CN111908470A - Preparation method of antibacterial silver-loaded activated carbon - Google Patents
Preparation method of antibacterial silver-loaded activated carbon Download PDFInfo
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- CN111908470A CN111908470A CN202010817163.4A CN202010817163A CN111908470A CN 111908470 A CN111908470 A CN 111908470A CN 202010817163 A CN202010817163 A CN 202010817163A CN 111908470 A CN111908470 A CN 111908470A
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
- C01B32/354—After-treatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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Abstract
The invention discloses a preparation method of antibacterial silver-loaded activated carbon, which comprises the following steps: 1) weighing a certain amount of active carbon, and soaking in AgNO3In solution; 2) selecting deflocculant, and dissolving in AgNO under ultrasonic condition3In solution; 3) then slowly dripping glucose solution into AgNO in a stirring state3Heating in water bath in the solution, and magnetically stirring; 4) filtering the product of 3), washing with water for multiple times to remove redundant glucose until Ag + is completely removed, and then drying in vacuum; 5) and (3) drying the product in the step (4) in a blast oven, and then firing the product at a high temperature of 500 ℃ in a nitrogen atmosphere in a tubular furnace to obtain the product.
Description
Technical Field
The invention relates to activated carbon, in particular to a preparation method of silver-loaded activated carbon.
Background
Safe and reliable drinking water supply has important significance for guaranteeing the health of people and economic development, and water supply enterprises need to manage the whole process from water sources to users, particularly in the stage of pipe network water supply, so as to guarantee that end users obtain safe and high-quality drinking water. Although the factory water is disinfected by adding chlorine, a large number of microorganisms are killed, even the water in the pipe network is maintained to contain a certain residual chlorine amount so as to keep the disinfection effect, and the water using terminal still has the problem that the qualification rate of bacteriological indexes is obviously reduced. Recent research and industrial application results show that the conventional chlorine disinfection process, the contact oxidation iron and manganese removal and chlorination disinfection process, the coagulation, precipitation, filtration, chlorine disinfection process and other methods cannot effectively remove microorganisms in water.
The broad-spectrum bactericidal property of silver ions has a long application history, and the excellent adsorption property of the carbon-based material is also frequently applied to the field of water treatment. Through introducing silver antibacterial material in the charcoal base material, can not only kill the bacterial microorganism in the drinking water, can reduce the microorganism quantity on charcoal base material surface moreover, restrain the microorganism and proliferate on charcoal base material surface, promote the drinking water taste, further ensure drinking water safety.
Disclosure of Invention
The invention aims to provide a preparation method of antibacterial silver-loaded activated carbon, which has better silver adsorption capacity and antibacterial property.
The purpose of the invention is realized as follows: a preparation method of antibacterial silver-loaded activated carbon is characterized by comprising the following steps:
step 1) weighing a certain amount of active carbon, and soaking the active carbon in AgNO3In solution;
step 2) selecting a deflocculant, and dissolving the deflocculant in AgNO under the ultrasonic condition3In solution;
step 3) then slowly adding the glucose solution dropwise to AgNO under stirring3Heating in water bath in the solution, and magnetically stirring;
step 4) filtering the product obtained in the step 3), washing with water for multiple times to remove redundant glucose until Ag + is completely removed, and then drying in vacuum;
and 5) drying the product obtained in the step 4) in a blast oven, and then burning at a high temperature of 500 ℃ in a nitrogen atmosphere in a tubular furnace to obtain the product.
As a further improvement of the invention, AgNO in step 1)3The concentration of the solution was 0.08 mol/L.
As a further improvement of the invention, phosphate is selected as the deflocculant in the step 2), and the deflocculant is prepared by the following steps: weighing a certain amount of deflocculant according to the mass ratio of silver ions (0.2-1) to 1.
As a further improvement of the invention, the step 3) is heated by a water bath at 60 ℃ and stirred magnetically for 24 hours.
As a further improvement of the invention, the drying in step 4) is carried out for 8h at 70 ℃ under vacuum.
As a further development of the invention, in step 5) drying is carried out for 2h at 70 ℃ in a forced air oven.
As a further improvement of the invention, the specific temperature raising procedure in the step 5) is as follows: the room temperature is increased to 120 ℃, the temperature is kept for 30min, the temperature is increased to 300 ℃, the temperature is kept for 60min, the temperature is increased to 500 ℃, the temperature is kept for 120min, and the temperature is reduced.
Compared with the prior art, the invention has the beneficial effects that: according to the invention, the square flocculant is added in the preparation process of the activated carbon as a buffer solution, and as most of the deflocculant is ions or atomic groups with charges on the surfaces, the charged groups are adsorbed on the surfaces of silver particles, and coulomb repulsion is generated on the surfaces of crystals to repel each other, so that the silver particles with good dispersion effect are obtained; phosphate is selected as a deflocculant, so that the deflocculant has good fire resistance, and silver ion loss caused by high temperature influence is avoided when high-temperature ignition is carried out at the later stage; thereby avoiding silver ion agglomeration and further improving the antibacterial property; meanwhile, the internal structure of the activated carbon is changed physically, the activated carbon is subjected to high-temperature atmosphere treatment, the internal pore volume and the pore structure are changed, so that the silver carrying capacity of the activated carbon is increased, and the antibacterial performance of the activated carbon is further enhanced; the product structure is prevented from being damaged by high temperature rapidly through the temperature rise design.
Drawings
FIG. 1 is a flow chart of the present invention.
FIG. 2 is a graph of the silver loading detection of different activated carbons.
Fig. 3 is a comparative graph of antibacterial tests of different activated carbons.
Fig. 4 is an XRD spectrum of this example 1.
Detailed Description
The present invention is further illustrated by the following specific examples.
Example 1
The preparation method of the antibacterial silver-loaded activated carbon shown in figure 1 comprises the following steps:
step 1) weighing a certain amount of active carbon, and soaking the active carbon in AgNO with the concentration of 0.08mol/L3In solution;
step 2), selecting phosphate as a deflocculant, and performing deflocculant: weighing a certain amount of deflocculant with the silver ion mass ratio of 0.5:1, and dissolving the deflocculant in AgNO under the ultrasonic condition3In solution;
step 3) then slowly adding the glucose solution dropwise to AgNO under stirring3Heating in water bath at 60 deg.C in the solution, and magnetically stirring for 24 hr;
step 4) filtering the product obtained in the step 3), washing with water for multiple times to remove redundant glucose until Ag + is completely removed, and then drying in vacuum at 70 ℃ for 8 hours;
and 5) drying the product obtained in the step 4) in a blast oven at 70 ℃ for 2h, and then firing at a high temperature in a tubular furnace in a nitrogen atmosphere, wherein the specific temperature raising program is as follows: raising the temperature to 120 ℃, staying for 30min, raising the temperature to 300 ℃, staying for 60min, raising the temperature to 500 ℃, staying for 120min, and cooling to obtain the product.
Example 2
It differs from example 1 only in that: deflocculant silver ion =0.3:1, and no high temperature firing was performed.
Example 3
It differs from example 1 only in that: deflocculant silver ion =0.2:1, and no high temperature firing was performed.
Example 4
It differs from example 1 only in that: deflocculant silver ion =1:1, and no high temperature firing was performed.
The following description is made by comparing the antibacterial silver-loaded activated carbon prepared in this example with the comparative example.
Comparative example 1
Step 1) weighing a certain amount of active carbon, and soaking the active carbon in AgNO with the concentration of 0.08mol/L3In solution;
step 2), selecting polyethylene glycol (PEG) as a dispersing agent, and mixing the components according to the following ratio: weighing a certain amount of dispersing agent according to the silver ion mass ratio of 0.5:1, and dissolving the dispersing agent in AgNO under the ultrasonic condition3In solution;
step 3) then slowly adding the glucose solution dropwise to AgNO under stirring3Heating in water bath at 60 deg.C in the solution, and magnetically stirring for 24 hr;
and 4) filtering the product obtained in the step 3), washing with water for multiple times, removing redundant glucose until Ag + is completely removed, and then drying in vacuum at 70 ℃ for 8 hours to obtain the product.
Comparative example 2
The difference from comparative example 1 is: dispersing agent: the mass ratio of silver ions is 0.8: 1.
Comparative example 3
The difference from comparative example 1 is: dispersing agent: the mass ratio of silver ions is 1: 1.
Comparative example 4
The difference from comparative example 1 is: dispersing agent: the mass ratio of silver ions is 1.5: 1.
Comparative example 5
And adding no dispersant or deflocculant to prepare the silver-loaded activated carbon.
The silver-carrying amount of the silver-carrying activated carbon in the above examples and comparative examples was measured, as shown in FIG. 2, under different protective agents, wherein Nos. 1 to 4 represent examples 1 to 4, Nos. 5 to 8 represent comparative examples 1 to 4, and No. 9 represents comparative example 5. It can be seen from the figure that the maximum silver carrying amount of the material after the high-temperature ignition is matched under the protection of the deflocculant in the aspect of silver carrying amount is 17.53%, and the maximum silver carrying amounts of the material after the high-temperature ignition is not carried out under the protection of the phosphate deflocculant are respectively: 17.17%, 17.12%, 17.08%, the maximum silver loading of the material under the protection of the PEG dispersant was 17.11%, and the silver loading of comparative example 5 was 17.09%. It can be concluded that the silver content of the silver-loaded material prepared by the cooperation of the deflocculant is slightly larger than that of the PEG dispersant and slightly larger than that of the silver-loaded active carbon without the action of the protective agent, which indicates that the deflocculant has the advantages that groups with charges on the surface are adsorbed by the surfaces of silver particles, so that coulomb repulsion is generated on the surfaces of crystals to repel each other, silver particles with good dispersion effect are obtained, and the silver-loaded energy is enhanced; however, as can be seen from the silver loading of the dispersant PEG, the silver loading of the PEG-protected silver-loaded material is relatively not increased or even decreased, which indicates that the dispersant can not promote the reaction, and the dispersion state of the silver particles in the reaction system is changed. In addition, the silver-carrying amount of the activated carbon after high-temperature burning treatment is obviously increased, and the particle size of the activated carbon is continuously reduced along with the increase of the treatment temperature, so that the activated carbon is changed into a fine-crushed granular material from obvious irregular large granules; the collapse of the pores of the activated carbon begins to occur as the temperature is increased, exposing the silver particles hidden in the pores, because in the reaction system, the Ag + diffuses into the pores as the reaction proceeds, thereby increasing the silver ion content after the collapse of the pores begins to occur.
The following examples and comparative antibacterial tests were carried out.
Placing prepared agar culture medium, normal saline and other glass instruments used in experiments in a high pressure steam sterilization pot, and sterilizing at 121 deg.C for 30 min. The melted culture medium is placed in a constant-temperature water bath at the temperature of about 45 ℃, the melted culture medium is used as soon as possible, and the standing time is generally not more than 4 hours. The strain was diluted 1000 times, and an equal amount of the particles of examples 1 to 4 and comparative examples 1 to 5 was placed in a petri dish, 0.25mL of the diluted strain was inoculated in the petri dish using a pipette, and the inoculated petri dish was placed in a constant temperature incubator and cultured in an inverted state at 37 ℃ for 12 hours while keeping ventilation.
As shown in FIG. 3, in which comparative example No. 1, comparative example Nos. 2 to 5 represent comparative examples 1 to 4, and comparative example Nos. 6 to 9 represent examples 1 to 4. From the colony growth beside the two protectant materials, it is clear that the sterilization effect of the examples is significantly better than that of the comparative examples 1-5; the deflocculant does not influence the growth amount of silver particles in the reaction, changes the existing state among the particles, prevents the nano silver from agglomerating, and thus improves the antibacterial property of the material.
The XRD spectrum of example 1 is analyzed again, and the spectrum is obtained by a Transmission Electron Microscope (TEM), as shown in fig. 4, the elemental silver particles generated by the reaction are dispersed in the surface of the activated carbon material in the existing state, and the aggregation state is not serious, further illustrating that the protective effect of the deflocculant is effective, and the particle size of the generated silver particles reaches the nano level. The silver particles with small particle size and good dispersibility can further increase the contact chance of the silver particles with the cell surface, thereby improving the antibacterial property of the material.
The present invention is not limited to the above-mentioned embodiments, and based on the technical solutions disclosed in the present invention, those skilled in the art can make some substitutions and modifications to some technical features without creative efforts according to the disclosed technical contents, and these substitutions and modifications are all within the protection scope of the present invention.
Claims (7)
1. A preparation method of antibacterial silver-loaded activated carbon is characterized by comprising the following steps:
step 1) weighing a certain amount of active carbon, and soaking the active carbon in AgNO3In solution;
step 2) selecting a deflocculant, and dissolving the deflocculant in AgNO under the ultrasonic condition3In solution;
step 3) then slowly adding the glucose solution dropwise to AgNO under stirring3Heating in water bath in the solution, and magnetically stirring;
step 4) filtering the product obtained in the step 3), washing with water for multiple times to remove redundant glucose until Ag + is completely removed, and then drying in vacuum;
and 5) drying the product obtained in the step 4) in a blast oven, and then burning at a high temperature of 500 ℃ in a nitrogen atmosphere in a tubular furnace to obtain the product.
2. The method for preparing an antimicrobial silver-loaded activated carbon as claimed in claim 1, wherein AgNO in step 1)3The concentration of the solution was 0.08 mol/L.
3. The process for preparing an antimicrobial silver-loaded activated carbon as claimed in claim 1, wherein the deflocculant in step 2) is phosphate, and the deflocculant: weighing a certain amount of deflocculant according to the mass ratio of silver ions (0.2-1) to 1.
4. The method for preparing an antibacterial silver-loaded activated carbon as claimed in claim 1, wherein step 3) is performed by heating in a water bath at 60 ℃ and magnetic stirring for 24 h.
5. The method for preparing an antibacterial silver-loaded activated carbon as claimed in claim 1, wherein the vacuum drying at 70 ℃ is performed for 8h in the step 4).
6. The process for preparing an antibacterial silver-loaded activated carbon as claimed in claim 1, wherein the drying in step 5) is carried out for 2 hours at 70 ℃ in a blast oven.
7. The method for preparing an antibacterial silver-loaded activated carbon as claimed in claim 1, wherein the specific temperature raising procedure in the step 5) is as follows: the room temperature is increased to 120 ℃, the temperature is kept for 30min, the temperature is increased to 300 ℃, the temperature is kept for 60min, the temperature is increased to 500 ℃, the temperature is kept for 120min, and the temperature is reduced.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0120604A1 (en) * | 1983-02-28 | 1984-10-03 | Amoco Corporation | Metal-containing active carbon and methods for making and using same |
| CN1876927A (en) * | 2006-06-28 | 2006-12-13 | 陆书明 | Silver-supported active carbon cloth and production method thereof |
| WO2009053972A1 (en) * | 2007-10-22 | 2009-04-30 | Toxsorb Ltd | Modified activated carbon as adsorbent for anionic and cationic inorganic pollutants |
| CN103232035A (en) * | 2013-03-26 | 2013-08-07 | 赵建树 | Nanometer silver-loaded active carbon and preparation method thereof |
| CN106958140A (en) * | 2017-03-24 | 2017-07-18 | 北京璟胜科技有限公司 | A kind of NACF of loading nano silvery and preparation method thereof |
| CN108176354A (en) * | 2017-12-11 | 2018-06-19 | 广东韩研活性炭科技股份有限公司 | A kind of preparation method of the special sizing active carbon loading silver of refrigerator |
| CN109279675A (en) * | 2018-09-30 | 2019-01-29 | 江苏斯沃得环保科技有限公司 | A kind of preparation method of active carbon loading silver |
-
2020
- 2020-08-14 CN CN202010817163.4A patent/CN111908470A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0120604A1 (en) * | 1983-02-28 | 1984-10-03 | Amoco Corporation | Metal-containing active carbon and methods for making and using same |
| CN1876927A (en) * | 2006-06-28 | 2006-12-13 | 陆书明 | Silver-supported active carbon cloth and production method thereof |
| WO2009053972A1 (en) * | 2007-10-22 | 2009-04-30 | Toxsorb Ltd | Modified activated carbon as adsorbent for anionic and cationic inorganic pollutants |
| CN103232035A (en) * | 2013-03-26 | 2013-08-07 | 赵建树 | Nanometer silver-loaded active carbon and preparation method thereof |
| CN106958140A (en) * | 2017-03-24 | 2017-07-18 | 北京璟胜科技有限公司 | A kind of NACF of loading nano silvery and preparation method thereof |
| CN108176354A (en) * | 2017-12-11 | 2018-06-19 | 广东韩研活性炭科技股份有限公司 | A kind of preparation method of the special sizing active carbon loading silver of refrigerator |
| CN109279675A (en) * | 2018-09-30 | 2019-01-29 | 江苏斯沃得环保科技有限公司 | A kind of preparation method of active carbon loading silver |
Non-Patent Citations (1)
| Title |
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| 王世宇: "《药用辅料学 十三五规划》", 30 April 2019 * |
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