CN110142050A - The preparation method of zinc sulphide doped titanium dioxide photocatalyst - Google Patents
The preparation method of zinc sulphide doped titanium dioxide photocatalyst Download PDFInfo
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- CN110142050A CN110142050A CN201910443973.5A CN201910443973A CN110142050A CN 110142050 A CN110142050 A CN 110142050A CN 201910443973 A CN201910443973 A CN 201910443973A CN 110142050 A CN110142050 A CN 110142050A
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- titanium dioxide
- zinc
- preparation
- doped titanium
- zinc sulphide
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 78
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 35
- 239000005083 Zinc sulfide Substances 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- DRDVZXDWVBGGMH-UHFFFAOYSA-N zinc;sulfide Chemical compound [S-2].[Zn+2] DRDVZXDWVBGGMH-UHFFFAOYSA-N 0.000 title claims abstract description 15
- 239000011941 photocatalyst Substances 0.000 title claims abstract description 14
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000007787 solid Substances 0.000 claims abstract description 20
- NWONKYPBYAMBJT-UHFFFAOYSA-L zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 claims abstract description 18
- 229960001763 zinc sulfate Drugs 0.000 claims abstract description 18
- 229910000368 zinc sulfate Inorganic materials 0.000 claims abstract description 18
- 239000003054 catalyst Substances 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910001868 water Inorganic materials 0.000 claims abstract description 14
- 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 claims abstract description 13
- 239000011734 sodium Substances 0.000 claims abstract description 13
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 10
- 238000002425 crystallisation Methods 0.000 claims abstract description 8
- 230000008025 crystallization Effects 0.000 claims abstract description 8
- 239000000203 mixture Substances 0.000 claims abstract description 6
- 150000001875 compounds Chemical class 0.000 claims abstract description 5
- 238000005245 sintering Methods 0.000 claims abstract description 5
- 229910052979 sodium sulfide Inorganic materials 0.000 claims abstract description 5
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000005485 electric heating Methods 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- 229910001948 sodium oxide Inorganic materials 0.000 claims description 3
- 239000000975 dye Substances 0.000 abstract description 15
- 238000000034 method Methods 0.000 abstract description 7
- 238000005303 weighing Methods 0.000 abstract description 5
- 239000002994 raw material Substances 0.000 abstract description 4
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 abstract description 3
- 238000001816 cooling Methods 0.000 abstract description 3
- 238000012986 modification Methods 0.000 abstract description 3
- 230000004048 modification Effects 0.000 abstract description 3
- 238000007146 photocatalysis Methods 0.000 abstract description 3
- 230000001699 photocatalysis Effects 0.000 abstract description 3
- 230000003197 catalytic effect Effects 0.000 description 12
- 230000015556 catabolic process Effects 0.000 description 10
- 238000006731 degradation reaction Methods 0.000 description 10
- 230000000694 effects Effects 0.000 description 8
- 238000005562 fading Methods 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 6
- 238000006555 catalytic reaction Methods 0.000 description 5
- 238000002474 experimental method Methods 0.000 description 5
- 238000002835 absorbance Methods 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- 229910052804 chromium Inorganic materials 0.000 description 3
- 239000011651 chromium Substances 0.000 description 3
- 238000005286 illumination Methods 0.000 description 3
- 239000000376 reactant Substances 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000001514 detection method Methods 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- 150000003751 zinc Chemical class 0.000 description 2
- 150000001299 aldehydes Chemical class 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 125000000753 cycloalkyl group Chemical group 0.000 description 1
- 230000000593 degrading effect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- -1 sensor Substances 0.000 description 1
- 238000005406 washing Methods 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
-
- 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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
Abstract
The present invention relates to technical field of visible-light-driven catalyst, and in particular to a kind of preparation method of zinc sulphide doped titanium dioxide photocatalyst；The following steps are included: a, weighing zinc sulfate or zinc nitrate is dissolved in water, titanium dioxide is then added, is stirred evenly；B, it weighs vulcanized sodium to be dissolved in water, blend compounds head dropper, which instills sodium sulfide solution, obtains mixed liquor A in the solution of step a；C, by the mixed liquor A of step b, evaporative crystallization obtains solid in electric heating cover；D, step c obtained solid is placed in cupel to be put into box-type high-temperature furnace and carries out high temperature sintering, after take out solid and cooling, wash, be dried to obtain new photochemical catalyst；Raw material and titanium dioxide are doped by the method for the present invention using the method for evaporative crystallization, it is more suitable for the doping and modification of zinc ion and titanium dioxide under alkaline condition, new photocatalysis prepared by the method for the present invention meets required for us under conditions of the irradiation of normal sunlight to the fade treatment of organic dyestuff.
Description
Technical field
The present invention relates to technical field of visible-light-driven catalyst, and in particular to a kind of zinc sulphide doped titanium dioxide photocatalyst
Preparation method.
Background technique
The semiconductor light-catalyst studied at present mainly has Ti02、ZnO、CdS。TiO2Physics, chemical property are more steady
Fixed, catalytic effect is good, nontoxic, is ideal environmentally friendly material, has a good application prospect.TiO2Catalysis is lived
Property is stronger, and TiO2Compared with other semiconductor materials, have the advantage that resistance to corrosion is strong, chemical property is stablized；Light
High catalytic efficiency, the hole in valence band have the very strong ability for obtaining electronics, can be by the OH in water-And H20 is converted into oxygen
Very capable, this performance can be used to some organic pollutants of degrading.TiO2It is inexpensive nontoxic, it is at low cost, so TiO2It answers extensively
For production fields such as catalyst, sensor, material, coating and cosmetics.But there is also insufficient.As forbidden band is wider, right
The utilization efficiency of sunlight is low etc..
Summary of the invention
The present invention is to solve TiO2As photochemical catalyst exist it is low to dyestuff organic removal rate, photocatalysis efficiency it is low etc.
Technical problem provides a kind of preparation method of zinc sulphide doped titanium dioxide photocatalyst.
In order to solve the above technical problems, the technical scheme adopted by the invention is as follows: a kind of titania-doped light of zinc sulphide
The preparation method of catalyst, which comprises the following steps:
A kind of preparation method of zinc sulphide doped titanium dioxide photocatalyst, which comprises the following steps:
A, it weighs zinc sulfate or zinc nitrate is dissolved in water, then add titanium dioxide, stir evenly；
B, it weighs vulcanized sodium to be dissolved in water, blend compounds head dropper will must mix in the solution of sodium sulfide solution instillation step a
Liquid A；
C, by the mixed liquor A of step b, evaporative crystallization obtains solid in electric heating cover；
D, step c obtained solid is placed in cupel to be put into box-type high-temperature furnace and carries out high temperature sintering, after take out it is solid
Body and cooling wash, are dried to obtain new photochemical catalyst, i.e. zinc sulphide doped titanium dioxide photocatalyst.
Preferably, the mixed liquor A in step b will carry out again step c's with concentrated ammonia liquor after the pH value adjustment of mixed liquor A to 8
Evaporative crystallization.
Preferably, the molar ratio of zinc sulfate or zinc nitrate used, vulcanized sodium and titanium dioxide is 2:5:1.
Preferably, the mass volume ratio of zinc sulfate added in step a, titanium dioxide and water is 2.51g:5g:20mL.
Preferably, the mass volume ratio of added vulcanized sodium and water is 1g:4ml in step b.
Preferably, the temperature of step d high temperature sintering is 500 DEG C, and the time is 3 hours.
Compared with prior art the invention has the following advantages:
It is 3.0eV or so in titanium dioxide band gap, and ZnS is also a kind of semiconductor material, its addition can prevent to be excited
Hair transits to the electronics (e of conduction band-) fall back to hole (h+).The hole in electronics and valence band in this way in conduction band just has sufficient
Some pollutants (organic compound, dyestuff, cyclic hydrocarbon, aromatic hydrocarbons, poisonous gas, aldehydes etc.) on time and surface react.
Raw material and titanium dioxide are doped by the method for the present invention using the method for evaporative crystallization, be more suitable under alkaline condition zinc ion and
The doping and modification of titanium dioxide, colour fading or degree of degradation to dyestuff can also reach nearly 100%, when pH value is 8, can have most
The amount of big reactant generates.It is required in normal sunlight that new photocatalysis prepared by the method for the present invention meets us
To the fade treatment of organic dyestuff under conditions of irradiation, convenient for from now on we be applied in production practices, common
It by wastewater degradation is our utilizable transparent liquid under illumination condition.When zinc sulfate or zinc nitrate, vulcanized sodium and
When the molar ratio of titanium dioxide is 2:5:1, the solid matter that reactant generates is most.The fading effect of dyestuff is also preferable.Too
Fading effect under sunlight is significantly better than fading effect under the conditions of ultraviolet.And photochemical catalyst of the invention can also repeat to make
With.
Specific embodiment
Below in conjunction with specific embodiment, the invention will be further described.
Embodiment 1
The preparation of new photochemical catalyst and result detection
Weighing zinc sulfate 2.51g adds 20mL water to dissolve, and titanium dioxide 5.00g is then added in solution again, stirs evenly.It will
2.50g vulcanized sodium 10mL water dissolves, and blend compounds head dropper instills sodium sulfide solution in above-mentioned solution.It is steamed in electric heating cover
Hair crystallization, weighing solid masses is 7.75g, and places it in cupel and be put into box-type high-temperature furnace at 500 DEG C, is placed 3 hours,
Cooling after taking-up, washing, drying, weighing solid masses are 6.14g.
It weighs above-mentioned 1g solid addition 20mL acid chromium blue k to stir in the sun 1.5 hours, solid matter is allowed to fill with dyestuff
Point reaction, folds filter paper filtering with hand, after measured with ultraviolet specrophotometer after clear liquid transmissivity and absorbance, and calculate
The degradation rate of the solution.Aforesaid operations are repeated, irradiation condition is changed to irradiate 1.5 hours under portable uv analyzer, weight
Experimental implementation under multiple sunlight.The transmitance for measuring brand-new acid chromium blue k solution is 29.1%, absorbance 0.537, will be real
It tests data and calculates the degradation rate of acid chromium blue k indicator with by formula (2-1), and be organized into such as the following table 1,.
In formula, A0For initial absorbance；A is the absorbance after catalysis.
Table 1
Zinc sulfate is changed into the result such as the following table 2 measured after zinc nitrate in the case where experiment condition is constant.
Table 2
From the point of view of the wavelength angle of illumination, catalytic effect in the sun is better than catalytic effect under the conditions of ultraviolet,
It is suitble to be conducive to react by the atom and the wave band separated with electronics of photochemical catalyst the reason is that having under sunlight；From the angle of zinc salt
From the point of view of degree, the catalytic effect of zinc nitrate is better than the catalytic effect of zinc sulfate, and zinc nitrate has more effectively with reacting for vulcanized sodium
Product generates, and is conducive to the progress of reaction.
Embodiment 2
Result detection after quadric catalysis
Solid after being once catalyzed in embodiment 1 is cleaned in sand mold funnel with deionized water, and solution is filtered, is obtained
To the first freeze-day with constant temperature in digital display air dry oven of solid, solid is put in box-type high-temperature furnace again after dry.Weight after taking-up
Experimental implementation more than multiple, if the quality of solid is divided into two parts less than 2g, by remaining all solids, according to raw material and
The ratio of the 1:20 of dyestuff compares test, is organized into such as the following table 3.
Table 3
Zinc sulfate is changed into the result such as the following table 4 measured after zinc nitrate in the case where experiment condition is constant.
Table 4
Result trend after quadric catalysis is essentially identical with embodiment 1, but there is no be catalyzed for the first time for catalytic effect
Effect it is good, analyzed from the principle of reaction, after quadric catalysis, photochemical catalyst there is no generate more for reaction
Atomic nucleus and electronics, so the result reacted with colored dyes will be lower than the result being catalyzed for the first time.
Embodiment 3
Comparative test
The zinc sulfate of 2.50g and the vulcanized sodium of 2.51g is only added in raw material, is added without titanium dioxide, reaction condition and operation
It is fully equivalent to Examples 1 and 2.Equally experimental data is arranged, calculates degree of degradation, data preparation is at entering the following table 5,6.
Table 5
Table 6
Under conditions of no addition titanium dioxide, product can be with degradation of dye, but catalytic effect is obviously not so good as joined
The later catalytic effect of titanium dioxide can make full use of in sunlight under the conditions of illustrating that product and titanium dioxide are well-bound
Effective wave band, and then achieve the purpose that degrade colored dyes.
Zinc sulfate is changed into the result measured after zinc nitrate such as the following table 7,8 in the case where experiment condition is constant.
Table 7
Table 8
Under comparable conditions, the catalytic effect of zinc nitrate is still better than the catalytic effect of zinc sulfate.
Embodiment 4
It will be detected after pH value adjustment to 8
Weighing zinc sulfate 2.51g adds 20mlL to dissolve, and titanium dioxide 5.00g is then added in solution again, stirs evenly.It will
2.50g vulcanized sodium 10mL water dissolves, and blend compounds head dropper instills sodium sulfide solution in above-mentioned solution.With concentrated ammonia liquor by solution
PH value adjustment to 8, then the repeatedly experimental procedure in embodiment 1 and embodiment 2, measures the product after first time is catalyzed
Quality is 8.16g, by interpretation at such as the following table 9,10.
Table 9
Table 10
After adjusting pH value, not only the amount of product increases, but also reaction effect is enhanced, under solar irradiation
Can by organic dyestuff almost 100% degradation, illustrate that PH=8 is most suitable degradation environment.
Zinc sulfate is changed into the result measured after zinc nitrate such as the following table 11,12 in the case where experiment condition is constant.
Table 11
Table 12
Which kind of zinc salt is explanation either use it can be seen from table 11 and table 12, and OH's-is a large amount of under conditions of PH=8
In the presence of TiO2Particle surface is negatively charged, is conducive to hole and is transferred to particle surface, reaches better catalytic effect, Er Qie
It is also photochemical catalyst production quantity maximum acid-base property condition when PH=8.
It is more suitable for the doping and modification of zinc ion and titanium dioxide under alkaline condition, the colour fading or degree of degradation to dyestuff
Nearly 100% can be reached, substantially meet and organic dyestuff is taken off under conditions of the irradiation of normal sunlight required for us
Color processing, convenient for from now on we be applied in production practices, by wastewater degradation be us under common illumination condition
Utilizable transparent liquid.When the molar ratio of zinc sulfate or zinc nitrate, vulcanized sodium and titanium dioxide is 2.5:1,
The solid matter that reactant generates is most.The fading effect of dyestuff is also preferable.Fading effect in experimentation, under sunlight
Significantly better than fading effect under the conditions of ultraviolet.
Claims (6)
1. a kind of preparation method of zinc sulphide doped titanium dioxide photocatalyst, which comprises the following steps:
A, it weighs zinc sulfate or zinc nitrate is dissolved in water, then add titanium dioxide, stir evenly；
B, it weighs vulcanized sodium to be dissolved in water, blend compounds head dropper, which instills sodium sulfide solution, obtains mixed liquor A in the solution of step a；
C, by the mixed liquor A of step b, evaporative crystallization obtains solid in electric heating cover；
D, step c obtained solid is placed in cupel to be put into box-type high-temperature furnace and carries out high temperature sintering, after take out solid simultaneously
It cools down, wash, being dried to obtain new photochemical catalyst, i.e. zinc sulphide doped titanium dioxide photocatalyst.
2. the preparation method of zinc sulphide doped titanium dioxide photocatalyst according to claim 1, which is characterized in that step
Mixed liquor A in b will carry out again the evaporative crystallization of step c with concentrated ammonia liquor after the pH value adjustment of mixed liquor A to 8.
3. the preparation method of zinc sulphide doped titanium dioxide photocatalyst according to claim 1, which is characterized in that used
The molar ratio of zinc sulfate or zinc nitrate, vulcanized sodium and titanium dioxide is 2:5:1.
4. the preparation method of zinc sulphide doped titanium dioxide photocatalyst according to claim 1, which is characterized in that step
The mass volume ratio of added zinc sulfate, titanium dioxide and water is 2.51g:5g:20mL in a.
5. the preparation method of zinc sulphide doped titanium dioxide photocatalyst according to claim 3 or 4, which is characterized in that
The mass volume ratio of added vulcanized sodium and water is 1g:4ml in step b.
6. the preparation method of zinc sulphide doped titanium dioxide photocatalyst according to claim 5, which is characterized in that step
The temperature of d high temperature sintering is 500 DEG C, and the time is 3 hours.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113213579A (en) * | 2021-05-25 | 2021-08-06 | 贵州省材料产业技术研究院 | Application of photocatalytic biochar composite material in catalytic degradation of printing and dyeing wastewater |
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| CN101003020A (en) * | 2007-01-11 | 2007-07-25 | 南京大学 | Sensitized titanium oxide and zinc sulfide visible light responsing photocalalyst, and its preparing method |
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| CN101003020A (en) * | 2007-01-11 | 2007-07-25 | 南京大学 | Sensitized titanium oxide and zinc sulfide visible light responsing photocalalyst, and its preparing method |
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| CN113213579A (en) * | 2021-05-25 | 2021-08-06 | 贵州省材料产业技术研究院 | Application of photocatalytic biochar composite material in catalytic degradation of printing and dyeing wastewater |
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