CN106925302B - Molybdenum disulfide-antimony trisulfide composite material and preparation method and application - Google Patents
Molybdenum disulfide-antimony trisulfide composite material and preparation method and application Download PDFInfo
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- 229940007424 antimony trisulfide Drugs 0.000 title claims abstract description 97
- 239000002131 composite material Substances 0.000 title claims abstract description 87
- UICKUOVXTQKMMX-UHFFFAOYSA-N [Mo]=S.[Sb]=S Chemical compound [Mo]=S.[Sb]=S UICKUOVXTQKMMX-UHFFFAOYSA-N 0.000 title claims abstract description 52
- 238000002360 preparation method Methods 0.000 title claims abstract description 31
- 229910052982 molybdenum disulfide Inorganic materials 0.000 claims abstract description 85
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 claims abstract description 76
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 48
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 28
- NVWBARWTDVQPJD-UHFFFAOYSA-N antimony(3+);trisulfide Chemical compound [S-2].[S-2].[S-2].[Sb+3].[Sb+3] NVWBARWTDVQPJD-UHFFFAOYSA-N 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910052787 antimony Inorganic materials 0.000 claims abstract description 16
- WATWJIUSRGPENY-UHFFFAOYSA-N antimony atom Chemical compound [Sb] WATWJIUSRGPENY-UHFFFAOYSA-N 0.000 claims abstract description 15
- 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 12
- 239000011734 sodium Substances 0.000 claims abstract description 12
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims abstract description 7
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 7
- 239000011684 sodium molybdate Substances 0.000 claims abstract description 6
- 235000015393 sodium molybdate Nutrition 0.000 claims abstract description 6
- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims abstract description 6
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 claims abstract description 5
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000002351 wastewater Substances 0.000 claims description 33
- 238000006243 chemical reaction Methods 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 15
- 239000000463 material Substances 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 10
- 229910052724 xenon Inorganic materials 0.000 claims description 10
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims description 10
- ZOKXTWBITQBERF-UHFFFAOYSA-N Molybdenum Chemical compound [Mo] ZOKXTWBITQBERF-UHFFFAOYSA-N 0.000 claims description 8
- 238000006555 catalytic reaction Methods 0.000 claims description 8
- 229910052750 molybdenum Inorganic materials 0.000 claims description 8
- 239000011733 molybdenum Substances 0.000 claims description 8
- 238000004073 vulcanization Methods 0.000 claims description 8
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 6
- 239000005864 Sulphur Substances 0.000 claims description 6
- 239000007795 chemical reaction product Substances 0.000 claims description 6
- 239000002243 precursor Substances 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- WYWFMUBFNXLFJK-UHFFFAOYSA-N [Mo].[Sb] Chemical compound [Mo].[Sb] WYWFMUBFNXLFJK-UHFFFAOYSA-N 0.000 claims description 5
- FAPDDOBMIUGHIN-UHFFFAOYSA-K antimony trichloride Chemical compound Cl[Sb](Cl)Cl FAPDDOBMIUGHIN-UHFFFAOYSA-K 0.000 claims description 5
- 230000008859 change Effects 0.000 claims description 5
- 230000009467 reduction Effects 0.000 claims description 5
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 238000005119 centrifugation Methods 0.000 claims description 3
- 239000000047 product Substances 0.000 claims description 3
- 239000002023 wood Substances 0.000 claims description 3
- 239000000654 additive Substances 0.000 claims description 2
- 229910001948 sodium oxide Inorganic materials 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 238000003786 synthesis reaction Methods 0.000 claims 2
- 150000001408 amides Chemical class 0.000 claims 1
- 238000001035 drying Methods 0.000 claims 1
- 125000000446 sulfanediyl group Chemical group *S* 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 abstract description 21
- 238000000034 method Methods 0.000 abstract description 12
- 238000007146 photocatalysis Methods 0.000 abstract description 10
- 238000013033 photocatalytic degradation reaction Methods 0.000 abstract description 3
- 230000008569 process Effects 0.000 abstract description 3
- 238000004064 recycling Methods 0.000 abstract description 3
- 239000010842 industrial wastewater Substances 0.000 abstract description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract 1
- 229910052799 carbon Inorganic materials 0.000 abstract 1
- 239000011651 chromium Substances 0.000 description 30
- 229910052961 molybdenite Inorganic materials 0.000 description 23
- 229910052959 stibnite Inorganic materials 0.000 description 22
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 7
- 229910052804 chromium Inorganic materials 0.000 description 7
- JOPOVCBBYLSVDA-UHFFFAOYSA-N chromium(6+) Chemical compound [Cr+6] JOPOVCBBYLSVDA-UHFFFAOYSA-N 0.000 description 7
- 239000000975 dye Substances 0.000 description 6
- 238000005286 illumination Methods 0.000 description 6
- 238000010531 catalytic reduction reaction Methods 0.000 description 4
- 230000000593 degrading effect Effects 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 239000003344 environmental pollutant Substances 0.000 description 4
- 231100000719 pollutant Toxicity 0.000 description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 description 4
- 238000006722 reduction reaction Methods 0.000 description 4
- 238000001179 sorption measurement Methods 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 3
- 238000001914 filtration Methods 0.000 description 3
- 230000005484 gravity Effects 0.000 description 3
- 230000001788 irregular Effects 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004044 response Effects 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 2
- 230000004087 circulation Effects 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000004570 mortar (masonry) Substances 0.000 description 2
- -1 polytetrafluoroethylene Polymers 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 230000006641 stabilisation Effects 0.000 description 2
- 238000011105 stabilization Methods 0.000 description 2
- 239000006228 supernatant Substances 0.000 description 2
- QXNVGIXVLWOKEQ-UHFFFAOYSA-N Disodium Chemical compound [Na][Na] QXNVGIXVLWOKEQ-UHFFFAOYSA-N 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- PJRNYFTWHCILGX-UHFFFAOYSA-N [Sb].[Mo]=S Chemical compound [Sb].[Mo]=S PJRNYFTWHCILGX-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003426 co-catalyst Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 229960000935 dehydrated alcohol Drugs 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229960004756 ethanol Drugs 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 239000011941 photocatalyst Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000005303 weighing 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
- B01J27/047—Sulfides with chromium, molybdenum, tungsten or polonium
- B01J27/051—Molybdenum
-
- 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
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
- C02F2101/22—Chromium or chromium compounds, e.g. chromates
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/30—Nature of the water, waste water, sewage or sludge to be treated from the textile industry
Abstract
The invention discloses a kind of molybdenum disulfide-antimony trisulfide composite material and preparation method and applications, and the molybdenum disulfide-antimony trisulfide composite material includes molybdenum disulfide and antimony trisulfide, and molybdenum disulfide is entrained in antimony trisulfide.Preparation method includes first with sodium molybdate and thioacetamide through hydrothermal synthesis of carbon/molybdenum disulfide, and then molybdenum disulfide ultrasonic disperse is added to nine water vulcanized sodium after sodium hydroxide solution, the hydrochloric acid solution of chloride containing antimony is added dropwise in the sodium hydroxide solution containing molybdenum disulfide and vulcanized sodium again and forms presoma, it is finally heated to obtain molybdenum disulfide-antimony trisulfide composite material.Composite material of the invention strong, the recycling property height with stability, has many advantages, such as high photocatalytic activity site, preparation method simple process, operability are high, at low cost, and composite material has superior photocatalysis performance, can be widely applied to photocatalytic degradation industrial wastewater field.
Description
Technical field
The invention belongs to the preparation technical field of composite material, it is related to a kind of Photocatalytic nano composite material and its preparation side
Method and application, and in particular to a kind of molybdenum disulfide-antimony trisulfide composite material and preparation method and application.
Background technique
In recent years, photocatalysis technology is widely used to the pollutant in processing waste water.Many catalysis material such as metals
Oxide, sulfide and nitride have obtained extensive concern and research.In these photochemical catalysts, antimony trisulfide (Sb2S3) be
The semiconductor material of V-VI race direct band gap is urged with its suitable band gap (1.5~2.2eV) and good light sensitive characteristic in light
There is potential application prospect in change field.However individually using antimony trisulfide as when photochemical catalyst, due to its relatively narrow band-gap energy and
Lower quantum efficiency and cause its photocatalytic activity not high.Therefore, by with other materials it is compound go improve Sb2S3Light urge
Changing performance becomes very necessary.
Summary of the invention
The technical problem to be solved by the present invention is to overcome the deficiencies in the prior art, and it is excellent, steady to provide a kind of photocatalysis performance
Qualitative strong, recycling property height, molybdenum disulfide-antimony trisulfide composite material with high photocatalytic activity site also provide one
Plant simple preparation process, operability height, molybdenum disulfide at low cost-antimony trisulfide composite material preparation method and the curing
The application of molybdenum-antimony trisulfide composite material Cr VI in removal industrial wastewater.
In order to solve the above technical problems, the invention adopts the following technical scheme:
A kind of molybdenum disulfide-antimony trisulfide composite material, the molybdenum disulfide-antimony trisulfide composite material include molybdenum disulfide and
Antimony trisulfide, the molybdenum disulfide are doped in composition molybdenum disulfide-antimony trisulfide composite material in the antimony trisulfide.
Above-mentioned molybdenum disulfide-antimony trisulfide composite material, it is preferred that the mass fraction of the molybdenum disulfide is 5%~11%.
As a general technical idea, the present invention also provides a kind of preparations of molybdenum disulfide-antimony trisulfide composite material
Method, comprising the following steps:
(1) sodium molybdate and thioacetamide is soluble in water, hydrothermal synthesis reaction is carried out, molybdenum disulfide is obtained；
(2) then nine water vulcanized sodium are added in sodium hydroxide solution in the resulting molybdenum disulfide ultrasonic disperse of step (1)
As sulphur source, the sodium hydroxide solution containing molybdenum disulfide and vulcanized sodium is obtained；
(3) antimony chloride is dissolved in hydrochloric acid solution, obtains the hydrochloric acid solution of chloride containing antimony；
(4) by the hydrochloric acid solution of the resulting chloride containing antimony of step (3) be added dropwise step (2) it is resulting containing molybdenum disulfide and
It is reacted in the sodium hydroxide solution of vulcanized sodium, obtains molybdenum disulfide-vulcanization antimony precursors；
(5) the resulting molybdenum disulfide of step (4)-vulcanization antimony precursors are heated, it is multiple obtains molybdenum disulfide-antimony trisulfide
Condensation material.
Above-mentioned preparation method, it is preferred that in the step (1), the molar ratio of the sodium molybdate and thioacetamide is 1
: 2~8.
Above-mentioned preparation method, it is preferred that in the step (2), the quality of the molybdenum disulfide and sodium hydroxide solution
Volume ratio is 200mg~400mg: 1L(, that is, 200mg/L~400mg/L), the matter of the nine water vulcanized sodium and sodium hydroxide solution
Amount volume ratio is 7.2g~20g: 1L(, that is, 7.2g/L~20g/L), the concentration of the sodium hydroxide solution is 1mol/L~2mol/
L；
And/or in the step (3), the mass volume ratio of the antimony chloride and hydrochloric acid solution is for 9g~12g: 1L(
9g/L~12g/L), the concentration of the hydrochloric acid solution is 6mol/L~8mol/L.
Above-mentioned preparation method, it is preferred that in the step (1), the condition of the hydrothermal synthesis reaction are as follows: heating temperature
It is 180 DEG C~200 DEG C, heating time is for 24 hours~26h；
And/or in the step (5), the temperature of the heating is 100 DEG C~150 DEG C, and the time of the heating is 12h
~15h.
Above-mentioned preparation method, it is preferred that in the step (1), after the hydrothermal synthesis reaction, by gained reaction product
Deionized water, ethanol washing are successively used, is then centrifuged for separating, centrifugal rotational speed is 5000 revs/min~7000 revs/min, centrifugation time
It is 3 minutes~5 minutes, then dry 4h~6h in the environment of temperature is 50 DEG C~70 DEG C, obtains molybdenum disulfide；
And/or in the step (5), after the heating, gained reaction product is washed with deionized, then in temperature
Dry 6h~12h in the environment of being 40 DEG C~60 DEG C.
As a general technical idea, the present invention also provides a kind of above-mentioned molybdenum disulfide-antimony trisulfide composite materials
Or molybdenum disulfide-antimony trisulfide composite material that above-mentioned preparation method is prepared is in the application for removing the Cr VI in waste water.
Above-mentioned application, it is preferred that the application is the following steps are included: by the molybdenum disulfide-antimony trisulfide composite material
It is added in waste water, light-catalyzed reaction is carried out under visible light or near infrared light, completes the reduction to Cr VI, the curing
Molybdenum-additive amount of the antimony trisulfide composite material in waste water is 0.8g/L~1.2g/L.
Above-mentioned application, it is preferred that in the application, by the molybdenum disulfide-antimony trisulfide composite wood under the conditions of being protected from light
Material is added in waste water and stirs；And/or the light source of the visible light or near infrared light is the xenon lamp of 300W~500W, it is described
The liquid level of xenon lamp and waste water distance is 14cm~16cm, and the time of the light-catalyzed reaction is 120min~150min；With/
Or, the concentration of Cr VI is 50mg/L~60mg/L in the waste water.
Compared with the prior art, the advantages of the present invention are as follows:
1, the present invention provides a kind of molybdenum disulfide-antimony trisulfide composite material, stability is strong, recycling property is high, has
High photocatalytic activity, therefore, molybdenum disulfide of the invention-antimony trisulfide composite material is in photocatalysis removal Pollutants in Wastewater tool
There is potential application value；And with the Sb of one-dimentional structure2S3Nanometer rods are as matrix, compared to zero dimension, 2 and 3 dimensional organization,
It has many advantages, such as that transmission electron velocity is fast, light absorption is strong, intensity is big, not easy to reunite and adsorption area is big.Two sulphur of graphite-phase
Change molybdenum (MoS2) there is the two-dimensional structure being laminated, there is lesser band gap (1.8eV) and optical response range is wide, can be used as effective
The photocatalytic activity of co-catalyst raising semiconductor material.
2, the present invention provides a kind of molybdenum disulfide-antimony trisulfide composite material preparation method, simple hydro-thermal method is utilized
Prepare molybdenum disulfide-antimony trisulfide composite material.Preparation method simple process of the invention, easy control of reaction conditions, operation
Method is simple and low in cost.
3, molybdenum disulfide of the invention-antimony trisulfide composite material has good photocatalysis under visible light or near infrared light
Performance can be widely used for light removal waste water from dyestuff field, remove Cr VI waste water from dyestuff especially suitable for light, has technique letter
Single, the advantages that operation is convenient, excellent catalytic effect.
Detailed description of the invention
Fig. 1 is MoS2、Sb2S3And the molybdenum disulfide in the embodiment of the present invention 1-corresponding SEM of antimony trisulfide composite material
Figure.
Fig. 2 is the corresponding TEM figure of molybdenum disulfide-antimony trisulfide composite material in the embodiment of the present invention 1, and (a) and (b) figure are
It is shot from different location.
Fig. 3 is the distribution diagram of element of a-quadrant in the TEM figure of Fig. 2 (b).
Fig. 4 is the schematic diagram for the Cr VI that molybdenum disulfide of the invention-antimony trisulfide composite material photocatalysis removes in waste water.
Fig. 5 is Sb2S3And in the molybdenum disulfide of the embodiment of the present invention 1-antimony trisulfide composite material photo catalytic reduction waste water
The relational graph of m- removal efficiency when Cr VI is corresponding.
Fig. 6 is six in molybdenum disulfide-antimony trisulfide composite material photo catalytic reduction waste water in the embodiment of the present invention 1~3
The relational graph of valence chromium m- removal efficiency when corresponding.
Fig. 7 is molybdenum disulfide-antimony trisulfide composite material circular response five times photocatalysis performance in the embodiment of the present invention 1
Curve graph.
Specific embodiment
Below in conjunction with Figure of description and specific preferred embodiment, the invention will be further described, but not therefore and
It limits the scope of the invention.
Material employed in following embodiment and instrument are commercially available.
Embodiment 1:
A kind of molybdenum disulfide of the invention-antimony trisulfide composite material, the composite material include molybdenum disulfide and antimony trisulfide,
Middle molybdenum disulfide be bulk, antimony trisulfide be it is rodlike, block-like molybdenum disulfide is doped in rodlike antimony trisulfide surface and centre, wherein
The mass fraction of molybdenum disulfide is 8%.
A kind of preparation method of the molybdenum disulfide of above-mentioned the present embodiment-antimony trisulfide composite material, comprising the following steps:
(1) 242mg sodium molybdate and 601mg thioacetamide (the two molar ratio is 1: 8) are dissolved in deionized water, are shifted
Into polytetrafluoroethylene (PTFE) slot, 180 DEG C of progress hydrothermal synthesis are heated to, after maintaining 24 hours, natural cooling.Reaction product is successive
It is washed with deionized water, dehydrated alcohol, is then centrifuged for separating, centrifugal speed is 7000 revs/min, and centrifugation time is 3 minutes,
Dry 6h in the environment of temperature is 60 DEG C again, obtains product, with mortar grinder to powdered, obtains the curing of bright black
Molybdenum.
(2) it takes the resulting molybdenum disulfide 15mg of step (1) to be added in the sodium hydroxide solution that 50ml concentration is 1mol/L to surpass
Sound disperses 10min, and nine water vulcanized sodium of 800mg is and then added as sulphur source, obtains the hydroxide containing molybdenum disulfide and vulcanized sodium
Sodium solution.
(3) 228mg antimony chloride is dissolved in the hydrochloric acid solution that 25mL concentration is 6mol/L, obtains the hydrochloric acid of chloride containing antimony
Solution.
(4) by the hydrochloric acid solution of the resulting chloride containing antimony of step (3) be added dropwise step (2) it is resulting containing molybdenum disulfide and
It is stirred continuously reaction in the sodium hydroxide solution of vulcanized sodium, after solution becomes orange completely, then stirs 30 minutes persistently with true
Fully reacting is protected, supernatant is outwelled, obtains orange molybdenum disulfide-vulcanization antimony precursors；
(5) the resulting molybdenum disulfide of step (4)-vulcanization antimony precursors are transferred in polytetrafluoroethylene (PTFE) slot, are heated to 100
DEG C maintain 12 hours after, natural cooling.It is dry in the environment of temperature is 60 DEG C after reaction product is washed with deionized
12h takes out product, with mortar grinder to powdered, obtains molybdenum disulfide-antimony trisulfide composite material.
Fig. 1 is MoS2、Sb2S3And the molybdenum disulfide of the present embodiment-antimony trisulfide composite material (MoS2/Sb2S3- 8%) corresponding
SEM figure.Wherein (a) figure is MoS2, (b) figure is Sb2S3, (c) figure is the molybdenum disulfide-antimony trisulfide composite material of the present embodiment.
As can be seen that MoS from (a) figure2In irregular bulk, as can be seen that Sb from (b) figure2S3In not of uniform size rodlike, from
(c) figure can be seen that irregular rodlike Sb2S3Appear in blocky MoS2Surface, part then appear in blocky MoS2Block and block
Between gap in, illustrate MoS2Successfully it is doped in Sb2S3In.
Fig. 2 and Fig. 3 is respectively the molybdenum disulfide-antimony trisulfide composite material (MoS of the present embodiment2/Sb2S3- 8%) corresponding
TEM figure and distribution diagram of element.(a) and (b) figure are the molybdenum disulfide-antimony trisulfide composite material of the present embodiment from different positions in Fig. 2
Set the TEM figure of shooting, it can be seen that MoS2In irregular sheet, Sb2S3In rodlike, the MoS of sheet2With rodlike Sb2S3It is interspersed
Together, MoS is further confirmed2Successfully it is doped in Sb2S3In.Fig. 3 be material corresponding diagram 2(b) in a-quadrant Elemental redistribution
Figure, wherein (A-1) is the distribution of Mo element, (A-2) is the distribution of S element, and (A-3) is the distribution of Sb element, it can be seen that Mo,
S, Sb Elemental redistribution demonstrates MoS in molybdenum disulfide-antimony trisulfide composite material2Successfully it is doped in Sb2S3。
Embodiment 2:
A kind of molybdenum disulfide of the invention-antimony trisulfide composite material, including molybdenum disulfide and antimony trisulfide, wherein molybdenum disulfide
For bulk, antimony trisulfide be it is rodlike, block-like molybdenum disulfide is doped in rodlike antimony trisulfide surface and centre, wherein molybdenum disulfide
Mass fraction is 5%.
A kind of preparation method of the molybdenum disulfide of above-mentioned the present embodiment-antimony trisulfide composite material, the preparation side with embodiment 1
The difference of method is only that in step (2) that molybdenum disulfide dosage is 10mg, remaining step is all the same.
Embodiment 3:
A kind of molybdenum disulfide of the invention-antimony trisulfide composite material, including molybdenum disulfide and antimony trisulfide, wherein molybdenum disulfide
For bulk, antimony trisulfide be it is rodlike, block-like molybdenum disulfide is doped in rodlike antimony trisulfide surface and centre, wherein molybdenum disulfide
Mass fraction is 11%.
A kind of preparation method of the molybdenum disulfide of above-mentioned the present embodiment-antimony trisulfide composite material, the preparation side with embodiment 1
The difference of method is only that in step (2) that molybdenum disulfide dosage is 20mg, remaining step is all the same.
Embodiment 4:
A kind of molybdenum disulfide of embodiment 1-antimony trisulfide composite material and Sb2S3The effect of Cr VI in removal waste water
Comparison, comprising the following steps:
(1) 2 groups of (group 1 and group 2) each 50ml of hexavalent chromium solution that concentration is 50mg/L are prepared, the solution of preparation is put in yin
Dark place.
(2) Sb is weighed2S3With molybdenum disulfide-each 50mg of antimony trisulfide composite material of embodiment 1, by weighed Sb2S3It is added
Into the hexavalent chromium solution of group 1, molybdenum disulfide-antimony trisulfide composite material of embodiment 1 is added in the hexavalent chromium solution of group 2,
One hour of magnetic agitation reaches adsorption equilibrium in the dark.To represent initial liquid to be degraded, i.e., every group is taken out 3ml solution
Solution when reaction time is 0min, surveys its concentration with UV, visible light spectrophotometer, and be denoted as C0。
(3) by 2 groups of remaining solution in step (2) visible light (use near infrared light can also with) light source 300W xenon lamp
Irradiation is lower to be carried out light-catalyzed reaction and starts timing, and light source and liquid level distance are 15cm.
(4) 3ml solution is drawn out of every group reaction system every 30min, after being filtered with 0.45 μm of filter of water phase
Clear liquid surveys Cr VI residual concentration in clear liquid with UV, visible light spectrophotometer.After illumination reaction 120min, xenon lamp is closed.
Fig. 4 is the reduction of the Cr VI in molybdenum disulfide-antimony trisulfide composite material photo catalytic reduction waste water in the present invention
Mechanism figure.Wherein, e-Indicate electronics, h+Indicate hole.As shown, when light is irradiated in MoS2/Sb2S3After composite material,
MoS2In electron excitation transit to conduction band (CB), due to MoS2Conduction band positions ratio Sb2S3Conduction band positions it is more negative, MoS2Conduction band
On electronics transfer to Sb2S3On conduction band and leave hole.Meanwhile the hole of generation is from Sb2S3Valence band (VB) is transferred to MoS2
Valence band.So light induced electron makes its removal for the Cr VI that those are adsorbed on photocatalyst surface is attacked.
Fig. 5 is Sb2S3And in the molybdenum disulfide in the embodiment of the present invention 1-antimony trisulfide composite material photo catalytic reduction waste water
Cr VI it is corresponding when m- removal efficiency relational graph.Wherein C represents the residual concentration of the Cr VI after illumination, C0It indicates
Cr VI initial concentration.With C/C0For ordinate, using light application time as abscissa, Sb2S3And two in the embodiment of the present invention 1
Molybdenum sulfide-antimony trisulfide composite material photocatalysis performance curve is as shown in Figure 5.As seen from the figure, it is seen that after light irradiates 120min,
Sb2S3To the removal of Cr VI almost without effect, and the molybdenum disulfide in the embodiment of the present invention 1-antimony trisulfide composite material is to six
Valence chromium reduction efficiency reaches 99%, hence it is evident that higher than monomer to the removal rate of Cr VI.This shows molybdenum disulfide-vulcanization of the invention
Antimony composite material has very strong photocatalytic activity.
Embodiment 5:
A kind of application of the molybdenum disulfide of Examples 1 to 3-antimony trisulfide composite material in hexavalent chromium wastewater processing, including
Following steps:
(1) 3 groups of (group 1, group 2 and group 3) chromyl waste water from dyestuff 50mL are taken, the concentration of Cr VI is in every group
50mg/L.It is molybdenum disulfide-antimony trisulfide composite material that 1g/L adds embodiment 1 in the waste water from dyestuff of group 1 according to dosage, presses
It is molybdenum disulfide-antimony trisulfide composite material that 1g/L adds embodiment 2 in the waste water from dyestuff of group 2 according to dosage, is according to dosage
1g/L adds molybdenum disulfide-antimony trisulfide composite material of embodiment 3 in the waste water from dyestuff of group 3.MoS in Examples 1 to 32's
Mass percentage respectively may be about 8%, 5% and 11%, number consecutively MoS2/Sb2S3- 8%, MoS2/Sb2S3- 5%, MoS2/Sb2S3-
11%。
(2) every group of reaction system (added with the chromyl waste water of molybdenum disulfide-antimony trisulfide composite material) is set
In on magnetic stirring apparatus, being protected from light stirring 1h, molybdenum disulfide-antimony trisulfide composite material and pollutant waste water is made to reach adsorption equilibrium,
Take out 3ml solution respectively from 3 groups to represent the initial liquid that each group waits for illumination, i.e., the solution when reaction time is 0min, with purple
Outer visible spectrophotometric instrument surveys its concentration, and is denoted as C0。
(3) by 3 groups of remaining solution in step (2) visible light (use near infrared light can also with) light source 300W xenon lamp
Irradiation is lower to be carried out light-catalyzed reaction and starts timing, and light source and liquid level distance are 15cm.Every 30min from every group of reaction system
Interior each absorption 3ml solution surveys sexavalence in clear liquid with UV, visible light spectrophotometer with clear liquid is obtained after 0.45 μm of filter filtering of water phase
Chromium residual concentration.After illumination reaction 120min, xenon lamp is closed.
Fig. 6 is molybdenum disulfide-antimony trisulfide composite material reduction of hexavalent chromium under visible light of the embodiment of the present invention 1~3
Performance curve.Wherein C represents the concentration of the Cr VI after degradation, C0Indicate Cr VI initial concentration.With C/C0For ordinate, with
Light application time is abscissa.As seen from the figure, with MoS2Specific gravity in molybdenum disulfide-antimony trisulfide composite material gradually increases,
Molybdenum disulfide-antimony trisulfide composite material enhances six-valent chromium degrading efficiency therewith, works as MoS2Specific gravity when increasing to 8%, curing
Molybdenum-antimony trisulfide composite material reaches maximum value 99% to six-valent chromium degrading efficiency.And work as MoS2When specific gravity continues growing, curing
Molybdenum-antimony trisulfide composite material gradually decreases six-valent chromium degrading efficiency.The molybdenum disulfide of embodiment 2-antimony trisulfide composite material
(MoS2/Sb2S3- 5%), the molybdenum disulfide of embodiment 1-antimony trisulfide composite material (MoS2/Sb2S3- 8%) and two sulphur of embodiment 3
Change molybdenum-antimony trisulfide composite material (MoS2/Sb2S3It -11%) is respectively 49%, 99%, 82% to six-valent chromium degrading efficiency.Pass through the figure
As can be seen that molybdenum disulfide-antimony trisulfide composite material (MoS of embodiment 12/Sb2S3- 8%) photocatalytic degradation of Cr VI is imitated
Fruit is best.
Embodiment 6:
The corrosion resistance and stabilization of a kind of molybdenum disulfide of the invention-antimony trisulfide composite material in Photocatalytic Degradation Process
Journal of Sex Research, comprising the following steps:
(1) molybdenum disulfide-antimony trisulfide composite material for weighing 50mg embodiment 1, is added to the chromyl waste water of 50ml
In, hexavalent chromium concentration 50mg/L.
(2) reaction system (waste water added with molybdenum disulfide-antimony trisulfide composite material Cr VI) magnetic force is placed in stir
It mixes on device, is protected from light stirring 1h to reach adsorption equilibrium, be taken out 3ml solution to represent initial liquid to be degraded, that is, when reacting
Between be 0min when solution, survey its concentration with UV, visible light spectrophotometer, and be denoted as C0。
(3) by step (2) remaining solution under the xenon lamp of visible light (use near infrared light can also with) light source 300W into
Row light-catalyzed reaction simultaneously starts timing, and light source and liquid level distance are 15cm.3ml solution is taken out of reaction system every 30min, is used
Clear liquid is obtained after 0.45 μm of filter filtering of water phase, Cr VI residual concentration in clear liquid is surveyed with UV, visible light spectrophotometer, is denoted as Ct。
After illumination reaction 120min, xenon lamp is closed.
(4) solution after step (3) illumination reaction 120min is used into UV, visible light after 0.45 μm of filter filtering of water phase
Spectrophotometer surveys pollutant residual concentration in supernatant and calculates degradation efficiency.0.45 μm of filter separation material of water phase is used again
With waste water, molybdenum disulfide-antimony trisulfide composite material after reacting is collected, and being added to 50ml hexavalent chromium concentration again is 50mg/L
Waste water in.
(5) continue to repeat step (2)~(4) four times.
Fig. 7 is that molybdenum disulfide-antimony trisulfide composite material circular response five times photocatalysis performance of the embodiment of the present invention 1 is bent
Line.Using the removal efficiency of Cr VI as ordinate, using cycle-index as abscissa, as seen from the figure, after five circulations,
Molybdenum disulfide-antimony trisulfide composite material still shows efficient photocatalysis performance, and the removal efficiency of five circulations is followed successively by
99%, 97.5%, 96.9%, 95.1% and 94.8%.Thus illustrate that molybdenum disulfide-antimony trisulfide composite material is a kind of stabilization and efficiently
NEW TYPE OF COMPOSITE photochemical catalyst, have good actual application prospect.
The above described is only a preferred embodiment of the present invention, being not intended to limit the present invention in any form.Though
So the present invention is disclosed as above with preferred embodiment, and however, it is not intended to limit the invention.It is any to be familiar with those skilled in the art
Member, in the case where not departing from Spirit Essence of the invention and technical solution, all using in the methods and techniques of the disclosure above
Appearance makes many possible changes and modifications or equivalent example modified to equivalent change to technical solution of the present invention.Therefore,
Anything that does not depart from the technical scheme of the invention are made to the above embodiment any simple according to the technical essence of the invention
Modification, equivalent replacement, equivalence changes and modification, all of which are still within the scope of protection of the technical scheme of the invention.
Claims (9)
1. a kind of molybdenum disulfide-antimony trisulfide composite material preparation method, which comprises the following steps:
(1) sodium molybdate and thioacetamide is soluble in water, hydrothermal synthesis reaction is carried out, molybdenum disulfide is obtained；
(2) by the resulting molybdenum disulfide ultrasonic disperse of step (1) in sodium hydroxide solution, nine water vulcanized sodium conducts are then added
Sulphur source obtains the sodium hydroxide solution containing molybdenum disulfide and vulcanized sodium；The mass body of the molybdenum disulfide and sodium hydroxide solution
For product than being 200mg~400mg: 1L, the mass volume ratio of the nine water vulcanized sodium and sodium hydroxide solution is 7.2g~20g: 1L,
The concentration of the sodium hydroxide solution is 1mol/L~2mol/L；
(3) antimony chloride is dissolved in hydrochloric acid solution, obtains the hydrochloric acid solution of chloride containing antimony；
(4) that step (2) is added dropwise in the hydrochloric acid solution of the resulting chloride containing antimony of step (3) is resulting containing molybdenum disulfide and vulcanization
It is reacted in the sodium hydroxide solution of sodium, obtains molybdenum disulfide-vulcanization antimony precursors；
(5) the resulting molybdenum disulfide of step (4)-vulcanization antimony precursors are heated, obtains molybdenum disulfide-antimony trisulfide composite wood
Material；The temperature of the heating is 100 DEG C~150 DEG C, and the time of the heating is 12h~15h；
The molybdenum disulfide-antimony trisulfide composite material includes molybdenum disulfide and antimony trisulfide, and the molybdenum disulfide is doped in the sulphur
Change and constitutes molybdenum disulfide-antimony trisulfide composite material in antimony.
2. preparation method according to claim 1, which is characterized in that in the step (1), the sodium molybdate and thio second
The molar ratio of amide is 1: 2~8.
3. preparation method according to claim 1, which is characterized in that in the step (3), the antimony chloride and hydrochloric acid are molten
The mass volume ratio of liquid is 9g~12g: 1L, and the concentration of the hydrochloric acid solution is 6mol/L~8mol/L.
4. preparation method described in any one of claim 1 to 3, which is characterized in that in the step (1), the water
The condition of thermal synthesis reaction are as follows: heating temperature is 180 DEG C~200 DEG C, and heating time is for 24 hours~26h.
5. preparation method described in any one of claim 1 to 3, which is characterized in that in the step (1), the water
After thermal synthesis reaction, gained reaction product is successively used into deionized water, ethanol washing, is then centrifuged for separating, centrifugal rotational speed is
5000 revs/min~7000 revs/min, centrifugation time is 3 minutes~5 minutes, then drying in the environment of temperature is 50 DEG C~70 DEG C
4h~6h obtains molybdenum disulfide；
And/or in the step (5), after the heating, gained reaction product is washed with deionized, then temperature be 40
DEG C~60 DEG C in the environment of dry 6h~12h.
6. preparation method according to claim 1, which is characterized in that two in the molybdenum disulfide-antimony trisulfide composite material
The mass fraction of molybdenum sulfide is 5%~11%.
7. a kind of molybdenum disulfide-antimony trisulfide composite wood being prepared such as preparation method according to any one of claims 1 to 6
Expect the application of the Cr VI in removal waste water.
8. application according to claim 7, which is characterized in that the application is the following steps are included: by the molybdenum disulfide-
Antimony trisulfide composite material is added in waste water, and light-catalyzed reaction is carried out under visible light or near infrared light, completes to Cr VI
Reduction, the molybdenum disulfide-additive amount of the antimony trisulfide composite material in waste water are 0.8g/L~1.2g/L.
9. application according to claim 8, which is characterized in that in the application, by the curing under the conditions of being protected from light
Molybdenum-antimony trisulfide composite material is added in waste water and stirs；And/or the light source of the visible light or near infrared light be 300W~
The liquid level distance of the xenon lamp of 500W, the xenon lamp and the waste water is 14cm~16cm, and the time of the light-catalyzed reaction is
120min~150min；And/or the concentration of Cr VI is 50mg/L~60mg/L in the waste water.
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| CN108892175A (en) * | 2018-08-31 | 2018-11-27 | 济南大学 | A kind of preparation method and electro-catalysis application having defective vanadium doping molybdenum disulfide nano flower |
| CN109569658B (en) * | 2019-01-09 | 2021-04-02 | 中南大学 | Method for improving photoelectric property of antimony sulfide film |
| CN110681400B (en) * | 2019-09-30 | 2022-06-07 | 内江师范学院 | H-molybdenum trioxide/bimetal sulfide composite material, preparation method and application |
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