CN110975887A - SiO (silicon dioxide)2/Ag2Preparation method of S composite powder - Google Patents
SiO (silicon dioxide)2/Ag2Preparation method of S composite powder Download PDFInfo
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- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 239000000377 silicon dioxide Substances 0.000 title claims abstract description 44
- 239000002131 composite material Substances 0.000 title claims abstract description 33
- 239000000843 powder Substances 0.000 title claims abstract description 30
- 235000012239 silicon dioxide Nutrition 0.000 title claims abstract description 6
- 238000000034 method Methods 0.000 title claims description 12
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 38
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 38
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 38
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 38
- 239000000243 solution Substances 0.000 claims abstract description 31
- 239000004005 microsphere Substances 0.000 claims abstract description 26
- 238000002360 preparation method Methods 0.000 claims abstract description 25
- 239000000839 emulsion Substances 0.000 claims abstract description 23
- 229920000058 polyacrylate Polymers 0.000 claims abstract description 22
- 238000003756 stirring Methods 0.000 claims abstract description 16
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 12
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000011259 mixed solution Substances 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000008367 deionised water Substances 0.000 claims abstract description 8
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 8
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(I) nitrate Inorganic materials [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims abstract description 8
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 8
- OYNOOANKSLJSCV-UHFFFAOYSA-N silver;thiourea Chemical compound [Ag].NC(N)=S OYNOOANKSLJSCV-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000001035 drying Methods 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 4
- 239000007864 aqueous solution Substances 0.000 claims abstract description 4
- 238000001914 filtration Methods 0.000 claims abstract description 4
- 238000005406 washing Methods 0.000 claims abstract description 4
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical group [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 9
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 9
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 9
- 229910052946 acanthite Inorganic materials 0.000 claims description 8
- FSJWWSXPIWGYKC-UHFFFAOYSA-M silver;silver;sulfanide Chemical compound [SH-].[Ag].[Ag+] FSJWWSXPIWGYKC-UHFFFAOYSA-M 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 5
- 239000002244 precipitate Substances 0.000 claims description 3
- 239000002245 particle Substances 0.000 abstract description 24
- 230000000694 effects Effects 0.000 abstract description 5
- 239000011941 photocatalyst Substances 0.000 abstract description 5
- 238000000975 co-precipitation Methods 0.000 abstract description 3
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 3
- 239000000047 product Substances 0.000 description 12
- 238000009826 distribution Methods 0.000 description 7
- 238000001228 spectrum Methods 0.000 description 6
- 238000010521 absorption reaction Methods 0.000 description 5
- 238000002474 experimental method Methods 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 238000010335 hydrothermal treatment Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 230000000536 complexating effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 238000010899 nucleation Methods 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 239000012629 purifying agent Substances 0.000 description 2
- 239000010865 sewage Substances 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 239000006104 solid solution Substances 0.000 description 2
- KEQXNNJHMWSZHK-UHFFFAOYSA-L 1,3,2,4$l^{2}-dioxathiaplumbetane 2,2-dioxide Chemical compound [Pb+2].[O-]S([O-])(=O)=O KEQXNNJHMWSZHK-UHFFFAOYSA-L 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- -1 and at the same time Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000007431 microscopic evaluation Methods 0.000 description 1
- 239000008267 milk Substances 0.000 description 1
- 210000004080 milk Anatomy 0.000 description 1
- 235000013336 milk Nutrition 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- XUARKZBEFFVFRG-UHFFFAOYSA-N silver sulfide Chemical compound [S-2].[Ag+].[Ag+] XUARKZBEFFVFRG-UHFFFAOYSA-N 0.000 description 1
- 229940056910 silver sulfide Drugs 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000010183 spectrum analysis Methods 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
- C01B33/145—Preparation of hydroorganosols, organosols or dispersions in an organic medium
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
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- Hydrology & Water Resources (AREA)
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Abstract
SiO (silicon dioxide)2/Ag2A preparation method of S composite powder relates to the technical field of composite photocatalyst preparation. Uniformly mixing absolute ethyl alcohol and deionized water in a beaker, adding a morphology control agent and a polyacrylate emulsion, stirring and uniformly mixing, slowly dropwise adding ethyl orthosilicate into the mixed solution, and heating to react after dropwise adding is finished to obtain SiO2A colloidal solution; mixing AgNO3Dripping the solution into thiourea aqueous solution to form thiourea silver complex, uniformly stirring, and dripping SiO2Colloidal solution, reacting at room temperature to generate black precipitateAnd then washing, filtering and drying. The invention can reduce the nano SiO to a certain extent by adding a proper amount of polyacrylate emulsion2The particle size of the microspheres can be controlled by adding different shape control agents to obtain nano SiO with different shapes2The microspheres are subjected to hydrothermal reaction at 140 ℃ for 6 hours and room temperature coprecipitation to obtain SiO2/Ag2The S powder has the best composite effect.
Description
Technical Field
The invention relates to the technical field of preparation of composite photocatalysts, in particular to SiO2/Ag2A preparation method of S composite powder.
Background
Silver sulfide (Ag)2S) is a common photocatalyst, in contrast to TiO2Iso-traditional photocatalytic materials, Ag2S has a narrow energy band gap (about 0.92 ev), so that the absorption range of visible light can be effectively expanded, the utilization efficiency of the visible light is improved, and the S has wide application in the aspects of removal of heavy metals and organic dyes, purification of wastewater and the like due to the outstanding optical performance.
Nano SiO2Because of its good biocompatibility, optical transparency, chemical stability, non-toxicity and easy preparation, etc., it is often used as matrix and template of composite material, and at the same time, SiO2As an inert carrier, it can effectively block Ag2And (4) agglomeration of S nano particles. However, the nano SiO prepared by the traditional stober method2The particle size distribution of the microspheres is not uniform, and submicron SiO with the particle size of 0.05-2 mu m is generally obtained2And (3) microspheres. With respect to SiO2With Ag2The reports and articles for compounding S nano materials are few, and the invention focuses on discussing SiO2With Ag2The composite process of S nanometer particle provides one kind of photocatalyst and sewage purifying agent with simple process, low cost and excellent performance.
Disclosure of Invention
In order to overcome the technical problems in the prior art, the invention aims to provide SiO2/Ag2The preparation method of the S composite powder has simple and convenient process and low cost, and can prepare the photocatalyst and the sewage purifying agent with excellent performance.
To achieve the purpose, the invention adoptsThe following technical scheme is used: SiO (silicon dioxide)2/Ag2The preparation method of the S composite powder comprises the following specific steps:
1) nano SiO2Preparation of microspheres
Firstly, respectively and uniformly mixing 50mL of absolute ethyl alcohol and 15mL of deionized water in a beaker, then adding a morphology control agent and 0-4 mL of polyacrylate emulsion into the beaker, stirring and uniformly mixing the mixture by using a constant-temperature magnetic stirrer, then slowly dropwise adding 3mL of Tetraethoxysilane (TEOS) into the mixed solution, heating the mixed solution to react after the dropwise adding is finished, and continuously stirring the mixed solution for a period of time to obtain SiO2A colloidal solution;
2)、SiO2/Ag2preparation of S composite powder
50mL of 0.005mol/L AgNO3Dropwise adding the solution into 25mL of thiourea aqueous solution of 0.01mol/L by a micropipette to form thiourea silver complex, uniformly stirring, and dropwise adding 12mL of SiO prepared in the step 1) into the thiourea silver complex solution2Reacting the colloidal solution at room temperature to generate black precipitate, repeatedly washing with deionized water and absolute ethyl alcohol for multiple times, filtering, and drying to obtain SiO2/Ag2S composite powder.
SiO as an object of the present invention2/Ag2The preferable technical scheme of the preparation method of the S composite powder comprises the following steps:
stirring for 10min by using a constant-temperature magnetic stirrer in the step 1). After the dropwise addition, the temperature is raised to 140 ℃ for reaction, and when the solution begins to turn to milk white, the solution is continuously stirred for 6 hours to obtain SiO2A colloidal solution. The drying temperature in the step 2) is 160 ℃.
SiO as an object of the present invention2/Ag2The preferable technical scheme of the S composite powder preparation method is that the morphology control agent in the step 1) is a sodium carbonate solution, the concentration is 0.04mol/L, the addition amount is 10mL, and the addition mode is dropwise addition.
SiO as an object of the present invention2/Ag2In another preferable technical scheme of the S composite powder preparation method, the morphology control agent in the step 1) is ammonia water, the concentration of the ammonia water is 25%, the addition amount of the ammonia water is 5mL, and the ammonia water is addedThe addition mode is one-time addition.
Compared with the prior art, the invention has the beneficial effects that:
1) the invention researches the nano SiO with uniform particle size distribution by changing the type of the control agent2The preparation method of the microsphere can prepare SiO with good monodispersity and uniformity of particle size distribution2Micro-spheres, and mixing Ag2S nano-particles are loaded on SiO2Preparation of SiO on the surface of microspheres2/Ag2S composite powder. Preparation of SiO by coprecipitation at room temperature2/Ag2The S powder has the advantages of simple and convenient operation, easily controlled reaction conditions, good composite effect and the like.
2) SiO of the present invention2/Ag2The preparation method of the S composite powder can reduce the nano SiO to a certain extent by adding a proper amount of polyacrylate emulsion2The particle size of the microspheres can be controlled by adding different shape control agents to obtain nano SiO with different shapes2The microspheres are subjected to hydrothermal reaction at 140 ℃ for 6 hours and room temperature coprecipitation to obtain SiO2/Ag2The S powder has the best composite effect.
Drawings
FIG. 1 is a graph of polyacrylate emulsion dosage versus SiO generation2Influence of particle size, a, b and c respectively correspond to three groups of experiments of 0, 1mL and 4mL of the addition amount of the polyacrylate emulsion to prepare SiO2SEM image of (a), d shows three experimental preparations of SiO2Average particle size distribution diagram of (a).
FIG. 2 is a SiO solid prepared without polyacrylate emulsion and with 4mL polyacrylate emulsion2XRD spectrum of the microspheres.
FIG. 3 is SiO prepared in example 12/Ag2XRD spectrogram of S powder.
FIG. 4 is SiO prepared in example 12/Ag2SEM image of S powder.
FIG. 5 shows the effect of reaction temperature on the morphology and complexing effect of the complexed product (a, b, c correspond to 140 ℃, 160 ℃, 180 ℃ respectively) and the chemical composition of the product (d).
FIG. 6 is NaCO3The solution is used as a control agentTo SiO2Influence of morphology (a, b are respectively corresponding to dropwise adding in steps and adding Na in one time2CO3Solution prepared SiO2SEM pictures of microspheres).
Detailed Description
The SiO of the present invention is described in further detail below with reference to specific examples2/Ag2A preparation method of S composite powder. The product was characterized by an X-ray diffractometer (XRD), a scanning electron microscope (SEM, SU-8010), particle size distribution calculation software (NanoMersure), and the like, respectively.
Example 1
SiO (silicon dioxide)2/Ag2The preparation method of the S composite powder comprises the following specific steps:
1) nano SiO2Preparation of microspheres
Firstly, respectively and uniformly mixing 50mL of absolute ethyl alcohol and 15mL of deionized water in a beaker, then adding 5mL of 25% ammonia water and polyacrylate emulsion (three groups of experiments of 0, 1mL and 4 mL) into the beaker, stirring for 10min by using a constant-temperature magnetic stirrer, uniformly mixing, then slowly dropwise adding 3mL of Tetraethoxysilane (TEOS) into the mixed solution, heating to 140 ℃ after dropwise adding, reacting, and continuously stirring for 6h to obtain SiO when the solution begins to turn to be milky white2A colloidal solution.
The solvent system can affect the particle size of the powder particles to a certain extent. Obtaining nano SiO prepared by adding different amounts of polyacrylate emulsion through scanning electron microscope microscopic analysis2. FIG. 1 is a graph of polyacrylate emulsion dosage versus SiO generation2Influence of particle size, a, b and c respectively correspond to three groups of experiments of 0, 1mL and 4mL of the addition amount of the polyacrylate emulsion to prepare SiO2SEM image of (a), d shows three experimental preparations of SiO2Average particle size distribution diagram of (a).
Can obtain nano SiO with good monodispersity and particle size distribution uniformity when no polyacrylate emulsion is added2Microspheres (see fig. 1 a). With the increase of polyacrylate emulsion, the prepared nano SiO2Is not changed, but SiO2The particle size of the microspheres is gradually reduced (see fig. 1b and c), and the particle size is determined by the particle size systemThe analysis revealed that SiO was obtained when 1mL of polyacrylate emulsion was added and 4mL of polyacrylate emulsion was added without addition of polyacrylate emulsion2Respectively, 242.60nm, 225.51nm and 218.98nm (see FIG. 1 d). Mainly because of SiO2The particle size of the SiO solid solution can increase along with the increase of the viscosity of the solvent in different solvent systems, and the viscosity of the solvent can influence the SiO solid solution2Rate and diffusion of microsphere nucleation. The polyacrylate has strong adhesiveness and high viscosity at room temperature, so that SiO is limited to a certain extent2Nucleation of microspheres.
In addition, SiO prepared by adding no polyacrylate emulsion and 4mL polyacrylate emulsion respectively2The microspheres are subjected to characterization tests of XRD, and XRD spectrums between diffraction angles 2 theta and diffraction peak intensities I are drawn as shown in figure 2. From the figure, SiO can be seen2Has obvious characteristic absorption peak at 2 theta 23.5 degrees, and the intensity of the absorption peak is gradually reduced along with the gradual increase of 2 theta, and SiO of the emulsion is not added2The absorption intensity of diffraction peak is higher than that of SiO prepared by adding 4mL of polyacrylate emulsion2Absorption intensity of powder diffraction peak, which indicates SiO prepared without adding emulsion2The crystallinity of (a) is higher.
2)、SiO2/Ag2Preparation of S composite powder
50mL of 0.005mol/L AgNO3Dropwise adding the solution into 25mL of thiourea aqueous solution of 0.01mol/L by a micropipette to form thiourea silver complex, uniformly stirring, and dropwise adding 12mL of SiO prepared in the step 1) into the thiourea silver complex solution2Reacting the colloidal solution at room temperature to generate black precipitate, repeatedly washing with deionized water and absolute ethyl alcohol for multiple times, filtering, and drying at 160 ℃ to obtain SiO2/Ag2S composite powder.
SiO prepared in example 12/Ag2The XRD spectrum of the S powder is shown in figure 3, from which the spectrum of the composite product and SiO can be seen2Standard Spectrum (PDF #43-0745) and Ag2The standard peaks of the S standard spectrum (PDF #14-0072) are identical, and the compound product SiO is known2/Ag2The S powder has good crystallinityAnd has high purity and no unnecessary impurities.
SiO prepared in example 12/Ag2The SEM image of the S powder is shown in FIG. 4, from which it can be seen that Ag is used as the composite product2S chain-like particles as a matrix, by SiO2Coating the microspheres on Ag2S particle surface of Ag2The surface of S chain particles is basically coated with nano SiO2And (4) covering the microspheres.
Example 2
The specific steps are the same as example 1, except that the hydrothermal reaction temperature in step 1) is adjusted to 160 ℃ and 180 ℃.
FIG. 5 shows the effect of reaction temperature on the morphology and complexing effect of the complexed product (a, b, c correspond to 140 ℃, 160 ℃, 180 ℃ respectively) and the chemical composition of the product (d). It can be seen from the figure that the binding degree of the composite product obtained by hydrothermal treatment at 140 ℃ for 6h is the highest (see inset in fig. 5 a), and the binding degree of the composite product obtained by hydrothermal treatment at 160 ℃ and 180 ℃ respectively is gradually reduced under the same experimental conditions (see inset in fig. 5b and 5 c). The energy spectrum analysis (see fig. 5d) is carried out on the composite product after the hydrothermal treatment at 140 ℃, and the main element composition of the composite product is Si, O, S and Ag, wherein the Si element content is the highest, which is consistent with the phase analysis of XRD.
Example 3
Selecting sodium carbonate solution as a morphology control agent, and inspecting the generated SiO2Influence of topography
Firstly, respectively and uniformly mixing 50mL of absolute ethyl alcohol and 15mL of deionized water in a beaker, then adding 10mL of sodium carbonate solution with the concentration of 0.04mol/L into the beaker (step-by-step addition and one-time addition of two groups of experiments), stirring for 10min by using a constant-temperature magnetic stirrer, uniformly mixing, then slowly dropwise adding 3mL of Tetraethoxysilane (TEOS) into the mixed solution, heating to 140 ℃ after dropwise adding is finished, reacting, and continuously stirring for 6h to obtain SiO when the solution begins to turn to milk white2A colloidal solution.
Can be applied to the nano SiO by changing the kind and the adding mode of the control agent2The morphology and particle size of (a) have a great influence. FIG. 6a is a step-wise addition of Na2CO3Solution prepared SiO2SEM picture of the microspheres, SiO can be observed2The particle size of the microspheres is larger than that of SiO prepared by ammonia water2The microspheres are larger, but the dispersity is not as good as that of the ammonia water for preparing SiO2Good results are obtained. FIG. 6b shows the addition of Na in one portion2CO3Solution prepared SiO2SEM pictures of the microspheres, the SiO similar to dendritic shape can be obviously observed2Exists and SiO exists simultaneously2And (3) microspheres.
It should be noted that the present invention is not limited to the above-mentioned embodiments, and all the related technologies that can be directly derived or suggested from the present disclosure should fall within the protection scope of the present invention.
Claims (6)
1. SiO (silicon dioxide)2/Ag2The preparation method of the S composite powder is characterized by comprising the following steps: the method comprises the following specific steps:
1) nano SiO2Preparation of microspheres
Firstly, respectively and uniformly mixing 50mL of absolute ethyl alcohol and 15mL of deionized water in a beaker, then adding a morphology control agent and 0-4 mL of polyacrylate emulsion into the beaker, stirring and uniformly mixing the mixture by using a constant-temperature magnetic stirrer, then slowly dropwise adding 3mL of Tetraethoxysilane (TEOS) into the mixed solution, heating the mixed solution to react after the dropwise adding is finished, and continuously stirring the mixed solution for a period of time to obtain SiO2A colloidal solution;
2)、SiO2/Ag2preparation of S composite powder
50mL of 0.005mol/L AgNO3Dropwise adding the solution into 25mL of thiourea aqueous solution of 0.01mol/L by a micropipette to form thiourea silver complex, uniformly stirring, and dropwise adding 12mL of SiO prepared in the step 1) into the thiourea silver complex solution2Reacting the colloidal solution at room temperature to generate black precipitate, repeatedly washing with deionized water and absolute ethyl alcohol for multiple times, filtering, and drying to obtain SiO2/Ag2S composite powder.
2. The method of claim 1, wherein: stirring for 10min by using a constant-temperature magnetic stirrer in the step 1).
3. The method of claim 1, wherein: after the dropwise addition is finished in the step 1), heating to 140 ℃ for reaction, and continuously stirring for 6 hours to obtain SiO when the solution begins to become milky white2A colloidal solution.
4. The method of claim 1, 2 or 3, wherein: the morphology control agent in the step 1) is a sodium carbonate solution, the concentration is 0.04mol/L, the addition amount is 10mL, and the addition mode is dropwise addition.
5. The method of claim 1, 2 or 3, wherein: in the step 1), the morphology control agent is ammonia water, the concentration of the ammonia water is 25%, the addition amount of the ammonia water is 5mL, and the addition mode is one-time addition.
6. The method of claim 1, wherein: the drying temperature in the step 2) is 160 ℃.
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Citations (5)
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