CN112427016A - Silver-loaded porous carbon microsphere and preparation method thereof - Google Patents
Silver-loaded porous carbon microsphere and preparation method thereof Download PDFInfo
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 132
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 94
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 title claims abstract description 84
- 229910052709 silver Inorganic materials 0.000 title claims abstract description 66
- 239000004332 silver Substances 0.000 title claims abstract description 66
- 239000004005 microsphere Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 28
- 239000002245 particle Substances 0.000 claims abstract description 23
- 238000011065 in-situ storage Methods 0.000 claims abstract description 15
- 239000000243 solution Substances 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 229910021389 graphene Inorganic materials 0.000 claims description 20
- SQGYOTSLMSWVJD-UHFFFAOYSA-N silver(1+) nitrate Chemical group [Ag+].[O-]N(=O)=O SQGYOTSLMSWVJD-UHFFFAOYSA-N 0.000 claims description 16
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 10
- 239000012153 distilled water Substances 0.000 claims description 10
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 9
- 229910052751 metal Inorganic materials 0.000 claims description 9
- 239000002184 metal Substances 0.000 claims description 9
- 239000002243 precursor Substances 0.000 claims description 9
- 239000000463 material Substances 0.000 claims description 7
- 239000000843 powder Substances 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 238000001291 vacuum drying Methods 0.000 claims description 7
- 238000009210 therapy by ultrasound Methods 0.000 claims description 6
- 229910052786 argon Inorganic materials 0.000 claims description 5
- 239000012159 carrier gas Substances 0.000 claims description 5
- 239000007789 gas Substances 0.000 claims description 5
- 239000005416 organic matter Substances 0.000 claims description 5
- 239000010453 quartz Substances 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- GGCZERPQGJTIQP-UHFFFAOYSA-N sodium;9,10-dioxoanthracene-2-sulfonic acid Chemical group [Na+].C1=CC=C2C(=O)C3=CC(S(=O)(=O)O)=CC=C3C(=O)C2=C1 GGCZERPQGJTIQP-UHFFFAOYSA-N 0.000 claims description 5
- 238000005118 spray pyrolysis Methods 0.000 claims description 5
- 239000000126 substance Substances 0.000 claims description 5
- 238000005979 thermal decomposition reaction Methods 0.000 claims description 5
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims description 4
- 229930006000 Sucrose Natural products 0.000 claims description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 4
- 229910000069 nitrogen hydride Inorganic materials 0.000 claims description 4
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 4
- 239000012266 salt solution Substances 0.000 claims description 4
- 239000005720 sucrose Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 3
- 238000005406 washing Methods 0.000 claims description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 2
- 229920001661 Chitosan Polymers 0.000 claims description 2
- 108010010803 Gelatin Proteins 0.000 claims description 2
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 2
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 2
- 239000004202 carbamide Substances 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 229920000159 gelatin Polymers 0.000 claims description 2
- 239000008273 gelatin Substances 0.000 claims description 2
- 235000019322 gelatine Nutrition 0.000 claims description 2
- 235000011852 gelatine desserts Nutrition 0.000 claims description 2
- 239000008103 glucose Substances 0.000 claims description 2
- 229910021382 natural graphite Inorganic materials 0.000 claims description 2
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 2
- 229910001961 silver nitrate Inorganic materials 0.000 claims description 2
- 230000008569 process Effects 0.000 abstract description 12
- 239000011159 matrix material Substances 0.000 abstract description 4
- 239000007833 carbon precursor Substances 0.000 description 6
- 239000003595 mist Substances 0.000 description 6
- 238000001179 sorption measurement Methods 0.000 description 4
- 230000000844 anti-bacterial effect Effects 0.000 description 3
- 238000005087 graphitization Methods 0.000 description 3
- 239000006199 nebulizer Substances 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 239000003242 anti bacterial agent Substances 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 125000004432 carbon atom Chemical group C* 0.000 description 2
- 238000003763 carbonization Methods 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 238000005470 impregnation Methods 0.000 description 2
- 238000002844 melting Methods 0.000 description 2
- 230000008018 melting Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 238000000197 pyrolysis Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 239000003651 drinking water Substances 0.000 description 1
- 235000020188 drinking water Nutrition 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 230000001151 other effect Effects 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- -1 silver ions Chemical class 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 238000009827 uniform distribution Methods 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
-
- 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
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28016—Particle form
- B01J20/28021—Hollow particles, e.g. hollow spheres, microspheres or cenospheres
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- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a silver-loaded porous carbon microsphere and a preparation method thereof, belongs to the field of activated carbon, and relates to the silver-loaded porous carbon microsphere formed by uniformly embedding nano silver in hollow porous carbon in an in-situ mode. According to the invention, the silver-loaded porous carbon microspheres formed by inlaying silver particles in the hollow porous carbon in an in-situ manner are adopted, so that the nano silver is uniformly distributed, and the nano silver is firmly combined with the carbon matrix, so that the silver particles are not easy to fall off, and the effectiveness and the service life in the use process are ensured.
Description
Technical Field
The invention mainly relates to the field of activated carbon, in particular to silver-loaded porous carbon microspheres and a preparation method thereof.
Background
The porous activated carbon material has huge specific surface area and abundant pore structure, has larger adsorption capacity and faster adsorption rate to chlorine, organic matters and other undesirable impurities in water, is easy to regenerate, is matched with silver with stronger bactericidal performance, and is considered to be the best combination in air or drinking water treatment. The silver-carrying antibacterial agent using the porous activated carbon material as a carrier is usually formed by loading metallic silver particles on the carrier through physical adsorption. The preparation method of the antibacterial agent generally utilizes the high-efficiency adsorption performance of a porous activated carbon material (activated carbon or carbon fiber), metal or metal compounds such as silver, silver salt and the like are adsorbed and deposited on the activated carbon material by a mixed melting method or an impregnation method, and the activated carbon material is properly treated to prepare the porous carbon containing the nano metal silver particles with high specific surface area and high dispersibility. The antibacterial performance of the silver-loaded porous carbon depends on the size of the specific surface area, and when the specific surface area is the same, the antibacterial property is enhanced along with the increase of the silver content; when the silver content is the same, the larger the specific surface area is, the stronger the sterilization ability is. The surface properties (the number of micropores, graphitization degree, reactivity and the like) of porous carbon and the initial concentration of silver ions in a solution influence the size and the form of metal silver particles, the metal silver adsorbed to the surface can be reduced into nano-scale particles through a mixed melting method or an impregnation method, but the silver particles are still difficult to wrap the micropores of the active porous carbon and are adsorbed to the outer surface, and part of the micropores are blocked, so that the washing resistance of the porous carbon is poor.
Disclosure of Invention
The invention aims to solve the technical problem of providing a silver-loaded porous carbon microsphere and a preparation method thereof, so that nano silver is embedded in mesoporous porous carbon in an in-situ manner and is firmly combined with a carbon matrix, silver particles are not easy to fall off, and the effectiveness and the service life in the using process are ensured.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
on the one hand, the invention provides a silver-loaded porous carbon microsphere, which is formed by uniformly embedding nano silver in hollow porous carbon in an in-situ mode.
The in-situ mode of the invention means that the silver particles are combined with the raw material of the hollow porous carbon before the hollow porous carbon is formed, and are embedded in the hollow porous carbon in the forming process (usually the high-temperature pyrolysis process) of the hollow porous carbon, namely, the silver particles are formed in situ, so that the silver particles are uniformly distributed and firmly combined, and the silver particles are not easy to fall off, thereby ensuring the effectiveness and the service life in the using process.
Further, the carbon microspheres are hollow porous carbon microspheres embedded with nano-silver particles, which are synthesized by pre-mixing a carbon source and a metallic silver precursor and then performing spray pyrolysis, wherein the carbon source is a carbon-containing organic substance and graphene oxide. Further, the metallic silver precursor may be silver nitrate.
The forming principle of the carbon microsphere is as follows: the fogdrop is utilized to form a spherical shape, the graphene oxide and an organic carbon precursor (carbon-containing organic matter) are pyrolyzed at high temperature to form carbon spheres, and the carbon spheres have rich pore structures and higher graphitization degree due to the decomposition of the organic matter and other effects; meanwhile, after high-temperature reduction, the nano-scale metal silver particles are uniformly embedded in the porous carbon spheres in situ. Because the graphene oxide contains various oxygen-containing functional groups, the graphene oxide has a strong bonding effect with an organic carbon precursor, and carbon atoms are rearranged and mutually diffused in the carbonization process to form an integrated carbon sphere with a consistent structure. In addition, the silver salt solution and the organic carbon precursor solution are fully mixed in advance, and the nano silver and the porous carbon spheres are formed in situ, so that the distribution is uniform, the combination is firm, the silver particles are not easy to fall off, and the effectiveness and the service life in the use process are ensured.
On the other hand, a preparation method of the silver-loaded porous carbon microspheres is provided, the silver-loaded porous carbon microspheres are synthesized by a spray pyrolysis method after a carbon source and a metal silver precursor are mixed in advance, so that the nano silver is embedded in the mesoporous porous carbon in an in-situ manner, and the carbon source comprises a carbon-containing organic matter and graphene oxide.
Further, the carbon source is a solution formed by dissolving a carbon-containing organic substance, potassium carbonate and graphene oxide in water and then performing ultrasonic treatment for a period of time.
Further, the metal silver precursor is a clear solution obtained by dropwise adding ammonia water to a silver salt solution.
Further, one specific method may include the following steps:
1) 0.5-2.0 parts by weight of AgNO3Dissolved in 100 parts by weight of water and added dropwise with NH3·H2Solution of O to clear (general Ag/NH)3·H2O is 1: 2) forming a solution A;
2) 0.5 part by weight of organic carbon-containing material and 0.25 part by weight of K were mixed under stirring2CO3And 0.02-0.2 part by weight of graphene oxide is dissolved in 100 parts by weight of distilled water, and ultrasonic treatment is carried out for a period of time to form a solution B;
3) mixing and stirring the A, B solution, performing ultrasonic treatment for a period of time, atomizing by using an ultrasonic atomizer to generate a large amount of fog drops, carrying the fog drops into a quartz tube of a tube furnace by using argon gas as a carrier gas at 800 ℃ for carrying out thermal decomposition reaction for 1 hour, collecting the prepared powder, washing the powder with distilled water for a plurality of times, and performing vacuum drying on the collected sample to obtain the silver-loaded porous carbon sample.
Further, the ultrasonic time in the step 2) is 25-35 minutes.
Further, the ultrasonic time in the step 3) is 25-35 minutes.
Further, the ultrasonic sprayer in the step 3) is a 1.7MHz ultrasonic sprayer.
Further, the temperature of vacuum drying in the step 3) is 80 ℃, and the drying time is 12 hours.
Further, the carbon-containing organic matter is one or more of gelatin, chitosan, sucrose, citric acid, glucose and urea.
Further, the graphene oxide is 325-mesh natural graphite and is prepared by a modified Hummers method.
The forming principle of the carbon microsphere is as follows: forming spherical shape by using fog drops, and forming carbon spheres, organic matters and K by carrying out high-temperature pyrolysis on graphene oxide and organic carbon precursor2CO3The carbon spheres have rich pore structures and higher graphitization degree under the catalysis of potassium steam; meanwhile, after high-temperature reduction, the nano-scale metal silver particles are uniformly embedded in the porous carbon spheres in situ. Because the graphene oxide contains various oxygen-containing functional groups, the graphene oxide has a strong bonding effect with an organic carbon precursor, and carbon atoms are rearranged and mutually diffused in the carbonization process to form an integrated carbon sphere with a consistent structure. In addition, the silver salt solution and the carbon precursor solution are fully mixed in advance, and the nano silver and the porous carbon spheres are formed in situ, so that the distribution is uniform, the combination is firm, the silver particles are not easy to fall off, and the effectiveness and the service life in the use process are ensured.
The method selects carbon-containing organic matters and graphene as carbon sources and AgNO3The hollow porous carbon microspheres embedded with nano-silver particles are synthesized for a metallic silver precursor by adopting a spray pyrolysis method, and the nano-silver is uniformly distributed and firmly combined with a carbon substrate. And the method has simple equipment, low cost and environmental protection.
After adopting such design, the invention has at least the following advantages:
according to the invention, the silver-loaded porous carbon microspheres formed by inlaying silver particles in the hollow porous carbon in an in-situ manner are adopted, so that the nano silver is uniformly distributed, and the nano silver is firmly combined with the carbon matrix, so that the silver particles are not easy to fall off, and the effectiveness and the service life in the use process are ensured.
Drawings
The foregoing is only an overview of the technical solutions of the present invention, and in order to make the technical solutions of the present invention more clearly understood, the present invention is further described in detail below with reference to the accompanying drawings and the detailed description.
FIG. 1 is a scanning electron micrograph of silver-loaded porous carbon microspheres prepared according to the present invention; wherein (a), (b), (c) and (d) are spherical activated carbon prepared in different examples.
Detailed Description
The present invention is further illustrated by the following examples, but the present invention is not limited to the following examples, and any products similar or equivalent to the present invention, which are obtained by the teaching of the present invention, are within the scope of protection.
According to the invention, the silver-loaded porous carbon microspheres formed by inlaying silver particles in the hollow porous carbon in an in-situ manner are adopted, so that the nano silver is uniformly distributed, and the nano silver is firmly combined with the carbon matrix, so that the silver particles are not easy to fall off, and the effectiveness and the service life in the use process are ensured. The specific preparation examples are as follows:
example 1
0.5g of AgNO3Dissolved in 100 ml of aqueous solution and added dropwise with NH3·H2Solution of O to clear (Ag/NH)3·H2O is 1: 2). 0.5g of sucrose, 0.25g K was mixed under stirring2CO3And 0.05g of graphene oxide was dissolved in 100 ml of distilled water and sonicated for 30 minutes. Then, the two solutions were poured into a three-necked flask, stirred and sonicated for 30min, and then atomized with a 1.7MHz ultrasonic nebulizer to generate a large amount of mist droplets, the mist droplets were carried into a quartz tube of a tube furnace using argon gas as a carrier gas to perform a thermal decomposition reaction at 800 ℃ for 1 hour, then the prepared powder was collected and washed with distilled water several times, and the collected sample was dried in a 80 ℃ vacuum drying oven for 12 hours to obtain a silver-loaded porous carbon sample.
Example 2
1.0g of AgNO3Dissolved in 100 ml of aqueous solution and added dropwise with NH3·H2Solution of O to clear (Ag/NH)3·H2O is 1: 2). 0.5g of citric acid, 0.25g K was mixed under stirring2CO3And 0.05g of graphene oxide was dissolved in 100 ml of distilled water and sonicated for 30 minutes. Then, the two solutions were poured into a three-necked flask, stirred and sonicated for 30min, and then atomized with a 1.7MHz ultrasonic nebulizer to generate a large amount of mist droplets, the mist droplets were carried into a quartz tube of a tube furnace using argon gas as a carrier gas to perform a thermal decomposition reaction at 800 ℃ for 1 hour, then the prepared powder was collected and washed with distilled water several times, and the collected sample was dried in a 80 ℃ vacuum drying oven for 12 hours to obtain a silver-loaded porous carbon sample.
Example 3
1.0g of AgNO3Dissolving in 100 ml of water solution, and dripping NH 3. H2O solution until the solution is clear (Ag/NH)3·H2O is 1: 2). 0.5g of sucrose, 0.25g K was mixed under stirring2CO3And 0.1g of graphene oxide was dissolved in 100 ml of distilled water and sonicated for 30 minutes. Then, the two solutions were poured into a three-necked flask, stirred and sonicated for 30min, and then atomized with a 1.7MHz ultrasonic nebulizer to generate a large amount of mist droplets, the mist droplets were carried into a quartz tube of a tube furnace using argon gas as a carrier gas to perform a thermal decomposition reaction at 800 ℃ for 1 hour, then the prepared powder was collected and washed with distilled water several times, and the collected sample was dried in a 80 ℃ vacuum drying oven for 12 hours to obtain a silver-loaded porous carbon sample.
The silver-loaded porous carbon microspheres prepared in the embodiments 1 to 3 have uniform distribution of nano silver and firm combination with a carbon substrate, so that silver particles are not easy to fall off, and the effectiveness and the service life in the use process are ensured. And the method has simple equipment, low cost and environmental protection.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the present invention in any way, and it will be apparent to those skilled in the art that the above description of the present invention can be applied to various modifications, equivalent variations or modifications without departing from the spirit and scope of the present invention.
Claims (10)
1. The silver-loaded porous carbon microsphere is characterized in that nano silver is uniformly embedded in hollow porous carbon in an in-situ mode to form the silver-loaded porous carbon microsphere.
2. The silver-loaded porous carbon microsphere according to claim 1, wherein the carbon microsphere is a hollow porous carbon microsphere embedded with nano-silver particles, which is synthesized by a spray pyrolysis method after a carbon source and a metallic silver precursor are mixed in advance, and the carbon source is a carbon-containing organic substance and graphene oxide.
3. The silver-loaded porous carbon microsphere according to claim 2, wherein the metallic silver precursor is silver nitrate.
4. The preparation method of the silver-loaded porous carbon microspheres is characterized in that a carbon source and a metal silver precursor are premixed and then synthesized by a spray pyrolysis method, so that nano silver is embedded in mesoporous porous carbon in an in-situ manner, and the carbon source comprises a carbon-containing organic matter and graphene oxide.
5. The method for preparing the silver-loaded porous carbon microspheres according to claim 4, wherein the carbon source is a solution formed by dissolving a carbon-containing organic substance, potassium carbonate and graphene oxide in water and then performing ultrasonic treatment for a period of time.
6. The method for preparing the silver-loaded porous carbon microspheres according to claim 4 or 5, wherein the metallic silver precursor is a silver salt solution which is clarified by dripping ammonia water.
7. The method for preparing silver-loaded porous carbon microspheres according to any one of claims 4 to 6, characterized in that the specific method comprises the following steps:
1) 0.5-2.0 parts by weight of AgNO3Dissolved in 100 parts by weight of water and added dropwise with NH3·H2Clarifying the solution O to form solution A;
2) 0.5 part by weight of organic carbon-containing material and 0.25 part by weight of K were mixed under stirring2CO3And 0.02-0.2 part by weight of graphene oxide is dissolved in 100 parts by weight of distilled water, and ultrasonic treatment is carried out for a period of time to form a solution B;
3) mixing and stirring the A, B solution, performing ultrasonic treatment for a period of time, atomizing by using an ultrasonic atomizer to generate a large amount of fog drops, carrying the fog drops into a quartz tube of a tube furnace by using argon gas as a carrier gas at 800 ℃ for carrying out thermal decomposition reaction for 1 hour, collecting the prepared powder, washing the powder with distilled water for a plurality of times, and performing vacuum drying on the collected sample to obtain the silver-loaded porous carbon sample.
8. The preparation method of the silver-loaded porous carbon microsphere according to claim 7, wherein the ultrasonic time in the step 2) is 25-35 minutes;
and/or, the ultrasonic time in the step 3) is 25-35 minutes;
and/or, the ultrasonic sprayer in the step 3) is a 1.7MHz ultrasonic sprayer;
and/or the temperature of vacuum drying in the step 3) is 80 ℃, and the drying time is 12 hours.
9. The method for preparing the silver-loaded porous carbon microspheres according to any one of claims 4 to 8, wherein the carbon-containing organic substance is one or more of gelatin, chitosan, sucrose, citric acid, glucose and urea.
10. The method for preparing the silver-loaded porous carbon microspheres according to any one of claims 4 to 9, wherein the graphene oxide is 325-mesh natural graphite and is prepared by a modified Hummers method.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104857902A (en) * | 2015-04-13 | 2015-08-26 | 南京理工大学 | Preparation method of silver/carbon composite hollow nanospheres |
| CN107808955A (en) * | 2017-10-27 | 2018-03-16 | 湖南工业大学 | A kind of absorbent charcoal material with spherical structure and its preparation method and application |
| CN108275681A (en) * | 2018-01-16 | 2018-07-13 | 上海理工大学 | A kind of preparation method of cellular porous carbon ball |
| CN109437322A (en) * | 2018-11-05 | 2019-03-08 | 浙江工业大学 | A kind of compound carbon ball of metal oxide and preparation method thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104857902A (en) * | 2015-04-13 | 2015-08-26 | 南京理工大学 | Preparation method of silver/carbon composite hollow nanospheres |
| CN107808955A (en) * | 2017-10-27 | 2018-03-16 | 湖南工业大学 | A kind of absorbent charcoal material with spherical structure and its preparation method and application |
| CN108275681A (en) * | 2018-01-16 | 2018-07-13 | 上海理工大学 | A kind of preparation method of cellular porous carbon ball |
| CN109437322A (en) * | 2018-11-05 | 2019-03-08 | 浙江工业大学 | A kind of compound carbon ball of metal oxide and preparation method thereof |
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