CN107233910B - One type graphitic nitralloy carbon/stannous sulfide nano heterojunction synthetic method - Google Patents
One type graphitic nitralloy carbon/stannous sulfide nano heterojunction synthetic method Download PDFInfo
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- 238000010189 synthetic method Methods 0.000 title claims abstract description 15
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title abstract description 15
- 229910052799 carbon Inorganic materials 0.000 title abstract description 12
- DZXKSFDSPBRJPS-UHFFFAOYSA-N tin(2+);sulfide Chemical compound [S-2].[Sn+2] DZXKSFDSPBRJPS-UHFFFAOYSA-N 0.000 title abstract description 12
- 239000000725 suspension Substances 0.000 claims abstract description 22
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 18
- 239000010431 corundum Substances 0.000 claims abstract description 18
- 239000008367 deionised water Substances 0.000 claims abstract description 16
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 16
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000004202 carbamide Substances 0.000 claims abstract description 12
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims abstract description 10
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 claims abstract description 8
- 238000011065 in-situ storage Methods 0.000 claims abstract description 5
- 239000002105 nanoparticle Substances 0.000 claims abstract description 5
- 238000000926 separation method Methods 0.000 claims abstract description 3
- 239000000047 product Substances 0.000 claims description 21
- 239000007787 solid Substances 0.000 claims description 15
- 239000013049 sediment Substances 0.000 claims description 14
- 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 claims description 10
- 229960000907 methylthioninium chloride Drugs 0.000 claims description 10
- 239000011858 nanopowder Substances 0.000 claims description 9
- 229910052979 sodium sulfide Inorganic materials 0.000 claims description 9
- 238000004140 cleaning Methods 0.000 claims description 8
- 238000002360 preparation method Methods 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 7
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 7
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 7
- 239000004570 mortar (masonry) Substances 0.000 claims description 7
- 239000012265 solid product Substances 0.000 claims description 7
- 230000015556 catabolic process Effects 0.000 claims description 5
- 238000006731 degradation reaction Methods 0.000 claims description 5
- 238000005286 illumination Methods 0.000 claims description 3
- 229910052724 xenon Inorganic materials 0.000 claims description 3
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims description 3
- 239000007857 degradation product Substances 0.000 claims description 2
- AXZWODMDQAVCJE-UHFFFAOYSA-L tin(II) chloride (anhydrous) Chemical compound [Cl-].[Cl-].[Sn+2] AXZWODMDQAVCJE-UHFFFAOYSA-L 0.000 claims description 2
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims 2
- 229910052571 earthenware Inorganic materials 0.000 claims 1
- 238000007146 photocatalysis Methods 0.000 abstract description 7
- 230000001699 photocatalysis Effects 0.000 abstract description 6
- 238000003786 synthesis reaction Methods 0.000 abstract description 6
- 238000005516 engineering process Methods 0.000 abstract description 5
- 230000015572 biosynthetic process Effects 0.000 abstract description 4
- 238000005406 washing Methods 0.000 abstract description 2
- 238000003756 stirring Methods 0.000 abstract 2
- 239000012467 final product Substances 0.000 abstract 1
- 238000005303 weighing Methods 0.000 abstract 1
- 239000011734 sodium Substances 0.000 description 11
- 238000000034 method Methods 0.000 description 8
- 239000004065 semiconductor Substances 0.000 description 8
- VDQVEACBQKUUSU-UHFFFAOYSA-M disodium;sulfanide Chemical compound [Na+].[Na+].[SH-] VDQVEACBQKUUSU-UHFFFAOYSA-M 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 6
- 238000002791 soaking Methods 0.000 description 6
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 5
- 239000003125 aqueous solvent Substances 0.000 description 5
- 229910052708 sodium Inorganic materials 0.000 description 5
- 230000008859 change Effects 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 229910002804 graphite Inorganic materials 0.000 description 2
- 239000010439 graphite Substances 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 230000010748 Photoabsorption Effects 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 238000006053 organic reaction Methods 0.000 description 1
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 230000015843 photosynthesis, light reaction Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000012719 thermal polymerization 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
- B01J27/24—Nitrogen compounds
-
- 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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Carbon And Carbon Compounds (AREA)
- Catalysts (AREA)
Abstract
The present invention relates to a type graphitic nitralloy carbon/stannous sulfide (g-C3N4/ SnS) nano heterojunction synthetic method, include the following steps: that 1) weighing a certain amount of urea is put into corundum crucible；2) corundum crucible for filling urea is put into Muffle furnace to calcine at a certain temperature, obtains g-C3N4；3) a certain amount of SnCl is weighed2·2H2O is dissolved in deionized water, and a certain amount of g-C is added after being sufficiently stirred3N4, continue to stir；4) a certain amount of Na is weighed2S·9H2O is dissolved in deionized water, is added dropwise to g-C3N4And SnCl2Suspension in, through stirring sufficiently reaction；5) final product is obtained after separation, washing and drying.Synthesis technology of the present invention is simple, g-C3N4Growth in situ SnS nanoparticle in nanometer sheet, the g-C3N4/ SnS nano heterojunction has meso-hole structure feature, there is biggish specific surface area (80-90m2/ g), there is excellent photocatalysis performance under visible light conditions.
Description
Technical field
The present invention relates to a kind of chemical synthesis process of oxide semiconductor nano-powder, and in particular to a type graphite nitrogen
Change carbon/stannous sulfide (g-C3N4/ SnS) nano heterojunction synthetic method and product.
Background technique
Graphite phase carbon nitride (g-C3N4) it is a kind of organic polymer Nano semiconductor, metal component is not contained, is had similar
The laminated structure of graphene.With excellent chemical stability, semiconducting behavior, thermal stability, high-specific surface area, suitable energy level
Structure makes it be widely used in photolysis water hydrogen gas, the catalysis fields such as organic reaction and photocatalytic degradation of organic matter, causes
The attention of many researchers.However, pure phase g-C3N4Band gap is wide, it is seen that light utilization ratio is low, and photo-generate electron-hole is to multiple
It is fast to close rate.Therefore in order to widen g-C3N4Optical absorption spectra range, the present invention using with by the way of other semiconductors couplings to g-
C3N4It is modified.
Building heterojunction semiconductor can promote the transfers of photo-generate electron-hole pairs, and light induced electron and hole is effectively reduced
Recombination probability improves the separative efficiency of photo-generated carrier, increases its quantum efficiency, to improve photocatalysis performance.Semiconductor
The characteristics of hetero-junctions is can to control its forbidden bandwidth by adjusting constituent content, can also make wide band gap semiconducter and narrowband
Gap semiconductor is compound to widen spectral response range, can be improved solar energy utilization ratio.
The present invention chooses the different SnS and g-C of band gap width3N4System, SnS band gap magnitude is smaller, has under visible light conditions
Good photo absorption performance synthesizes g-C using thermal polymerization3N4Then nano powder uses precipitation method fabricated in situ nanometer g-C3N4/
SnS hetero-junctions, the product are expected to obtain under visible light conditions excellent photocatalysis performance, however g-C3N4The heterogeneous combination of/SnS
At method there is not yet related report.
Summary of the invention
The purpose of the present invention is to provide a type graphitic nitralloy carbon/stannous sulfide (g-C3N4/ SnS) nano heterojunction
Synthetic method, this method simple process, easy to operate, the product purity for reacting synthesis is high, and there is large specific surface area excellent light to urge
Change performance, fills up class graphitic nitralloy carbon/stannous sulfide (g-C3N4/ SnS) nanocomposite synthesis technical field blank.
The object of the invention to solve the technical problems adopts the following technical solutions to realize.It proposes according to the present invention
A type graphitic nitralloy carbon/stannous sulfide (g-C3N4/ SnS) nano heterojunction synthetic method, include the following steps:
(1) a certain amount of urea is weighed, places it in agate mortar after grinding and is transferred in corundum crucible；
(2) it is put into Muffle furnace and calcines after covering the corundum crucible in step (1), then cool to room temperature, take out, receive
Collect product g-C3N4；
(3) by SnCl2·2H2O is dissolved in deionized water, and uniform SnCl is obtained after being sufficiently stirred2Solution, acquired solution
Middle Sn2+Concentration be 0.2mol/L, in SnCl2G-C step (2) prepared is added in solution3N4Nano powder is sufficiently stirred mixed
It closes uniformly, is denoted as suspension A；
(4) by Na2S·9H2O is soluble in water, makes S in acquired solution2-Concentration be 0.2mol/L, then by Na2S solution
It is added with 0.5ml/min drop rate in the suspension A of step (3) preparation, 2h is stirred after completion of dropwise addition keeps its reaction abundant；Its
In, Na2The dropwise addition volume of S solution is equal to SnCl in suspension A2The volume of solution；
(5) product of step (4) is transferred in high-speed centrifuge and is centrifuged, solid is taken after centrifuge separation
Sediment cleans obtained solid sediment, then the solid product obtained after cleaning is put into drying box, in 50-
Dry 10-12h, obtains g-C at a temperature of 70 DEG C3N4/ SnS nano heterojunction.
The object of the invention to solve the technical problems also can be used following technical measures and further realize.
Type graphitic nitralloy carbon/stannous sulfide (g-C above-mentioned3N4/ SnS) nano heterojunction synthetic method, wherein
A certain amount of urea described in step (1) refers to that compactedness of the urea in corundum crucible is (50-60) %.
Type graphitic nitralloy carbon/stannous sulfide (g-C above-mentioned3N4/ SnS) nano heterojunction synthetic method, wherein
Holding temperature is 570-600 DEG C when calcining in step (2), and heating rate is 3-5 DEG C/min, soaking time 3-4h.
Type graphitic nitralloy carbon/stannous sulfide (g-C above-mentioned3N4/ SnS) nano heterojunction synthetic method, wherein
Cleaning method described in step (5) are as follows: successively obtained solid sediment is replaced using deionized water and dehydrated alcohol
Washing 3-5 times.
Type graphitic nitralloy carbon/stannous sulfide (g-C above-mentioned3N4/ SnS) nano heterojunction synthetic method, wherein
G-C obtained by step (5)3N4/ SnS nano heterojunction includes g-C3N4With SnS two-phase, wherein the mass fraction of SnS is (1-
10) %.
Type graphitic nitralloy carbon/stannous sulfide (g-C above-mentioned3N4/ SnS) nano heterojunction synthetic method, wherein
G-C in final gained synthetic product3N4For laminated structure, with a thickness of 20-30nm, g-C3N4Surface in situ growth has SnS nanometers
Particle, the diameter of SnS nano particle are 10-20nm.
The present invention has obvious advantages and beneficial effects compared with the existing technology, by above-mentioned technical proposal, the present invention
A kind of g-C3N4The synthetic method of/SnS nano heterojunction can reach comparable technical progress and practicability, and have in industry
Extensive utility value, at least have the advantage that
1, g-C is synthesized using two-step method3N4/ SnS nano heterojunction, synthesis technology used is simple, easy to operate, and reaction is closed
At product purity it is high.
2, the g-C of this method preparation3N4/ SnS nano heterojunction has meso-hole structure feature and biggish surface area
(80-90m2/ g), photocatalytic degradation experiment is carried out to methylene blue (MB) solution under visible light (xenon lamp) irradiation, it is shown that excellent
Different photocatalysis performance.
In conclusion a kind of g-C of the present invention3N4The synthetic method of/SnS nano heterojunction technically has significant progress,
And there is apparent good effect, it is really a new and innovative, progressive, practical new design.
The above description is only an overview of the technical scheme of the present invention, in order to better understand the technical means of the present invention,
And it can be implemented in accordance with the contents of the specification, and in order to allow above and other objects, features and advantages of the invention can
It is clearer and more comprehensible, it is special below to lift preferred embodiment, and cooperate attached drawing, detailed description are as follows.
Detailed description of the invention
Scheming (1) is g-C made from embodiment 13N4The XRD diagram of/SnS；
Scheming (2) is g-C made from embodiment 13N4The TEM of/SnS schemes；
Scheming (3) is g-C made from embodiment 13N4The concentration curve figure of/SnS degradation of methylene blue solution；
Scheming (4) is g-C made from embodiment 13N4/ SnS and g-C3N4Photocatalysis result under the same test conditions compares
Figure；
Specific embodiment
It is of the invention to reach the technical means and efficacy that predetermined goal of the invention is taken further to illustrate, below in conjunction with
Attached drawing and preferred embodiment, to a kind of g-C proposed according to the present invention3N4The synthetic method of/SnS nano heterojunction, it is specific real
Mode, structure, feature and its effect are applied, detailed description is as follows.
Embodiment 1:
(1) a certain amount of urea is weighed, places it in agate mortar after grinding and is transferred in corundum crucible；
(2) it being placed in Muffle furnace and calcines after covering the corundum crucible in step (1), heating rate is 3 DEG C/min,
Holding temperature is 600 DEG C, and soaking time 4h takes out after being cooled to room temperature, and collects product g-C3N4；
(3) a certain amount of SnCl is weighed2·2H2O is dissolved in deionized water, and uniform SnCl is obtained after being sufficiently stirred2Solution,
Sn in acquired solution2+Concentration be 0.2mol/L, in SnCl2A certain amount of g-C is added in solution3N4Nano powder is sufficiently stirred mixed
It closes uniformly, is denoted as suspension A；
(4) it weighs a certain amount of vulcanized sodium to be dissolved in aqueous solvent, makes S in acquired solution2-Concentration be 0.2 mol/L, so
Afterwards by Na2S solution is added with 0.5ml/min drop rate into the suspension A of step (3) preparation, and 2h is stirred after completion of dropwise addition
Keep its reaction abundant；Wherein, Na2The dropwise addition volume of S solution is equal to SnCl in suspension A2The volume of solution；
(5) product of step (4) is transferred in high-speed centrifuge and is centrifuged, take solid sediment, it
Afterwards, it successively uses deionized water and dehydrated alcohol alternately wash 3 times obtained solid sediment, then will be obtained after cleaning
Solid product be put into drying box, dry 10h at a temperature of 60 DEG C obtains g-C3N4/ SnS nano heterojunction.
Gained g-C3N4G-C in/SnS nano heterojunction3N4Mass fraction be 97%, SnS mass fraction be 3%.
The g-C that the present embodiment is obtained3N4/ SnS carries out XRD and TEM and tests, and test result is as depicted in figs. 1 and 2, by scheming
Known to: it include g-C in synthetic product3N4With SnS two-phase, g-C3N4For laminated structure, with a thickness of 20-30nm or so, surface
Growth in situ has SnS nano particle；The diameter of SnS nano particle is 10-20nm.
Photocatalysis performance test is carried out to synthetic product, takes the g-C of 0.05g respectively3N4(as a control group) and this implementation
The nanometer, composite semiconductor g-C of example synthesis3N4/ SnS (as test group) is used as photochemical catalyst, with methylene blue (MB) for target
Degradation product (concentration 7mg/L), the equal 50ml of volume select the xenon lamp of 150W as light source, and distance of the sample away from fluorescent tube is
15cm carries out photocatalytic degradation experiment.As a result as shown in figure 3, g-C after illumination 30min3N4/ SnS degrades to methylene blue solution
Almost, Fig. 4 shows by 30min illumination, g-C3N4Degradable MB degradation 62% or so, and g-C3N4The degradable MB of/SnS
Degradation 95%, comparison degradation results it can be concluded that, building composite semiconductor can significantly improve its photocatalysis performance.
Embodiment 2:
(1) a certain amount of urea is weighed, places it in agate mortar after grinding and is transferred in corundum crucible；
(2) it places after covering the corundum crucible in step (1) and is calcined in Muffle furnace, heating rate is 4 DEG C/min, is protected
Temperature is 570 DEG C, and soaking time 3h takes out after being cooled to room temperature, and collects product g-C3N4；
(3) a certain amount of SnCl is weighed2·2H2O is dissolved in deionized water, and uniform SnCl is obtained after being sufficiently stirred2Solution,
Sn in acquired solution2+Concentration be 0.2mol/L, in SnCl2The g-C that a certain amount of step (2) is prepared is added in solution3N4
Nano powder is thoroughly mixed uniformly；It is denoted as suspension A；
(4) it weighs a certain amount of vulcanized sodium to be dissolved in aqueous solvent, makes S in acquired solution2-Concentration be 0.2 mol/L, so
Afterwards by Na2S solution is added with 0.5ml/min drop rate into the suspension A of step (3) preparation, and 2h is stirred after completion of dropwise addition
Keep its reaction abundant；Wherein, Na2The dropwise addition volume of S solution is equal to SnCl in suspension A2The volume of solution；
(5) product of step (4) is transferred in high-speed centrifuge and is centrifuged, take solid sediment, it
Afterwards, it successively uses deionized water and dehydrated alcohol alternately wash 5 times obtained solid sediment, then will be obtained after cleaning
Solid product be put into drying box, dry 10h under the conditions of 70 DEG C obtains g-C3N4/ SnS nano heterojunction.
Gained g-C3N4G-C in/SnS nano heterojunction3N4Mass fraction be 95%, SnS mass fraction be 5%.
Embodiment 3:
(1) a certain amount of urea is weighed, places it in agate mortar after grinding and is transferred in corundum crucible；
(2) it places after covering the corundum crucible in step (1) and is calcined in Muffle furnace, heating rate is 3 DEG C/min, is protected
Temperature is 580 DEG C, and soaking time 3h takes out after being cooled to room temperature, and collects product g-C3N4；
(3) a certain amount of SnCl is weighed2·2H2O is dissolved in deionized water, and uniform SnCl is obtained after being sufficiently stirred2Solution,
Sn in acquired solution2+Concentration be 0.2mol/L, in SnCl2The g-C that a certain amount of step (2) is prepared is added in solution3N4
Nano powder is thoroughly mixed uniformly；It is denoted as suspension A；
(4) it weighs a certain amount of vulcanized sodium to be dissolved in aqueous solvent, makes S in acquired solution2-Concentration be 0.2 mol/L, so
Afterwards by Na2S solution is added with 0.5ml/min drop rate into the suspension A of step (3) preparation, and 2h is stirred after completion of dropwise addition
Keep its reaction abundant；Wherein, Na2The dropwise addition volume of S solution is equal to SnCl in suspension A2The volume of solution；
(5) product of step (4) is transferred in high-speed centrifuge and is centrifuged, take solid sediment, it
Afterwards, it successively uses deionized water and dehydrated alcohol alternately wash 3 times obtained solid sediment, then will be obtained after cleaning
Solid product be put into drying box, dry 12h under the conditions of 70 DEG C obtains g-C3N4/ SnS nano heterojunction.
Gained g-C3N4G-C in/SnS nano heterojunction3N4Mass fraction be 90%, SnS mass fraction be 10%.
Embodiment 4:
(1) a certain amount of urea is weighed, places it in agate mortar after grinding and is transferred in corundum crucible；
(2) it places after covering the corundum crucible in step (1) and is calcined in Muffle furnace, heating rate is 5 DEG C/min, is protected
Temperature is 600 DEG C, and soaking time 4h takes out after being cooled to room temperature, and collects product g-C3N4；
(3) a certain amount of SnCl is weighed2·2H2O is dissolved in deionized water, and uniform SnCl is obtained after being sufficiently stirred2Solution,
Sn in acquired solution2+Concentration be 0.2mol/L, in SnCl2The g-C that a certain amount of step (2) is prepared is added in solution3N4
Nano powder is thoroughly mixed uniformly；It is denoted as suspension A；
(4) it weighs a certain amount of vulcanized sodium to be dissolved in aqueous solvent, makes S in acquired solution2-Concentration be 0.2 mol/L, so
Afterwards by Na2S solution is added with 0.5ml/min drop rate into the suspension A of step (3) preparation, and 2h is stirred after completion of dropwise addition
Keep its reaction abundant；Wherein, Na2The dropwise addition volume of S solution is equal to SnCl in suspension A2The volume of solution；
(5) product of step (4) is transferred in high-speed centrifuge and is centrifuged, take solid sediment, it
Afterwards, it successively uses deionized water and dehydrated alcohol alternately wash 4 times obtained solid sediment, then will be obtained after cleaning
Solid product be put into drying box, dry 12h under the conditions of 65 DEG C obtains g-C3N4/ SnS nano heterojunction.
Gained g-C3N4G-C in/SnS nano heterojunction3N4Mass fraction be 94%, SnS mass fraction be 6%.
Embodiment 5:
(1) a certain amount of urea is weighed, places it in agate mortar after grinding and is transferred in corundum crucible；
(2) it places after covering the corundum crucible in step (1) and is calcined in Muffle furnace, heating rate is 4 DEG C/min, is protected
Temperature is 590 DEG C, and soaking time 4h takes out after being cooled to room temperature, and collects product g-C3N4；
(3) a certain amount of SnCl is weighed2·2H2O is dissolved in deionized water, and uniform SnCl is obtained after being sufficiently stirred2Solution,
Sn in acquired solution2+Concentration be 0.2mol/L, in SnCl2The g-C that a certain amount of step (2) is prepared is added in solution3N4
Nano powder is thoroughly mixed uniformly；It is denoted as suspension A；
(4) it weighs a certain amount of vulcanized sodium to be dissolved in aqueous solvent, makes S in acquired solution2-Concentration be 0.2 mol/L, so
Afterwards by Na2S solution is added with 0.5ml/min drop rate into the suspension A of step (3) preparation, and 2h is stirred after completion of dropwise addition
Keep its reaction abundant；Wherein, Na2The dropwise addition volume of S solution is equal to SnCl in suspension A2The volume of solution；
(5) product of step (4) is transferred in high-speed centrifuge and is centrifuged, take solid sediment, it
Afterwards, it successively uses deionized water and dehydrated alcohol alternately wash 4 times obtained solid sediment, then will be obtained after cleaning
To solid product be put into drying box, dry 12h under the conditions of 60 DEG C obtains g-C3N4/ SnS nano heterojunction.
Gained g-C3N4G-C in/SnS nano heterojunction3N4Mass fraction be 92%, SnS mass fraction be 8%.
The above described is only a preferred embodiment of the present invention, be not intended to limit the present invention in any form, though
So the present invention has been disclosed as a preferred embodiment, and however, it is not intended to limit the invention, any technology people for being familiar with this profession
Member, without departing from the scope of the present invention, when the technology contents using the disclosure above make a little change or modification
For the equivalent embodiment of equivalent variations, but anything that does not depart from the technical scheme of the invention content, according to the technical essence of the invention
Any simple modification, equivalent change and modification to the above embodiments, all of which are still within the scope of the technical scheme of the invention.
Claims (1)
1. a kind of g-C3N4The synthetic method of/SnS nano heterojunction, it is characterised in that include the following steps:
(1) a certain amount of urea is weighed, places it in agate mortar after grinding and is transferred in corundum crucible, urea is in corundum earthenware
Compactedness in crucible is (50-60) %；
(2) it is put into Muffle furnace and calcines after covering the corundum crucible in step (1), heated up with the rate of 3 DEG C/min, 600
4h is kept the temperature at DEG C, is then cooled to room temperature, is taken out, and product g-C is collected3N4；
(3) by SnCl2·2H2O is dissolved in deionized water, and uniform SnCl is obtained after being sufficiently stirred2Solution, Sn in acquired solution2+
Concentration be 0.2mol/L, in SnCl2G-C step (2) prepared is added in solution3N4Nano powder is thoroughly mixed
It is even, it is denoted as suspension A；
(4) by Na2S·9H2O is soluble in water, makes S in acquired solution2-Concentration be 0.2mol/L, then by Na2S solution with
0.5mL/min drop rate is added in the suspension A of step (3) preparation, and 2h is stirred after completion of dropwise addition keeps its reaction abundant；Its
In, Na2The dropwise addition volume of S solution is equal to SnCl in suspension A2The volume of solution；
(5) product of step (4) is transferred in high-speed centrifuge and is centrifuged, take solid to precipitate after centrifuge separation
Object successively uses deionized water and dehydrated alcohol alternately wash 3 times obtained solid sediment, then will obtain after cleaning
Solid product be put into drying box, the dry 10h at 60 DEG C obtains g-C3N4/ SnS nano heterojunction；Gained g-C3N4/SnS
G-C in nano heterojunction3N4Mass fraction be 97%, SnS mass fraction be 3%；The g-C3N4In/SnS nano heterojunction
Include g-C3N4With SnS two-phase, g-C3N4For laminated structure, with a thickness of 20-30nm, it is 10- that surface in situ growth, which has diameter,
The SnS nano particle of 20nm；
The methylene blue for selecting 50mL 7mg/L is target degradation product, using the xenon lamp of 150W as light source, gained after illumination 30min
g-C3N4The degradation rate of the nano heterogeneous peering methylene blue of/SnS is 95%.
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| CN103934012A (en) * | 2014-04-14 | 2014-07-23 | 大连民族学院 | SnS2/g-C3N4 composite nanosheet photocatalyst and preparation method thereof |
| CN106475117A (en) * | 2016-09-14 | 2017-03-08 | 东北师范大学 | A kind of preparation of three-dimensional ZnO SnS P N hetero-junctions and application |
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| CN103934012A (en) * | 2014-04-14 | 2014-07-23 | 大连民族学院 | SnS2/g-C3N4 composite nanosheet photocatalyst and preparation method thereof |
| CN106475117A (en) * | 2016-09-14 | 2017-03-08 | 东北师范大学 | A kind of preparation of three-dimensional ZnO SnS P N hetero-junctions and application |
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