so we will take measures, makes
Photo-generate electron-hole to separating as far as possible, so that so that electron-hole as much as possible is transitted to catalyst surface occurs oxidation also
Original reaction.(2) crystal configuration of catalyst.Under normal circumstances, big particle size can be such that electron-hole pair migration distance increases
Add, low crystallinity makes electron-hole pair migration slowly, is both unfavorable for improving the separative efficiency of electron-hole pair.(3)
The chemical reaction that catalyst surface occurs.It should avoid that side reaction occurs to greatest extent, electron-hole pair is made to transit to table
Face is merely able to occur specifically to react.(4) band gap width of catalysis material.The band gap width of catalysis material is narrower, more holds
Easily it is excited；Conversely, being less susceptible to be excited.(5) influence of specific surface area.Large specific surface area increases to a certain extent
Electron-hole pair recombination rate, reduces photocatalyst activity.(6) environmental factor.Including light intensity, light source, pH value, catalysis
Agent concentration, temperature etc..
Single g-C3N4Hole-electron recombination rate is high, so that photocatalytic activity is relatively low, in order to inhibit this compound, I
It is modified, but it is modified after be also faced with challenge below[13]: (1) graphite phase carbon nitride is to visible light
Using limited, it is concentrated mainly in royal purple optical range the absorption of visible light, so even if it is current there are many to its into
The modified method of row, photocatalysis performance is not still very high.(2) to g-C3N4Be difficult to control accurately when chemical doping, is easy
Introduce impurity.And the method for modifying that can be carried out has certain drawbacks, the substance compound with it mostly contain Ti, Zn, Sm,
The precious metals such as Ag, do so not only has certain pollution to water body, but also the price is very expensive.It (3) can be with although doing so
Refine product more, but the conversion ratio of recombination reaction is low, the time for reacting consuming is longer.(4) it closes in the lab
At g-C3N4Often contain a large amount of defect, crystallinity is low, and the bad dispersibility of catalysis material in water, can restrict material
The photocatalysis performance of material.
Metal sulfide and sulfide solid solution have suitable band gap, can respond sunlight, make good photochemical catalyst.
ZnxCd1-xSolid solution of the S as ZnS and CdS, has received widespread attention, in the condition for not making co-catalyst in noble metal
Under, there is good photocatalysis performance.The present invention is by g-C3N4With ZnxCd1-xS is compound to be provided and a kind of prepares efficient photocatalysis material
Preparation method for material.
Summary of the invention
The purpose of the present invention is it is described there are aiming at the problem that, a kind of preparation side of cadmium doped zinc sulphide/carbonitride is provided
Method.
The present invention adopts the following technical scheme:
Step 1, a certain amount of melamine is weighed in crucible, is covered on crucible and is made into semiclosed mode, with 10 DEG C
min-1Heating rate, 5 h are calcined at 520 DEG C, after being cooled to room temperature, with mortar grinder at powder；
Step 2, weigh a certain amount of thiocarbamide, a certain amount of carbonitride be put into three holes bottle in, by a certain amount of zinc acetate and caddy
It being added in 75 mL deionized waters, ultrasonic disperse processing is persistently carried out in this step, the power of ultrasonic disperse is 10 ~ 50W/h,
The time of ultrasonic disperse is 5 ~ 15min；
Step 3, continue to be passed through N to solution with the speed of 15 ~ 35mL/min2, and the left side pH to 13 is adjusted with the NaOH of 1 mol/L
30 min are stirred on the right side, continue 6 h of water-bath at 80 DEG C, precipitating centrifuge are centrifugated, drying, with mortar grinder at powder
End obtains cadmium doped zinc sulphide/carbonitride.
Compared with prior art, the present invention has beneficial below cadmium doped zinc sulphide/carbonitride preparation method
Effect:
The present invention is prepared for cadmium doped zinc sulphide/carbonitride using soft chemistry technique, by using simple ultrasonic disperse technology
The effective compound of cadmium doped zinc sulphide/nitridation carbon quantum dot and carbonitride is realized with reasonable control doping ratio.Present invention tool
There is preparation process simple, is easily manipulated, novel in design, the features such as production cost is low, and the reaction time is short, and photocatalysis efficiency is high.
Detailed description of the invention
Fig. 1 is the XRD diffracting spectrum that sample is prepared in 1-5 of the embodiment of the present invention.
Fig. 2 is the TEM figure of the sample prepared in comparative example 1 of the present invention.
Fig. 3 is the TEM figure of the sample prepared in the embodiment of the present invention 4.
Fig. 4 is the PL spectrum analysis that sample is prepared in 1-5 of the embodiment of the present invention.
Fig. 5 is the photocatalysis curve that sample is prepared in 1-5 of the embodiment of the present invention.
Fig. 6 is the photocatalysis curve that sample is prepared in comparative example 1 of the present invention.
Specific embodiment
The present invention is described further in the following with reference to the drawings and specific embodiments, raw material is that analysis is pure.
Embodiment 1:
Step 1, the melamine for weighing 15 grams covers on crucible in crucible and is made into semiclosed mode, with 10 DEG C of min-1
Heating rate, 5 h are calcined at 520 DEG C, after being cooled to room temperature, with mortar grinder at powder；
Step 2, weigh 0.7612 g thiocarbamide, 0.920 g carbonitride be put into three holes bottle in, 1.8348 grams of zinc acetates are added to 75
In mL deionized water, ultrasonic disperse processing is persistently carried out in this step, the power of ultrasonic disperse is 10 ~ 50W/h, ultrasonic disperse
Time is 5 ~ 15min；
Step 3, continue to be passed through N to solution with the speed of 15 ~ 35mL/min2, and the left side pH to 13 is adjusted with the NaOH of 1 mol/L
30 min are stirred on the right side, continue 6 h of water-bath at 80 DEG C, precipitating centrifuge are centrifugated, drying, with mortar grinder at powder
End obtains zinc sulphide/carbonitride.
Embodiment 2:
Step 1, the melamine for weighing 15 grams covers on crucible in crucible and is made into semiclosed mode, with 10 DEG C of min-1
Heating rate, 5 h are calcined at 520 DEG C, after being cooled to room temperature, with mortar grinder at powder；
Step 2, weigh 0.7612 g thiocarbamide, 0.920 g carbonitride be put into three holes bottle in, by 1.3761 grams of zinc acetates and 0.4583
Gram caddy is added in 75 mL deionized waters, and ultrasonic disperse processing is persistently carried out in this step, and the power of ultrasonic disperse is 10
~ 50W/h, the time of ultrasonic disperse are 5 ~ 15min；
Step 3, continue to be passed through N to solution with the speed of 15 ~ 35mL/min2, and the left side pH to 13 is adjusted with the NaOH of 1 mol/L
30 min are stirred on the right side, continue 6 h of water-bath at 80 DEG C, precipitating centrifuge are centrifugated, drying, with mortar grinder at powder
End obtains cadmium doped zinc sulphide/carbonitride.
Embodiment 3:
Step 1, the melamine for weighing 15 grams covers on crucible in crucible and is made into semiclosed mode, with 10 DEG C of min-1
Heating rate, 5 h are calcined at 520 DEG C, after being cooled to room temperature, with mortar grinder at powder；
Step 2, weigh 0.7612 g thiocarbamide, 0.920 g carbonitride be put into three holes bottle in, by 0.9174 gram of zinc acetate and 0.9166
Gram caddy is added in 75 mL deionized waters, and ultrasonic disperse processing is persistently carried out in this step, and the power of ultrasonic disperse is 10
~ 50W/h, the time of ultrasonic disperse are 5 ~ 15min；
Step 3, continue to be passed through N to solution with the speed of 15 ~ 35mL/min2, and the left side pH to 13 is adjusted with the NaOH of 1 mol/L
30 min are stirred on the right side, continue 6 h of water-bath at 80 DEG C, precipitating centrifuge are centrifugated, drying, with mortar grinder at powder
End obtains cadmium doped zinc sulphide/carbonitride.
Embodiment 4:
Step 1, the melamine for weighing 15 grams covers on crucible in crucible and is made into semiclosed mode, with 10 DEG C of min-1
Heating rate, 5 h are calcined at 520 DEG C, after being cooled to room temperature, with mortar grinder at powder；
Step 2, weigh 0.7612 g thiocarbamide, 0.920 g carbonitride be put into three holes bottle in, by 0.4587 gram of zinc acetate and 1.3749
Gram caddy is added in 75 mL deionized waters, and ultrasonic disperse processing is persistently carried out in this step, and the power of ultrasonic disperse is 10
~ 50W/h, the time of ultrasonic disperse are 5 ~ 15min；
Step 3, continue to be passed through N to solution with the speed of 15 ~ 35mL/min2, and the left side pH to 13 is adjusted with the NaOH of 1 mol/L
30 min are stirred on the right side, continue 6 h of water-bath at 80 DEG C, precipitating centrifuge are centrifugated, drying, with mortar grinder at powder
End obtains cadmium doped zinc sulphide/carbonitride.
Embodiment 5:
Step 1, the melamine for weighing 15 grams covers on crucible in crucible and is made into semiclosed mode, with 10 DEG C of min-1
Heating rate, 5 h are calcined at 520 DEG C, after being cooled to room temperature, with mortar grinder at powder；
Step 2, weigh 0.7612 g thiocarbamide, 0.920 g carbonitride be put into three holes bottle in, 1.8332 grams of caddies are added to 75
In mL deionized water, ultrasonic disperse processing is persistently carried out in this step, the power of ultrasonic disperse is 10 ~ 50W/h, ultrasonic disperse
Time is 5 ~ 15min；
Step 3, continue to be passed through N to solution with the speed of 15 ~ 35mL/min2, and the left side pH to 13 is adjusted with the NaOH of 1 mol/L
30 min are stirred on the right side, continue 6 h of water-bath at 80 DEG C, precipitating centrifuge are centrifugated, drying, with mortar grinder at powder
End obtains cadmium doped zinc sulphide/carbonitride.
Comparative example 1
Step 1, the melamine for weighing 15 grams covers on crucible in crucible and is made into semiclosed mode, with 10 DEG C of min-1
Heating rate, 5 h are calcined at 520 DEG C, after being cooled to room temperature, with mortar grinder at powder；
Step 2, weigh 0.7612 g thiocarbamide, 0.920 g carbonitride be put into three holes bottle in, by 0.4587 gram of zinc acetate and 1.3749
Gram caddy is added in 75 mL deionized waters, is stirred substitution ultrasonic disperse with the speed of 20 ~ 120r/min；
Step 3, continue to be passed through N to solution with the speed of 15 ~ 35mL/min2, and the left side pH to 13 is adjusted with the NaOH of 1 mol/L
30 min are stirred on the right side, continue 6 h of water-bath at 80 DEG C, precipitating centrifuge are centrifugated, drying, with mortar grinder at powder
End obtains cadmium doped zinc sulphide/carbonitride.
Application examples:
It weighs in Examples 1 to 5 and sample obtained by comparative example 1 takes 100 mg of photochemical catalyst respectively, add it to methylene
(100mL, 10mgL in base indigo plant dye solution-1), it is protected from light stirring 1h, opens 500W xenon source after De contamination reaches balance,
The concentration of a dyestuff is detected every 30min, material prepared is symbolized within given time to the catalytic decolorization of methylene blue
Situation.
By above embodiments and comparative example comparison discovery, by rationally adjusting during the preparation process and using ultrasound point
It dissipates, can significantly improve the photocatalysis characteristic and microstructure characteristic of composite material by rationally controlling doping concentration.
Above said content is only the basic explanation under present inventive concept, by reading description of the invention to the present invention
Any equivalent transformation that technical solution is taken should all belong to this hair as long as it does not depart from the spirit and scope of the technical scheme of the present invention
Bright protection scope.
Claims (5)
1. a kind of preparation method of cadmium doped zinc sulphide/carbonitride, it is characterised in that cadmium doped zinc sulphide granularity is 2 in compound
~3nm specifically includes following preparation step:
Step 1, a certain amount of melamine is weighed in crucible, is covered on crucible and is made into semiclosed mode, with 10 DEG C of min-1Heating rate, 5 h are calcined at 520 DEG C, after being cooled to room temperature, with mortar grinder at powder；
Step 2, weigh a certain amount of thiocarbamide, a certain amount of carbonitride be put into three holes bottle in, by a certain amount of zinc acetate and caddy
It being added in 75 mL deionized waters, ultrasonic disperse processing is persistently carried out in this step, the power of ultrasonic disperse is 10 ~ 50W/h,
The time of ultrasonic disperse is 5 ~ 15min；
Step 3, continue to be passed through N to solution with the speed of 15 ~ 35mL/min2, and pH to 13 or so is adjusted with the NaOH of 1 mol/L,
It stirs 30 min, continues 6 h of water-bath at 80 DEG C, precipitating centrifuge is centrifugated, drying, with mortar grinder at powder,
Obtain cadmium doped zinc sulphide/carbonitride.
2. heating rate is the method according to claim 1, wherein calcination time is 5 h in the step 1
10 ℃∙min-1。
3. the method according to claim 1, wherein the dosage of thiocarbamide is 0.7612 g, nitrogen in the step 2
The dosage for changing carbon is 0.920 g, and wherein the sum of mole of zinc acetate and caddy is equal to the mole of thiocarbamide.
4. the method according to claim 1, wherein in the step 3, N2Being passed through speed is 15 ~ 35mL/min,
The pH value of mixture is 13.
5. the method according to claim 1, wherein cadmium doped zinc sulphide/carbonitride is in photocatalysis field
In application.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112371155A (en) * | 2020-11-11 | 2021-02-19 | 陕西科技大学 | g-C3N4/Zn0.2Cd0.8Preparation method of S composite material |
| CN115400776A (en) * | 2022-08-01 | 2022-11-29 | 电子科技大学长三角研究院(湖州) | Zinc-cadmium-sulfur solid solution/graphite-phase carbon nitride sheet composite S-shaped heterojunction photocatalyst, and preparation and application thereof |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115400776A (en) * | 2022-08-01 | 2022-11-29 | 电子科技大学长三角研究院(湖州) | Zinc-cadmium-sulfur solid solution/graphite-phase carbon nitride sheet composite S-shaped heterojunction photocatalyst, and preparation and application thereof |
| CN115400776B (en) * | 2022-08-01 | 2023-05-16 | 电子科技大学长三角研究院(湖州) | Zinc-cadmium-sulfur solid solution/graphite phase carbon nitride sheet composite S-type heterojunction photocatalyst, preparation and application thereof |
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