CN116237062A - Method for preparing porous indium cadmium sulfide based on ultrasonic atomization - Google Patents
Method for preparing porous indium cadmium sulfide based on ultrasonic atomization Download PDFInfo
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- 238000000889 atomisation Methods 0.000 title claims abstract description 22
- UFEHSYWUPMDJLU-UHFFFAOYSA-N cadmium(2+) indium(3+) sulfide Chemical compound [S-2].[Cd+2].[In+3] UFEHSYWUPMDJLU-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 title claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 31
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000005406 washing Methods 0.000 claims abstract description 16
- 239000000843 powder Substances 0.000 claims abstract description 13
- 239000002243 precursor Substances 0.000 claims abstract description 13
- 238000001035 drying Methods 0.000 claims abstract description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 9
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 8
- AUIZLSZEDUYGDE-UHFFFAOYSA-L cadmium(2+);diacetate;dihydrate Chemical compound O.O.[Cd+2].CC([O-])=O.CC([O-])=O AUIZLSZEDUYGDE-UHFFFAOYSA-L 0.000 claims abstract description 8
- 238000005530 etching Methods 0.000 claims abstract description 8
- UKCIUOYPDVLQFW-UHFFFAOYSA-K indium(3+);trichloride;tetrahydrate Chemical compound O.O.O.O.Cl[In](Cl)Cl UKCIUOYPDVLQFW-UHFFFAOYSA-K 0.000 claims abstract description 8
- 239000007788 liquid Substances 0.000 claims abstract description 7
- 239000000741 silica gel Substances 0.000 claims abstract description 7
- 229910002027 silica gel Inorganic materials 0.000 claims abstract description 7
- 238000000227 grinding Methods 0.000 claims abstract description 6
- 238000003756 stirring Methods 0.000 claims abstract description 6
- 238000000926 separation method Methods 0.000 claims abstract description 3
- 239000000203 mixture Substances 0.000 claims abstract 5
- 239000012153 distilled water Substances 0.000 claims description 25
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 11
- 238000011068 loading method Methods 0.000 claims description 5
- 230000001699 photocatalysis Effects 0.000 abstract description 8
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 abstract description 5
- 229940012189 methyl orange Drugs 0.000 abstract description 5
- 239000004005 microsphere Substances 0.000 abstract description 4
- 230000031700 light absorption Effects 0.000 abstract description 3
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 3
- 230000000593 degrading effect Effects 0.000 abstract description 2
- 238000002474 experimental method Methods 0.000 abstract description 2
- 239000002086 nanomaterial Substances 0.000 description 6
- 239000011941 photocatalyst Substances 0.000 description 5
- 230000015556 catabolic process Effects 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000001048 orange dye Substances 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- STZCRXQWRGQSJD-UHFFFAOYSA-M sodium;4-[[4-(dimethylamino)phenyl]diazenyl]benzenesulfonate Chemical compound [Na+].C1=CC(N(C)C)=CC=C1N=NC1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-UHFFFAOYSA-M 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 2
- FCNBPGQGSGENIO-UHFFFAOYSA-N cadmium;sulfanylideneindium Chemical compound [Cd].[In]=S FCNBPGQGSGENIO-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- 150000004763 sulfides Chemical class 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 239000000443 aerosol Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 150000004770 chalcogenides Chemical class 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012761 high-performance material Substances 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 238000004088 simulation Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 150000003464 sulfur compounds Chemical class 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
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- 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
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- 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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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/0009—Use of binding agents; Moulding; Pressing; Powdering; Granulating; Addition of materials ameliorating the mechanical properties of the product catalyst
- B01J37/0018—Addition of a binding agent or of material, later completely removed among others as result of heat treatment, leaching or washing,(e.g. forming of pores; protective layer, desintegrating by heat)
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/341—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation
- B01J37/343—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation making use of electric or magnetic fields, wave energy or particle radiation of ultrasonic wave energy
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Abstract
The invention discloses a method for preparing porous indium cadmium sulfide based on ultrasonic atomization, which comprises the following steps: 1) Adding cadmium acetate dihydrate, indium chloride tetrahydrate and thiourea into water, stirring to dissolve completely, and adding a silica gel solution into the mixture to form a precursor solution; 2) Atomizing the precursor solution by using an ultrasonic atomizer to form small liquid dropsLoading the mixture into a tubular furnace by air to react at 500-600 ℃, collecting the obtained product by using water, centrifugally separating, washing, drying and grinding to obtain powder; 3) And (3) putting the powder into HF for etching, then carrying out centrifugal separation on the product, washing and drying to obtain the porous indium cadmium sulfide. CdIn synthesized by the invention 2 S 4 The microsphere has the energy band structure, light absorption characteristic and porosity related to the components, can efficiently degrade organic pollutants in water, and shows good photocatalytic activity in experiments for degrading organic dye methyl orange.
Description
Technical Field
The invention relates to the field of photocatalytic materials, in particular to a method for preparing porous indium cadmium sulfide based on ultrasonic atomization.
Background
The functional semiconductor nano material has excellent physical and chemical properties and wide application prospect in the fields of electricity, photoelectricity, photochemistry and the like, so that the controllable preparation, characterization and application of the functional semiconductor nano material are of great interest. The band structure of semiconductor nanomaterials is an important parameter for their application, and particularly in the field of photocatalysis, considerable attention has been paid. Among the various novel photocatalysts, ternary sulfides are attracting attention due to the instability of binary sulfides. Ternary metal chalcogenides have narrower band gap widths, higher visible light absorption capacity, and more excellent light stability and photoelectric properties, and are therefore favored by students at home and abroad. Cadmium indium sulfide (CdIn) 2 S 4 ) Belonging to the sulfur compound AB 2 X 4 Is considered to have a profound application prospect in the aspects of optical devices, solar cells, photocatalytic hydrogen production, photocatalytic sterilization and organic pollutant elimination. Taking into account the advantages of nanostructures over bulk materials, attempts have been made to synthesize Cd In with various nanostructures 2 S 4 。
To date, the preparation of CdIn is commonly used 2 S 4 The method comprises the following steps: chemical precipitation, hydrothermal, solvothermal, chemical reduction, and the like. However, these conventional synthetic methods generally require severe conditions such as high temperature, high pressure, toxic reagents, or complicated equipment. Furthermore, they are mostly not available for continuous manufacturing, limiting their use in mass and large-scale industrial production. It follows that a continuous synthesis of CdIn with specific nanostructure and high yield must be developed 2 S 4 To improve the applicability of various high performance materials.
Disclosure of Invention
The invention aims to provide a method for preparing porous indium cadmium sulfide based on ultrasonic atomization.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
a method for preparing porous indium cadmium sulfide based on ultrasonic atomization comprises the following steps:
1) Adding cadmium acetate dihydrate, indium chloride tetrahydrate and thiourea into 100-120 mL of distilled water according to a proportion, placing the distilled water on a magnetic stirrer for vigorous stirring to completely dissolve the distilled water, and adding 1.0-2.5 mL of silica gel solution into the distilled water to form colorless and transparent precursor solution;
2) Atomizing the precursor solution by utilizing an ultrasonic atomizer, loading small liquid drops formed by atomization into a tubular furnace to react at 500-600 ℃, collecting the obtained product by using distilled water, centrifugally separating, washing, placing the product into a 60 ℃ oven, drying for 10-12 hours, and grinding to obtain powder;
3) And (3) putting the ground powder into HF for etching, then carrying out centrifugal separation on the product, washing with distilled water and absolute ethyl alcohol, and drying to obtain the porous indium cadmium sulfide.
In the step 1), the molar ratio of the cadmium acetate dihydrate to the indium chloride tetrahydrate to the thiourea is 1.0-1.5:2.0-3.0:8.0-10.0.
In the step 2), the washing is carried out by adopting distilled water for 2 times and absolute ethyl alcohol for 1 time.
In the step 3), the concentration of the HF is 5-10%.
In the step 3), the etching time is 10-15 minutes.
In the step 3), the washing is sequentially performed by distilled water and absolute ethyl alcohol.
The invention takes silica gel as a template and forms CdIn in a tube furnace by utilizing an ultrasonic atomization method 2 S 4 The ultrasonic atomization technology mainly utilizes ultrasonic energy to break precursor solution mixed according to a certain proportion into micron-sized droplets to form aerosol; the small liquid drops are transported into a high-temperature reverse tube furnace chamber by using nitrogen as carrier gas, and the solvent is evaporated and the solute is concentrated under the high-temperature conditionThe CdIn is obtained in the crystallization reaction and other stages 2 S 4 Powder particles; then removing the template silicon dioxide by using an HF etching method, thereby obtaining the ternary sulfide photocatalyst CdIn with hollow microsphere appearance 2 S 4 。
CdIn synthesized by the invention 2 S 4 The microsphere has the energy band structure, light absorption characteristic and porosity related to the components, can efficiently degrade organic pollutants in water, and shows good photocatalytic activity in experiments for degrading organic dye methyl orange.
Drawings
FIG. 1 shows the CdIn synthesized in example 1 2 S 4 Is an X-ray powder diffraction pattern of (c).
FIG. 2 shows the CdIn synthesized in example 1 2 S 4 Microstructure architecture.
Detailed Description
Example 1
A method for preparing porous indium cadmium sulfide based on ultrasonic atomization comprises the following steps:
1) Adding 0.532 g cadmium acetate dihydrate, 1.2 g indium chloride tetrahydrate and 0.78 g thiourea into 100 mL distilled water, putting the distilled water on a magnetic stirrer, vigorously stirring to completely dissolve the distilled water, and adding 1.0 mL silica gel solution into the distilled water to form colorless transparent precursor solution;
2) Atomizing the precursor solution by utilizing an ultrasonic atomizer, loading small liquid drops formed by atomization into a tubular furnace to react at 600 ℃, collecting the obtained product by using distilled water, centrifugally separating the obtained product, washing the product by using distilled water for 2 times and absolute ethyl alcohol for 1 time, placing the product into a 60 ℃ oven, drying 12 h, and grinding to obtain powder;
3) And (3) putting the ground powder into HF with the concentration of 8% to etch for 15 minutes, centrifuging the product, washing with distilled water and absolute ethyl alcohol, and drying to obtain the porous indium cadmium sulfide.
Example 2
A method for preparing porous indium cadmium sulfide based on ultrasonic atomization comprises the following steps:
1) Cadmium acetate dihydrate, indium chloride tetrahydrate and thiourea are added into 110mL of distilled water according to the mol ratio of 1.2:2.5:9, and are placed on a magnetic stirrer for vigorous stirring to be completely dissolved, and 2.0mL of silica gel solution is taken and added into the solution to form colorless and transparent precursor solution;
2) Atomizing the precursor solution by utilizing an ultrasonic atomizer, loading small liquid drops formed by atomization into a tubular furnace to react at 550 ℃, collecting the obtained product by using distilled water, centrifugally separating the obtained product, washing the obtained product by using distilled water for 2 times and absolute ethyl alcohol for 1 time, then placing the product into a 60 ℃ oven, drying for 10 hours, and grinding to obtain powder;
3) And (3) putting the ground powder into HF with the concentration of 5% to etch for 12 minutes, centrifuging the product, washing with distilled water and absolute ethyl alcohol, and drying to obtain the porous indium cadmium sulfide.
Example 3
A method for preparing porous indium cadmium sulfide based on ultrasonic atomization comprises the following steps:
1) Cadmium acetate dihydrate, indium chloride tetrahydrate and thiourea are added into 120mL of distilled water according to the molar ratio of 1.5:3:10, and are placed on a magnetic stirrer for vigorous stirring to be completely dissolved, and 2.5mL of silica gel solution is taken and added into the solution to form colorless and transparent precursor solution;
2) Atomizing the precursor solution by utilizing an ultrasonic atomizer, loading small liquid drops formed by atomization into a tubular furnace to react at 600 ℃, collecting the obtained product by using distilled water, centrifugally separating the obtained product, washing the obtained product by using distilled water for 2 times and absolute ethyl alcohol for 1 time, then placing the product into a 60 ℃ oven, drying for 11 hours, and grinding to obtain powder;
3) Etching the ground powder in 10% HF for 10 min, centrifuging, washing with distilled water and absolute ethanol, and oven drying to obtain porous indium cadmium sulfide
Example 4
Porous cadmium indium sulfide (CdIn) 2 S 4 ) Photocatalytic Properties of microspheres
Dyeing with methyl orangeMaterial model, cdIn prepared in example 1 was evaluated by taking degradation rate of methyl orange dye as index 2 S 4 Photocatalytic activity index of the photocatalyst sample.
The results showed that (1) the methyl orange solution was hardly discolored in the absence of light with photocatalyst alone, indicating CdIn 2 S 4 The material itself had no degradation to the methyl orange solution.
(2) The slight change in methyl orange dye under light and no catalyst conditions was primarily a simulation of the effect of the light source.
(3) All samples are stirred for 45 min in the absence of illumination, so that the inside of the solution reaches adsorption degradation balance, and then a xenon lamp is used for simulating a natural light source to perform activity test. The color of the methyl orange solution was clearly seen to change after the addition of the photocatalyst. CdIn obtained after HF etching for 15 minutes 2 S 4 The photocatalytic degradation rate of the sample to the methyl orange dye reaches 95.6% in 120 minutes.
Claims (6)
1. The method for preparing the porous indium cadmium sulfide based on ultrasonic atomization is characterized by comprising the following steps of:
1) Adding cadmium acetate dihydrate, indium chloride tetrahydrate and thiourea into water according to a certain proportion, and placing the mixture on a magnetic stirrer for vigorous stirring to completely dissolve the mixture, and adding a silica gel solution into the mixture to form a colorless transparent precursor solution;
2) Atomizing the precursor solution by utilizing an ultrasonic atomizer, loading small liquid drops formed by atomization into a tubular furnace to react at 500-600 ℃ by air, collecting the obtained product by water, centrifugally separating, washing, drying and grinding the product to obtain powder;
3) And (3) putting the ground powder into HF for etching, then carrying out centrifugal separation on the product, washing and drying to obtain the porous indium cadmium sulfide.
2. The method for preparing porous indium cadmium sulfide based on ultrasonic atomization according to claim 1, wherein in the step 1), the molar ratio of the cadmium acetate dihydrate to the indium chloride tetrahydrate to the thiourea is 1.0-1.5:2.0-3.0:8.0-10.0.
3. The method for preparing porous indium cadmium sulfide based on ultrasonic atomization according to claim 1, wherein in the step 2), the washing is carried out 2 times by using distilled water and 1 time by using absolute ethyl alcohol.
4. The method for preparing porous indium cadmium sulfide based on ultrasonic atomization according to claim 1, wherein in the step 3), the concentration of HF is 5-10%.
5. The method for preparing porous indium cadmium sulfide based on ultrasonic atomization according to claim 1, wherein in the step 3), the etching time is 10-15 minutes.
6. The method for preparing porous indium cadmium sulfide based on ultrasonic atomization according to claim 1, wherein in the step 3), the washing is sequentially performed by distilled water and absolute ethyl alcohol.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009149540A1 (en) * | 2008-06-10 | 2009-12-17 | National Research Council Of Canada | Controllable synthesis of porous carbon spheres, and electrochemical applications thereof |
| CN103894211A (en) * | 2014-04-09 | 2014-07-02 | 莆田学院 | Multi-metal sulfide semiconductor photocatalytic material and preparation method thereof |
| CN105771957A (en) * | 2016-03-22 | 2016-07-20 | 中国科学院地球环境研究所 | Bismuth niobate porous microspheres with photocatalytic activity and ultrasonic atomizing preparation method thereof |
| CN110694603A (en) * | 2019-09-07 | 2020-01-17 | 苏州羿白环保科技有限公司 | Preparation method of novel porous structure photocatalyst |
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