CN106166494B - A kind of sluggish precipitation preparation Sm (OH)3The method of/CdS nano-complex - Google Patents
A kind of sluggish precipitation preparation Sm (OH)3The method of/CdS nano-complex Download PDFInfo
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- CN106166494B CN106166494B CN201610530002.0A CN201610530002A CN106166494B CN 106166494 B CN106166494 B CN 106166494B CN 201610530002 A CN201610530002 A CN 201610530002A CN 106166494 B CN106166494 B CN 106166494B
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- 238000000034 method Methods 0.000 title claims abstract description 12
- 238000001556 precipitation Methods 0.000 title claims abstract description 10
- 238000002360 preparation method Methods 0.000 title abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 46
- 239000012153 distilled water Substances 0.000 claims abstract description 40
- 239000000843 powder Substances 0.000 claims abstract description 28
- 239000007788 liquid Substances 0.000 claims abstract description 23
- 238000005406 washing Methods 0.000 claims abstract description 22
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000002243 precursor Substances 0.000 claims abstract description 16
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims abstract description 8
- 150000007530 organic bases Chemical class 0.000 claims abstract description 8
- 238000001291 vacuum drying Methods 0.000 claims abstract description 5
- 239000000243 solution Substances 0.000 claims description 82
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 14
- 229960000935 dehydrated alcohol Drugs 0.000 claims description 12
- 238000013019 agitation Methods 0.000 claims description 10
- 239000011259 mixed solution Substances 0.000 claims description 6
- 239000012456 homogeneous solution Substances 0.000 claims description 5
- 238000004458 analytical method Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- 230000005611 electricity Effects 0.000 claims description 2
- 238000006243 chemical reaction Methods 0.000 abstract description 9
- 239000006185 dispersion Substances 0.000 abstract description 3
- YKYOUMDCQGMQQO-UHFFFAOYSA-L Cadmium chloride Inorganic materials Cl[Cd]Cl YKYOUMDCQGMQQO-UHFFFAOYSA-L 0.000 abstract description 2
- 229910052979 sodium sulfide Inorganic materials 0.000 abstract 1
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 abstract 1
- 229910052980 cadmium sulfide Inorganic materials 0.000 description 25
- 230000001699 photocatalysis Effects 0.000 description 4
- 238000007146 photocatalysis Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 2
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 2
- 229940043267 rhodamine b Drugs 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- WUPHOULIZUERAE-UHFFFAOYSA-N 3-(oxolan-2-yl)propanoic acid Chemical compound OC(=O)CCC1CCCO1 WUPHOULIZUERAE-UHFFFAOYSA-N 0.000 description 1
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 244000248349 Citrus limon Species 0.000 description 1
- 235000005979 Citrus limon Nutrition 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003985 ceramic capacitor Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000002500 effect on skin Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229960004756 ethanol Drugs 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 229910052747 lanthanoid Inorganic materials 0.000 description 1
- 150000002602 lanthanoids Chemical class 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- LGZXYFMMLRYXLK-UHFFFAOYSA-N mercury(2+);sulfide Chemical compound [S-2].[Hg+2] LGZXYFMMLRYXLK-UHFFFAOYSA-N 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000012429 reaction media Substances 0.000 description 1
- 239000002344 surface layer Substances 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—
Abstract
The present invention discloses a kind of sluggish precipitation preparation Sm (OH)3The method of/CdS nano-complex, comprising: 1) by Sm (NO)3·6H2O is dissolved in distilled water, obtained solution A；2) obtained solution of pH to 7~13 B of solution A is adjusted；3) solution B is aged；4) product washing, dry, obtained white powder C；5) citric acid and white powder C are completely dissolved in distilled water, obtained solution D；6) pure CdCl will be analyzed2It is dissolved in distilled water, obtained solution E；7) E solution is added in solution D, obtains precursor liquid；8) by Na2S·9H2O is dissolved in distilled water, obtained solution F；9) solution F is added in precursor liquid；Product washing is dried to obtain product Sm (OH)3/ CdS nano-complex.The present invention uses sluggish precipitation, and great advantage is to adjust the pH of reaction system using organic base diethylenetriamine, solution obtained, using the obtained Sm (OH) of vacuum drying3Nanometer rods, by itself and CdCl2And Na2The Sm (OH) that S is reacted3/ CdS purity is high, crystallinity is strong, pattern uniformly and good dispersion.
Description
Technical field
The present invention relates to Nano semiconductor field of composite material preparation, in particular to a kind of to prepare Sm (OH)3/ CdS nanometers
The method of compound.
Background technique
Samaric hydroxide (Sm (OH)3) it is used as a kind of promising group of the lanthanides functional material, in catalysis material and opto-electronic device
In have certain application potential.Sm(OH)3It is a kind of with 4f electronic structure hydroxide, when temperature is increased to 180 from 140 DEG C
DEG C when pure hexagonal phase Sm (OH)3Forbidden bandwidth is 3.89-3.97eV, Sm (OH) at this time3With superior electricity, optics and magnetic
Performance is learned, ceramic capacitor, vehicle maintenance service, catalyst and medicine etc. are widely used in；
CdS crystal is divided into two kinds of α-types, lemon yellow powder, density 3.91~4.15；β-type, Chinese red powder, density
4.48~4.51.There are greenockite, hex crystal, density 4.82 in nature.It can distil in nitrogen.It is slightly soluble in water and ethyl alcohol,
It is dissolved in acid, is highly soluble in ammonium hydroxide.High-purity is good semiconductor.Forbidden bandwidth Eg=2.42ev, cadmium sulfide optical conductor are dashed forward
Out the advantages of is that electrostatic latent image potential difference is big, and the image contrast run off is big.Because surface layer is added with insulating film.
Because with nano material share small-size effect and skin effect, CdS light absorption, in terms of all
Show special effect, catalysis material, electrode material and in terms of all obtained extensively
Research and application.So, Sm (OH)3It is limited with the photocatalysis performance of CdS.
Summary of the invention
The purpose of the present invention is to provide a kind of sluggish precipitations to prepare Sm (OH)3The method of/CdS nano-complex, should
Reaction medium is aqueous solution in method, and the nanometer particle size narrow distribution of products therefrom, good dispersion, cost is relatively low, it is easy to accomplish
Industrialized production；Prepared Sm (OH)3/ CdS nano-complex has preferable photocatalysis performance.
To achieve the goals above, the present invention adopts the following technical scheme:
A kind of sluggish precipitation preparation Sm (OH)3The method of/CdS nano-complex, comprising the following steps:
1) pure Sm (NO) will be analyzed3·6H2O is dissolved in distilled water, and it is 0.015-0.050mol/L solution A that concentration, which is made,；
2) pH to 7~13 for adjusting solution A is sufficiently stirred 0.5~5h and homogeneous solution B is made；
3) cooled to room temperature after being aged solution B；
4) product washing, dry, obtained white powder C；
5) by molar ratio (0.4~0.7): the pure citric acid of 1 analysis and white powder C are completely dissolved in distilled water,
20~70 DEG C of magnetic agitation 0.5~4h obtained solution D；The concentration of white powder C is 0.01-0.04mol/L in solution D；
6) pure CdCl will be analyzed2It is dissolved in distilled water, is completely dissolved, the solution E that concentration is 0.02-0.05mol/L is made；
7) E solution is slowly added into solution D, obtains mixed solution, and in 30~60 DEG C of 0.5~4h of magnetic agitation,
Precursor liquid is made；Wherein, white powder C and CdCl in E solution in solution D2Molar ratio are as follows: 0.5:1-3:1；
8) pure Na will be analyzed2S·9H2O is completely dissolved in distilled water, and the solution F that concentration is 0.01-0.05mol/L is made；
9) solution F is added in precursor liquid, Na in solution F2S·9H2O and CdCl in precursor liquid2Molar ratio be 0.5:
1-2:1；Product washing is dried to obtain product Sm (OH)3/ CdS nano-complex.
Further, the pH of solution A is adjusted in step 2) using organic base diethylenetriamine.
Further, solution B is aged 1~5h in 40~80 DEG C of water-baths in step 3).
Further, washing, drying in step 4) specifically: successively use distilled water and dehydrated alcohol centrifuge washing 4~6
Secondary, the product of collection is dried in vacuo 1~5h under the conditions of 40~80 DEG C.
Further, washing, drying in step 9) specifically: successively use distilled water and dehydrated alcohol centrifuge washing 4~6
Secondary, the product utilization electric vacunm drying case of collection is dried in vacuo 2~5h under the conditions of 40~80 DEG C and obtains Sm (OH)3/ CdS nanometers
Compound.
Compared with the existing technology, the invention has the following advantages: the present invention uses sluggish precipitation, great advantage exists
In the pH for adjusting reaction system using organic base diethylenetriamine, solution obtained, using the obtained Sm of vacuum drying
(OH)3Nanometer rods, by itself and CdCl2And Na2The Sm (OH) that S is reacted3/ CdS purity is high, crystallinity is strong, and pattern is uniform
And good dispersion.The raw material of the reaction is easy to get and at low cost, and process equipment is simple, and low energy consumption, and the reaction under normal pressure into
Row, with water as reaction dissolvent, safety is good, and feasibility is strong, thus it is very economical, practical, there is good industrial prospect.
Sm prepared by the present invention (OH)3/ CdS nano-complex is substantially better than Sm (OH)3With the photocatalysis performance of CdS.
Detailed description of the invention
Fig. 1 is Sm prepared by the present invention (OH)3The XRD diagram of/CdS nano-complex；
Fig. 2 is Sm prepared by the present invention (OH)3The photocatalysis performance figure of/CdS nano-complex.
Specific embodiment
Embodiment 1:
1) 0.5mmol is analyzed into pure Sm (NO)3·6H2O is dissolved in appropriate distilled water, is completely dissolved, and obtained concentration is
0.015mol/L solution A；
2) using the pH to 7 for analyzing pure organic base diethylenetriamine adjusting solution A, 1h is sufficiently stirred, homogeneous solution B is made；
3) solution B is put into 40 DEG C of constant water bath box and is aged 1.5h, after reaction cooled to room temperature；
4) product successively uses distilled water and dehydrated alcohol centrifuge washing 4 times, collects vacuum drying 1h of the product under 40, system
Obtain white powder C；
5) pure citric acid and white powder C will be analyzed to be completely dissolved in distilled water with the molar ratio of 0.4:1, in 30 DEG C of magnetic
Power stirs 1h obtained solution D；The concentration of white powder C is 0.01mol/L in solution D；
6) pure CdCl will be analyzed2It is dissolved in appropriate distilled water, is completely dissolved, the solution E that concentration is 0.02mol/L is made；
7) E solution is slowly added into solution D, obtains mixed solution, and in 30 DEG C of magnetic agitation 0.5h, forerunner is made
Liquid；Wherein, white powder C and CdCl in E solution in solution D2Molar ratio are as follows: 0.5:1；
8) pure Na will be analyzed2S·9H2O is dissolved in appropriate distilled water, is sufficiently dissolved, and it is the molten of 0.01mol/L that concentration, which is made,
Liquid F；
9) solution F is added in precursor liquid, Na in solution F2S·9H2O and CdCl in precursor liquid2Molar ratio be 2:1；
Product successively uses distilled water and dehydrated alcohol centrifuge washing 4 times, and the product of collection is dried in vacuo 2h under the conditions of 40 DEG C, is cooled to
Product Sm (OH) can be obtained in room temperature3/ CdS nano-complex.
Embodiment 2:
1) 1mmol is analyzed into pure Sm (NO)3·6H2O is dissolved in appropriate distilled water, is completely dissolved, and obtained concentration is
0.05mol/L solution A；
2) using the pH to 8 for analyzing pure organic base diethylenetriamine adjusting solution A, 0.5h is sufficiently stirred, homogeneous solution is made
B；
3) solution B is put into 50 DEG C of constant water bath box and is aged 1h, after reaction cooled to room temperature；
4) product successively uses distilled water and dehydrated alcohol centrifuge washing 5 times, vacuum of the product of collection under the conditions of 80 DEG C
Dry 2h, is made white powder C；
5) pure citric acid and white powder C will be analyzed to be completely dissolved in distilled water with the molar ratio of 1:2, in 40 DEG C of magnetic force
Stir 2.5h obtained solution D；The concentration of white powder C is 0.04mol/L in solution D；
6) pure CdCl will be analyzed2It is dissolved in appropriate distilled water, is completely dissolved, the solution E that concentration is 0.05mol/L is made；
7) E solution is slowly added into solution D, obtains mixed solution, and in 40 DEG C of magnetic agitation 1h, forerunner is made
Liquid；Wherein, white powder C and CdCl in E solution in solution D2Molar ratio are as follows: 3:1；
8) pure Na will be analyzed2S·9H2O is dissolved in appropriate distilled water, is completely dissolved, and it is the molten of 0.05mol/L that concentration, which is made,
Liquid F；
9) solution F is added in precursor liquid, Na in solution F2S·9H2O and CdCl in precursor liquid2Molar ratio be 0.5:
1；Product successively uses distilled water and dehydrated alcohol centrifuge washing 5 times, and the product of collection is dried in vacuo 5h under the conditions of 55 DEG C, cooling
Product Sm (OH) can be obtained to room temperature3/ CdS nano-complex.
Embodiment 3:
1) 1.5mmol is analyzed into pure Sm (NO)3·6H2O is dissolved in appropriate distilled water, obtained solution A, and obtained concentration is
0.02mol/L solution A；
2) using the pH to 13 for analyzing pure organic base diethylenetriamine adjusting solution A, 5h is sufficiently stirred, homogeneous solution is made
B；
3) solution B is put into 80 DEG C of constant water bath box and is aged 5h, after reaction cooled to room temperature；
4) product successively uses distilled water and dehydrated alcohol centrifuge washing 6 times, vacuum drying of the product of collection at 55 DEG C
White powder C is made in 5h；
5) pure citric acid will be analyzed and white powder C is dissolved in appropriate distilled water with the molar ratio of 0.6:1 and being completely dissolved,
70 DEG C of magnetic agitation 4h obtained solution D；The concentration of white powder C is 0.03mol/L in solution D；
6) pure CdCl is analyzed according to quantity2It is dissolved in appropriate distilled water, is completely dissolved, the solution that concentration is 0.03mol/L is made
E；
7) E solution is slowly added into solution D, obtains mixed solution, and in 60 DEG C of magnetic agitation 4h, forerunner is made
Liquid；Wherein, white powder C and CdCl in E solution in solution D2Molar ratio are as follows: 1:1；
8) pure Na will be analyzed2S·9H2O is dissolved in appropriate distilled water, is sufficiently dissolved, and it is the molten of 0.03mol/L that concentration, which is made,
Liquid F；
9) solution F is added in precursor liquid, Na in solution F2S·9H2O and CdCl in precursor liquid2Molar ratio be 1:1；
Product successively uses distilled water and dehydrated alcohol centrifuge washing 5 times, and the product of collection is dried in vacuo 2h under the conditions of 60 DEG C, is cooled to
Product Sm (OH) can be obtained in room temperature3/ CdS nano-complex.
Embodiment 4:
1) by the pure Sm of the analysis of 2mmol (NO)3·6H2O is dissolved in appropriate distilled water, is completely dissolved, and obtained concentration is
0.02mol/L solution A；
2) using the pH to 12 for analyzing pure organic base diethylenetriamine adjusting solution A, 1.5 obtained homogeneous solutions are sufficiently stirred
B；
3) solution B is put into 70 DEG C of constant water bath box and is aged 2h, after reaction cooled to room temperature；
4) product successively uses distilled water and dehydrated alcohol centrifuge washing 5 times, and the product of collection vacuum under the conditions of 65 DEG C is dry
White powder C is made in dry 2h；
5) pure citric acid will be analyzed and white powder C is dissolved in appropriate distilled water with the molar ratio of 0.7:1 and being completely dissolved,
20 DEG C of magnetic agitation 0.5h obtained solution D；The concentration of white powder C is 0.02mol/L in solution D；
6) by a certain amount of pure CdCl of analysis2It is dissolved in appropriate distilled water, is completely dissolved, it is 0.01mol/L's that concentration, which is made,
Solution E；
7) E solution is slowly added into solution D, obtains mixed solution, and in 50 DEG C of magnetic agitation 1h, forerunner is made
Liquid；Wherein, white powder C and CdCl in E solution in solution D2Molar ratio are as follows: 2:1；
8) pure Na will be analyzed2S·9H2O is dissolved in appropriate distilled water, and the solution F that concentration is 0.05mol/L is made；
9) solution F is added in precursor liquid, Na in solution F2S·9H2O and CdCl in precursor liquid2Molar ratio be 0.5:
1；Product successively uses distilled water and dehydrated alcohol centrifuge washing 6 times, and the product of collection is dried in vacuo 5h under the conditions of 80 DEG C, cooling
Product Sm (OH) can be obtained to room temperature3/CdS。
Fig. 1 is Sm prepared by the embodiment of the present invention 1 (OH)3The XRD of/CdS nano-complex, as can be seen from the figure from
It can be seen that the purity is high of product, crystallinity are strong in figure.Fig. 2 is Sm prepared by the embodiment of the present invention 1 (OH)3/ CdS is nano combined
Photocatalytic degradation figure of the object to rhodamine B；It can be seen from the figure that when 30min, Sm (OH)3/ CdS nano-complex
To the photocatalytic degradation of rhodamine B close to 100%, hence it is evident that better than the Sm (OH) of comparative test3And CdS.
Claims (3)
1. a kind of sluggish precipitation prepares Sm (OH)3The method of/CdS nano-complex, which comprises the following steps:
1) pure Sm (NO) will be analyzed3·6H2O is dissolved in distilled water, and it is 0.015-0.050mol/L solution A that concentration, which is made,；
2) pH to 7~13 for adjusting solution A is sufficiently stirred 0.5~5h and homogeneous solution B is made；
3) cooled to room temperature after being aged solution B；
4) product washing, dry, obtained white powder C；
5) by molar ratio (0.4~0.7): the pure citric acid of 1 analysis and white powder C are completely dissolved in distilled water, 20~
70 DEG C of magnetic agitation 0.5~4h obtained solution D；The concentration of white powder C is 0.01-0.04mol/L in solution D；
6) pure CdCl will be analyzed2It is dissolved in distilled water, is completely dissolved, the solution E that concentration is 0.02-0.05mol/L is made；
7) E solution is slowly added into solution D, obtains mixed solution, and in 30~60 DEG C of 0.5~4h of magnetic agitation, be made
Precursor liquid；Wherein, white powder C and CdCl in E solution in solution D2Molar ratio are as follows: 0.5:1-3:1；
8) pure Na will be analyzed2S·9H2O is completely dissolved in distilled water, and the solution F that concentration is 0.01-0.05mol/L is made；
9) solution F is added in precursor liquid, Na in solution F2S·9H2O and CdCl in precursor liquid2Molar ratio be 0.5:1-2:
1；Product washing is dried to obtain product Sm (OH)3/ CdS nano-complex；
The pH of solution A is adjusted in step 2) using organic base diethylenetriamine；
Solution B is aged 1~5h in 40~80 DEG C of water-baths in step 3).
2. sluggish precipitation according to claim 1 prepares Sm (OH)3The method of/CdS nano-complex: it is characterized by:
It is washing in step 4), dry specifically: successively use distilled water and dehydrated alcohol centrifuge washing 4~6 times, the product of collection in 40~
1~5h is dried in vacuo under the conditions of 80 DEG C.
3. sluggish precipitation according to claim 1 prepares Sm (OH)3The method of/CdS nano-complex: it is characterized by:
Washing, drying in step 9) specifically: successively use distilled water and dehydrated alcohol centrifuge washing 4~6 times, the product utilization electricity of collection
Thermal vacuum drying box is dried in vacuo 2~5h under the conditions of 40~80 DEG C and obtains Sm (OH)3/ CdS nano-complex.
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| CN106166494A (en) | 2016-11-30 |
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