CN108325543B - Synthetic method of activated carbon-loaded petal-shaped silver phosphate complex-phase photocatalytic material - Google Patents
Synthetic method of activated carbon-loaded petal-shaped silver phosphate complex-phase photocatalytic material Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 119
- 229910000161 silver phosphate Inorganic materials 0.000 title claims abstract description 47
- 229940019931 silver phosphate Drugs 0.000 title claims abstract description 44
- FJOLTQXXWSRAIX-UHFFFAOYSA-K silver phosphate Chemical compound [Ag+].[Ag+].[Ag+].[O-]P([O-])([O-])=O FJOLTQXXWSRAIX-UHFFFAOYSA-K 0.000 title claims abstract description 41
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 29
- 239000000463 material Substances 0.000 title claims abstract description 24
- 238000010189 synthetic method Methods 0.000 title claims description 3
- 238000005507 spraying Methods 0.000 claims abstract description 32
- 230000010355 oscillation Effects 0.000 claims abstract description 29
- 238000001035 drying Methods 0.000 claims abstract description 26
- 238000000034 method Methods 0.000 claims abstract description 21
- 229910019142 PO4 Inorganic materials 0.000 claims abstract description 12
- 238000004140 cleaning Methods 0.000 claims abstract description 9
- 230000002194 synthesizing effect Effects 0.000 claims abstract description 7
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 11
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 238000005303 weighing Methods 0.000 claims description 9
- 230000003213 activating effect Effects 0.000 claims description 8
- 238000001354 calcination Methods 0.000 claims description 8
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(I) nitrate Inorganic materials [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 8
- 238000007664 blowing Methods 0.000 claims description 2
- 238000011068 loading method Methods 0.000 claims description 2
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 2
- 238000001291 vacuum drying Methods 0.000 claims description 2
- 239000002131 composite material Substances 0.000 claims 1
- 101710134784 Agnoprotein Proteins 0.000 abstract description 11
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 5
- 239000000843 powder Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 31
- 239000011941 photocatalyst Substances 0.000 description 18
- 238000002360 preparation method Methods 0.000 description 8
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 6
- 238000007605 air drying Methods 0.000 description 6
- HPTYUNKZVDYXLP-UHFFFAOYSA-N aluminum;trihydroxy(trihydroxysilyloxy)silane;hydrate Chemical compound O.[Al].[Al].O[Si](O)(O)O[Si](O)(O)O HPTYUNKZVDYXLP-UHFFFAOYSA-N 0.000 description 6
- 238000000861 blow drying Methods 0.000 description 6
- 229910052621 halloysite Inorganic materials 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 4
- 239000011521 glass Substances 0.000 description 4
- 229910052588 hydroxylapatite Inorganic materials 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- XYJRXVWERLGGKC-UHFFFAOYSA-D pentacalcium;hydroxide;triphosphate Chemical compound [OH-].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O XYJRXVWERLGGKC-UHFFFAOYSA-D 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 239000003054 catalyst Substances 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000004408 titanium dioxide Substances 0.000 description 3
- ISAKRJDGNUQOIC-UHFFFAOYSA-N Uracil Chemical compound O=C1C=CNC(=O)N1 ISAKRJDGNUQOIC-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 230000000593 degrading effect Effects 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 230000001376 precipitating effect Effects 0.000 description 2
- 239000000376 reactant Substances 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 229910001961 silver nitrate Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 229910002915 BiVO4 Inorganic materials 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- QANIADJLTJYOFI-UHFFFAOYSA-K aluminum;magnesium;carbonate;hydroxide;hydrate Chemical compound O.[OH-].[Mg+2].[Al+3].[O-]C([O-])=O QANIADJLTJYOFI-UHFFFAOYSA-K 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 239000003574 free electron Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
- 238000000520 microinjection Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 229910000403 monosodium phosphate Inorganic materials 0.000 description 1
- 235000019799 monosodium phosphate Nutrition 0.000 description 1
- 238000000643 oven drying Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000013032 photocatalytic reaction Methods 0.000 description 1
- 229940113115 polyethylene glycol 200 Drugs 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 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 1
- 229940043267 rhodamine b Drugs 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- CQLFBEKRDQMJLZ-UHFFFAOYSA-M silver acetate Chemical compound [Ag+].CC([O-])=O CQLFBEKRDQMJLZ-UHFFFAOYSA-M 0.000 description 1
- 229940071536 silver acetate Drugs 0.000 description 1
- HTRJDXQPCKIFIU-UHFFFAOYSA-N silver;ethanol;nitrate Chemical compound [Ag+].CCO.[O-][N+]([O-])=O HTRJDXQPCKIFIU-UHFFFAOYSA-N 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- AJPJDKMHJJGVTQ-UHFFFAOYSA-M sodium dihydrogen phosphate Chemical compound [Na+].OP(O)([O-])=O AJPJDKMHJJGVTQ-UHFFFAOYSA-M 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000007921 spray Substances 0.000 description 1
- 229940035893 uracil Drugs 0.000 description 1
- 238000003828 vacuum filtration Methods 0.000 description 1
Images
Classifications
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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
- B01J27/14—Phosphorus; Compounds thereof
- B01J27/16—Phosphorus; Compounds thereof containing oxygen, i.e. acids, anhydrides and their derivates with N, S, B or halogens without carriers or on carriers based on C, Si, Al or Zr; also salts of Si, Al and Zr
- B01J27/18—Phosphorus; Compounds thereof containing oxygen, i.e. acids, anhydrides and their derivates with N, S, B or halogens without carriers or on carriers based on C, Si, Al or Zr; also salts of Si, Al and Zr with metals other than Al or Zr
- B01J27/1802—Salts or mixtures of anhydrides with compounds of other metals than V, Nb, Ta, Cr, Mo, W, Mn, Tc, Re, e.g. phosphates, thiophosphates
- B01J27/1817—Salts or mixtures of anhydrides with compounds of other metals than V, Nb, Ta, Cr, Mo, W, Mn, Tc, Re, e.g. phosphates, thiophosphates with copper, silver or gold
-
- 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—
-
- B01J35/39—
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0201—Impregnation
- B01J37/0205—Impregnation in several steps
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0201—Impregnation
- B01J37/0207—Pretreatment of the support
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/0236—Drying, e.g. preparing a suspension, adding a soluble salt and drying
Abstract
The invention relates to a method for synthesizing an activated carbon-loaded petal-shaped silver phosphate complex-phase photocatalytic material, which is characterized by comprising the following steps of: placing the pretreated active carbon in a shaking table for oscillation, and alternately and uniformly spraying AgNO on the surface of the active carbon in the oscillation process3And H3PO4Repeatedly carrying out the solution for 5-20 times; and then taking out the activated carbon, cleaning and drying to obtain the activated carbon-loaded petal-shaped silver phosphate complex phase photocatalytic material. The heterogeneous material combines the huge specific surface area of the activated carbon and the excellent photocatalytic performance of the silver phosphate, has stronger organic pollutant treatment capacity, and is easier to recycle compared with silver phosphate powder.
Description
Technical Field
The invention relates to a method for synthesizing an activated carbon-loaded petal-shaped silver phosphate complex-phase photocatalytic material, belonging to the field of inorganic non-metallic materials.
Background
In the modern society, due to the high development of the traditional industry, the traditional fossil fuel is overused, on one hand, the traditional energy is exhausted, and on the other hand, serious pollution to the atmosphere and water is caused. Environmental pollution and conventional energy exhaustion have become the most important and urgent two problems to be solved in human society. In order to alleviate and solve the above problems, it is necessary to find new energy sources that are convenient to take, clean and have no environmental problems. The advent of photocatalytic technology has created a hope that the above problems will be solved, and it is expected that the healthy development of human society will be achieved.
The photocatalyst can absorb light energy, generate free electrons and holes, react to form active species, and further react with reactants, so that conversion of the light energy to chemical energy is realized. The research of Japanese scientists leads to find that the titanium dioxide has the functions of decomposing water and degrading organic pollutants in a photocatalytic way. Although titanium dioxide has the characteristics of high catalytic activity, good chemical stability and the like, and has a certain application at present, the development of titanium dioxide is limited by the disadvantages of absorption only in an ultraviolet region, low quantum efficiency and the like.
The research in the field of photocatalysis gradually shifts to visible light catalytic materials, and researchers find CdS and BiVO4、C3N4、Ag3PO4The photocatalyst with the narrow band gap has a wide absorption range and can be excited by visible light. Wherein Ag is3PO4The photocatalyst can absorb sunlight with the wavelength less than 520nm, shows extremely superior photocatalytic activity in degradation experiments of various organic dyes, and has considerable capability of decomposing water and producing oxygen.
The activated carbon is an adsorbent, has huge specific surface area and strong adsorption capacity, and can adsorb organic pollutants in liquid or gas. Ag3PO4After being compounded with the active carbon, not only the Ag is improved3PO4Self-dispersibility and huge surface area enables organic pollutants to be mixed with Ag3PO4The contact is more sufficient, thereby promoting the progress of the photocatalytic reaction.
Patent application No. 201310246213.8 reports a preparation method of a silver phosphate photocatalyst, which comprises the following steps: adding silver acetate and phosphoric acid aqueous solution into polyethylene glycol 200 in sequence, adjusting the pH to 5-6, and reacting under stirring; and after the reaction is finished, centrifuging to obtain a precipitate, washing and drying to obtain the silver phosphate photocatalyst. The silver phosphate photocatalyst obtained by the method is a novel tubular microporous structure and has higher photocatalytic activity. The patent with the application number of 201210341324.2 reports a preparation method of a visible light driven nano silver phosphate catalyst, and the invention prepares the nano silver phosphate photocatalyst which can exist stably by using different light sources for irradiation and microinjection of reactants, thereby avoiding the problem that the product can be decomposed when the nano silver phosphate photocatalyst is prepared under visible light. The silver phosphate particles prepared by the method are of a ball cluster structure, the diameter of a monomer is 20-60 nm, the overall diameter is 60-300 n, and the particle size is far smaller than that of common micron-sized silver phosphate in the market. However, the above cases are different from the present application in that they are all the preparation methods of pure silver phosphate.
The patent with application number 201410001356.7 reports a preparation method of a exfoliated hydrotalcite-supported silver phosphate catalyst, which comprises the following specific steps: dissolving uracil in NaOH solution, adding silver nitrate, stirring until the solution is clear and transparent, adding dried commercially available or self-made hydrotalcite powder, stirring, precipitating, separating, and oven drying; placing the dried product in a microwave oven, and performing microwave irradiation; and adding the product subjected to microwave irradiation into a phosphoric acid solution, stirring, precipitating, separating and drying to obtain the exfoliated hydrotalcite-supported silver phosphate catalyst. A preparation method of a halloysite-loaded silver phosphate photocatalyst is reported in a patent with the application number of 201410156228.X, and comprises the following specific steps: adding halloysite into a nitric acid solution to obtain acid-treated halloysite, placing 4-8 g of acid-treated halloysite into a vacuum filtration bottle, mixing with a silver nitrate ethanol solution in a vacuum state, allowing silver nitrate to fully enter a halloysite tube, continuously stirring for 2-3 h, performing solid-liquid separation, and drying at 70-80 ℃ in vacuum; and adding the dried product into 50mL of sodium dihydrogen phosphate solution with the concentration of 0.5-1.5 mol/L, stirring for 4-5 h, carrying out solid-liquid separation, washing, and drying at 100-105 ℃ to obtain the halloysite-loaded silver phosphate photocatalyst. The patent with the application number 201410259216.X reports a preparation method of a supported silver phosphate photocatalyst, and the preparation method comprises the following specific steps: weighing 80-100 g of porous hydroxyapatite which is ground and then sieved by a 40-mesh sieve, and filling the porous hydroxyapatite into a glass tube which is controlled by an upper valve and a lower valve; respectively preparing HNO with the concentration of 0.01-0.1 mol/L3Solution, NaNO with concentration of 0.01-0.1 mol/L3Solution and AgNO with concentration of 0.2-0.8 mol/L3200mL of each solution; the glass tube filled with the porous hydroxyapatite is erected, the upper valve and the lower valve are opened, and HNO is injected into the glass tube from the bottom3Solution, when the solution can submerge the porous hydroxyapatite, discharging HNO3Solution, keeping the bottom valve open, injecting NaNO from the top3Dissolving NaNO in a solvent3The solution flows out from the bottom after being injected from the top, then the bottom valve is closed, and AgNO is injected from the top3Soaking the solution for 20-30 min to obtain AgNO3And discharging the solution from the bottom, washing the particles in the glass tube by deionized water, and drying to obtain the supported silver phosphate photocatalyst. The above cases and the present application belong to the preparation of supported silver phosphate photocatalysts, but the sizes and appearances of the supported silver phosphate photocatalyst are completely different from those of the supported silver phosphate photocatalyst, the supported silver phosphate photocatalyst and the supported silver phosphate photocatalyst, and the final photocatalytic activities are also greatly different.
The application is different from the above reports, and the application repeatedly sprays AgNO on the surface of the activated carbon3Solution and H3PO4And (5) obtaining the activated carbon-loaded petal-shaped silver phosphate complex phase photocatalytic material through solution. The photocatalyst has wide application prospect in the fields of degrading organic pollutants and the like.
Disclosure of Invention
The invention mainly relates to a method for synthesizing an activated carbon-loaded petal-shaped silver phosphate complex-phase photocatalytic material, and specifically relates to the following contents.
1. Weighing 10-20 g of activated carbon, ultrasonically cleaning, drying, calcining and activating in a muffle furnace at 400-500 ℃ for 1-2 h, and then placing in a shaking table for oscillation; in the oscillation process, firstly, uniformly spraying 3mmol/L AgNO on the surface of the active carbon3Controlling the spraying speed of the solution to be about 5-10 mL/min, and spraying for 2min each time; then evenly spraying 1mmol/L H on the surface of the activated carbon3PO4Spraying the solution at a speed of 5-10 mL/min for 2min each time, and repeating the steps for 5-20 times; and then taking out the activated carbon, washing the activated carbon for 3-5 times by using deionized water, and drying to obtain the activated carbon-loaded petal-shaped silver phosphate complex phase photocatalytic material.
2. The ultrasonic cleaning temperature is room temperature, the frequency is 20kHz, and the power is 5 kW.
3. The drying mode of the activated carbon before loading is blast drying, the drying temperature is 100-150 ℃, and the drying time is 3-5 h.
4. The shaking table is in a rotary oscillation mode, the rotary frequency is 50-400 r/min, and the oscillation amplitude is 20-30 mm.
5. The drying method of the loaded activated carbon comprises the following steps: first N2Blowing for 5-10 min, N2The flow velocity is 0.2-0.5 m3Min; then vacuum drying at 80-100 ℃ for 10-12 DEG Ch, degree of vacuum<200Pa。
Drawings
Fig. 1 is an SEM image of an activated carbon-supported petal-shaped silver phosphate complex phase photocatalytic material prepared under the process conditions of example 1.
FIG. 2 is a graph showing the degradation curve of rhodamine B (0.5 g/L, 400 ml) in the amount of 1g of the activated carbon-supported petal-shaped silver phosphate complex phase photocatalytic material prepared under the process conditions of example 1.
Detailed Description
The present invention will be described in detail with reference to examples, but the present invention is not limited to these production examples.
Example 1
Weighing 10g of activated carbon, ultrasonically cleaning at room temperature, wherein the ultrasonic frequency is 20kHz, the ultrasonic power is 5kW, carrying out forced air drying at 110 ℃ for 3h, and then calcining and activating at 400 ℃ in a muffle furnace for 2 h; then placing the activated carbon in a shaking table for oscillation, wherein the gyration frequency is 200r/min, and the oscillation amplitude is 20 mm; in the oscillation process, firstly, uniformly spraying 3mmol/L AgNO on the surface of the active carbon3Spraying the solution at a speed of about 5mL/min for 2min each time; then evenly spraying 1mmol/L H on the surface of the activated carbon3PO4Spraying the solution at a speed of about 5mL/min for 2min each time, and repeating the steps for 10 times; then taking out the activated carbon, and washing the activated carbon for 3 times by using deionized water; n is a radical of2Blow drying for 5min, N2Flow velocity of 0.2m3Min; and then drying the mixture for 12h at 80 ℃ in vacuum with the vacuum degree =180Pa to obtain the activated carbon-loaded petal-shaped silver phosphate complex phase photocatalytic material.
Example 2
Weighing 10g of activated carbon, ultrasonically cleaning at room temperature, wherein the ultrasonic frequency is 20kHz, the ultrasonic power is 5kW, carrying out forced air drying at 100 ℃ for 4h, and then calcining and activating at 400 ℃ in a muffle furnace for 1 h; then placing the activated carbon in a shaking table for oscillation, wherein the gyration frequency is 200r/min, and the oscillation amplitude is 20 mm; in the oscillation process, firstly, uniformly spraying 3mmol/L AgNO on the surface of the active carbon3Spraying the solution at a speed of 7mL/min for 2min each time; then evenly spraying 1mmol/L H on the surface of the activated carbon3PO4The solution is sprayed at a speed of about 7mL/min per unitSpraying for 2min, and repeating the above steps for 12 times; then taking out the activated carbon, and washing the activated carbon for 3 times by using deionized water; n is a radical of2Blow-drying for 10min, N2Flow velocity of 0.5m3Min; and then drying the mixture for 12 hours in vacuum at the temperature of 80 ℃ with the vacuum degree =150Pa to obtain the activated carbon loaded petal-shaped silver phosphate complex phase photocatalytic material.
Example 3
Weighing 15g of activated carbon, ultrasonically cleaning at room temperature, wherein the ultrasonic frequency is 20kHz, the ultrasonic power is 5kW, carrying out forced air drying at 120 ℃ for 3h, and then calcining and activating at 450 ℃ in a muffle furnace for 1.5 h; then placing the activated carbon in a shaking table for oscillation, wherein the gyration frequency is 200r/min, and the oscillation amplitude is 30 mm; in the oscillation process, firstly, uniformly spraying 3mmol/L AgNO on the surface of the active carbon3Spraying the solution at a speed of about 8mL/min for 2min each time; then evenly spraying 1mmol/L H on the surface of the activated carbon3PO4Spraying the solution at a speed of about 8mL/min for 2min each time, and repeating the steps for 5 times; then taking out the activated carbon, and washing the activated carbon for 3 times by using deionized water; n is a radical of2Blow-drying for 10min, N2Flow velocity of 0.5m3Min; and then drying the mixture at 90 ℃ for 10h in vacuum with the vacuum degree =180Pa to obtain the activated carbon-loaded petal-shaped silver phosphate complex phase photocatalytic material.
Example 4
Weighing 15g of activated carbon, ultrasonically cleaning at room temperature, wherein the ultrasonic frequency is 20kHz, the ultrasonic power is 5kW, carrying out forced air drying at 130 ℃ for 4h, and then calcining and activating at 450 ℃ in a muffle furnace for 2 h; then placing the activated carbon in a shaking table for oscillation, wherein the gyration frequency is 200r/min, and the oscillation amplitude is 25 mm; in the oscillation process, firstly, uniformly spraying 3mmol/L AgNO on the surface of the active carbon3Spraying the solution at a speed of about 8mL/min for 2min each time; then evenly spraying 1mmol/L H on the surface of the activated carbon3PO4Spraying the solution at a speed of about 8mL/min for 2min each time, and repeating the steps for 10 times; then taking out the activated carbon, and washing the activated carbon for 3 times by using deionized water; n is a radical of2Blow-drying for 10min, N2Flow velocity of 0.5m3Min; and then drying for 12h at 90 ℃ in vacuum with the vacuum degree =160Pa to obtain the activated carbon-loaded petal-shaped silver phosphate complex phase photocatalytic material.
Example 5
Weighing 15g of activated carbon, ultrasonically cleaning at room temperature, wherein the ultrasonic frequency is 20kHz, the ultrasonic power is 5kW, carrying out forced air drying at 120 ℃ for 5h, and then calcining and activating at 500 ℃ in a muffle furnace for 1 h; then placing the activated carbon in a shaking table for oscillation, wherein the gyration frequency is 200r/min, and the oscillation amplitude is 30 mm; in the oscillation process, firstly, uniformly spraying 3mmol/L AgNO on the surface of the active carbon3Spraying the solution at a speed of about 10mL/min for 2min each time; then evenly spraying 1mmol/L H on the surface of the activated carbon3PO4Spraying the solution at a speed of about 10mL/min for 2min each time, and repeating the steps for 15 times; then taking out the activated carbon, and washing the activated carbon for 5 times by using deionized water; n is a radical of2Blow-drying for 10min, N2Flow velocity of 0.5m3Min; and then drying the mixture for 10 hours in vacuum at 100 ℃ with the vacuum degree =160Pa to obtain the activated carbon-loaded petal-shaped silver phosphate complex phase photocatalytic material.
Example 6
Weighing 20g of activated carbon, ultrasonically cleaning at room temperature, wherein the ultrasonic frequency is 20kHz, the ultrasonic power is 5kW, carrying out forced air drying at 150 ℃ for 5h, and then calcining and activating at 500 ℃ in a muffle furnace for 2 h; then placing the activated carbon in a shaking table for oscillation, wherein the gyration frequency is 300r/min, and the oscillation amplitude is 30 mm; in the oscillation process, firstly, uniformly spraying 3mmol/L AgNO on the surface of the active carbon3Spraying the solution at a speed of about 10mL/min for 2min each time; then evenly spraying 1mmol/L H on the surface of the activated carbon3PO4Spraying the solution at a speed of about 10mL/min for 2min each time, and repeating the steps for 20 times; then taking out the activated carbon, and washing the activated carbon for 5 times by using deionized water; n is a radical of2Blow-drying for 10min, N2Flow velocity of 0.5m3Min; and then drying for 12h at 100 ℃ in vacuum with the vacuum degree =180Pa to obtain the activated carbon-loaded petal-shaped silver phosphate complex phase photocatalytic material.
Claims (5)
1. A synthetic method of an activated carbon-loaded petaloid silver phosphate complex-phase photocatalytic material is characterized by comprising the following steps: weighing 10-20 g of activated carbon, ultrasonically cleaning, drying, calcining and activating in a muffle furnace at 400-500 ℃ for 1-2 h, and then placing in a shaking table for oscillation; during the oscillation process, firstlyThe surface of the active carbon is evenly sprayed with 3mmol/L AgNO3Spraying the solution at a speed of 5-10 mL/min for 2min each time; then evenly spraying 1mmol/L H on the surface of the activated carbon3PO4Spraying the solution at a speed of 5-10 mL/min for 2min each time, and repeating the steps for 5-20 times; and then taking out the activated carbon, washing the activated carbon for 3-5 times by using deionized water, and drying to obtain the activated carbon-loaded petal-shaped silver phosphate complex phase photocatalytic material.
2. The method for synthesizing the activated carbon-supported petal-shaped silver phosphate complex phase photocatalytic material as claimed in claim 1, wherein the ultrasonic cleaning temperature is room temperature, the frequency is 20kHz, and the power is 5 kW.
3. The method for synthesizing the activated carbon-supported petal-shaped silver phosphate complex phase photocatalytic material as claimed in claim 1, wherein the drying mode of the activated carbon before loading is blast drying, the drying temperature is 100-150 ℃, and the drying time is 3-5 h.
4. The method for synthesizing the activated carbon-supported petal-shaped silver phosphate composite photocatalytic material as claimed in claim 1, wherein the shaking table oscillation mode is cyclotron oscillation, the cyclotron frequency is 50-400 r/min, and the oscillation amplitude is 20-30 mm.
5. The method for synthesizing the activated carbon-supported petal-shaped silver phosphate complex phase photocatalytic material as claimed in claim 1, wherein the method for drying the supported activated carbon comprises the following steps: first N2Blowing for 5-10 min, N2The flow velocity is 0.2-0.5 m3Min; then vacuum drying for 10-12 h at 80-100 ℃ and vacuum degree<200Pa。
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| CN110756043B (en) * | 2019-10-31 | 2022-04-12 | 江苏清荷材料科技有限公司 | Automobile ceiling capable of purifying VOC in automobile and preparation method thereof |
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