CN110550709B - Bactericidal biochar loaded with silver particles and preparation method thereof - Google Patents
Bactericidal biochar loaded with silver particles and preparation method thereof Download PDFInfo
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- CN110550709B CN110550709B CN201910809557.2A CN201910809557A CN110550709B CN 110550709 B CN110550709 B CN 110550709B CN 201910809557 A CN201910809557 A CN 201910809557A CN 110550709 B CN110550709 B CN 110550709B
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/16—Heavy metals; Compounds thereof
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/50—Treatment of water, waste water, or sewage by addition or application of a germicide or by oligodynamic treatment
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2303/00—Specific treatment goals
- C02F2303/04—Disinfection
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A40/00—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production
- Y02A40/10—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production in agriculture
- Y02A40/22—Improving land use; Improving water use or availability; Controlling erosion
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P60/00—Technologies relating to agriculture, livestock or agroalimentary industries
- Y02P60/20—Reduction of greenhouse gas [GHG] emissions in agriculture, e.g. CO2
- Y02P60/21—Dinitrogen oxide [N2O], e.g. using aquaponics, hydroponics or efficiency measures
Abstract
The invention belongs to the field of water resource treatment, and particularly relates to a bactericidal biochar loaded with silver particles and a preparation method thereof. The method comprises the following steps: dropwise adding a potassium hydroxide or sodium hydroxide solution into the silver nitrate solution to obtain a silver hydroxide precipitate, and filtering to obtain a silver hydroxide solid; dispersing biomass powder in ethanol to form a biomass-ethanol system, adding the silver hydroxide solid into the biomass-ethanol system to obtain a mixed system, stirring the mixed system at room temperature for 10-24h, heating to 50-70 ℃, and stopping heating after the ethanol is completely volatilized to obtain Ag-biomass; and heating the Ag-biomass to 700 ℃ in the nitrogen atmosphere, maintaining for 2-4h, cooling to room temperature, and taking out to obtain the silver particle-loaded bactericidal biochar. The prepared charcoal not only can adsorb and remove bacteria in water in a short time, but also has a killing effect on the bacteria, and the killing rate can reach 50%.
Description
Technical Field
The invention belongs to the field of water resource treatment, and particularly relates to a bactericidal biochar loaded with silver particles and a preparation method thereof.
Background
Pollution of water-borne pathogens and related diseases in environmental water are water quality problems which are generally concerned by all countries in the world. Pathogen contamination is a serious problem for almost all types of environmental water, and therefore identification and understanding of pathogen contamination is of concern. The presence of E.coli in water bodies indicates contamination of the water body by animals and human feces, meaning the presence of many relevant pathogenic microorganisms, and thus monitoring the levels of indicator organisms (e.g., fecal coliform, E.coli) is a common method of quantifying the potential pathogen load in water bodies.
The biomass charcoal serving as a cheap and easily-obtained adsorbing material with a high specific surface area can better retain pathological microorganisms in a water environment, but cannot kill germs. Although silver ions can pass through cell membranes, bind to proteins in cells, denature them, lose normal physiological functions, and eventually cause the bacteria to die. However, it is difficult to recover it by directly adding it to water.
At present, in the prior art, there is a method for loading silver on biomass charcoal, and patent CN104307475A discloses a method for preparing coconut shell activated carbon with silver slow-release sterilization function by hydrothermal reaction, which is characterized in that: the method comprises the steps of taking coconut shell activated carbon as a raw material and silver nitrate as impregnation liquid, preparing silver-loaded activated carbon through hydrothermal reaction, and calcining at high temperature under the condition of nitrogen protection to obtain the product. The operation process is mainly characterized in that coconut shell activated carbon is used as a raw material, and the coconut shell activated carbon has high adsorption capacity, high speed, durability and reproducibility; the silver is more effectively loaded on the active carbon by the hydrothermal reaction method; the reactivation of the silver-loaded activated carbon is facilitated through high-temperature calcination, so that silver particles are more uniformly distributed on the surface of the activated carbon, and the silver slow-release function is realized.
Disclosure of Invention
The invention provides another preparation method of the bactericidal biochar loaded with silver particles, and the bactericidal biochar prepared by the method can be used for removing pathogenic microorganisms in water resources such as natural water bodies, tail water of sewage plants and the like, and has excellent bactericidal efficiency.
A preparation method of bactericidal biochar loaded with silver particles comprises the following steps:
(1) dropwise adding a potassium hydroxide or sodium hydroxide solution into the silver nitrate solution to obtain a silver hydroxide precipitate, and filtering to obtain a silver hydroxide solid;
(2) dispersing biomass powder in ethanol to form a biomass-ethanol system, adding the silver hydroxide solid into the biomass-ethanol system to obtain a mixed system, stirring the mixed system at room temperature for 10-24h, heating to 50-70 ℃, and stopping heating after the ethanol is completely volatilized to obtain Ag-biomass;
(3) and heating the Ag-biomass to 700 ℃ in the nitrogen atmosphere, maintaining for 2-4h, cooling to room temperature, and taking out to obtain the bactericidal biochar loaded with silver particles.
Preferably, the biomass powder is obtained by crushing peanut shells and sieving the crushed peanut shells with a 200-mesh sieve.
Preferably, in the step (3), the heating is performed at 10 ℃/min.
Preferably, the mass ratio of the silver nitrate to the biomass is 1-3: 100. More preferably, the mass ratio of the silver nitrate to the biomass is 1: 10.
Preferably, in the biomass-ethanol system, the mass-volume ratio of the biomass to the ethanol is 1 g: 500 mL.
Preferably, the step (1) comprises the following specific steps:
a1. treating with a dilute sodium hydroxide solution: weighing 10g of sodium hydroxide, dissolving the sodium hydroxide in 100mL of ultrapure water, and preparing a dilute sodium hydroxide solution with the mass fraction of 5% (w/v);
a2. weighing 1-3g of silver nitrate solid, dissolving the silver nitrate solid in 100mL of ultrapure water, carrying out ultrasonic treatment for 20 minutes, adding a dilute sodium hydroxide solution into the silver nitrate solution under the stirring condition, adjusting the pH to 14.5, maintaining the pH for 1 minute without jumping, and carrying out solid-water separation by using a suction filtration device, wherein the solid is a silver hydroxide solid.
Preferably, the step (3) comprises the following specific steps:
placing the Ag-biomass in a porcelain boat and placing the porcelain boat in a tube furnace; before the tube furnace is opened, firstly evacuating the air in the tube furnace by using a vacuum pump, introducing nitrogen into the tube furnace after confirming that the tube furnace is in a negative pressure closed state, and repeating the operation for three times to ensure that the air in the tube furnace is evacuated; starting the tubular furnace, setting the heating rate to be 10 ℃/min, setting the temperature to be 500-700 ℃, and maintaining the peak temperature for 2 h; and after the firing process of the tubular furnace is finished, cooling to room temperature, and taking out to obtain the bactericidal biochar.
Preferably, in the step (3), the Ag — biomass is heated to 700 ℃.
The bactericidal biochar prepared by the preparation method also belongs to the protection scope of the invention.
The room temperature of the invention is 15-25 ℃.
The invention has the beneficial effects that:
(1) the sterilization biochar prepared by the preparation method disclosed by the invention not only can adsorb and remove bacteria in a water body in a short time, but also has a sterilization effect on the bacteria, and the sterilization rate can reach 50%;
(2) the bactericidal biochar prepared by the preparation method disclosed by the invention is large in specific surface area and high in adsorption efficiency, can quickly remove bacteria in a water body, and is a massive solid and easy to recover.
Drawings
FIG. 1 is the xps test results for the six materials prepared in example 1;
FIG. 2 is the surface silver to silver oxide ratio of the six materials prepared in example 1;
FIG. 3 shows the 3h sterilization effect of the six materials in example 2;
FIG. 4 shows the adsorption and killing of Escherichia coli by the six materials in example 2, wherein (a) the percentage of Escherichia coli inactivated within 3 hours by bactericidal biochar (700 ℃) loaded with 1% Ag; (b) the percentage of the inactivated escherichia coli within 3 hours of the bactericidal biochar (700 ℃) with the load of 2 percent; (c) the percentage of the inactivated escherichia coli within 3 hours of the bactericidal biochar (700 ℃) with the load of 3 percent; (d) the percentage of the sterilized biological carbon (500 ℃) with the load of 1 percent in the inactivated colibacillus within 3 hours; (e) 2 percent of bactericidal biochar (500 ℃) with the loading capacity, and the percentage of inactivated escherichia coli in 3 hours; (f) the percentage of the inactivated escherichia coli in 3 hours with 3% of bactericidal biochar (500 ℃);
FIG. 5 shows the silver ion concentrations in the reaction solutions of the six materials in example 2.
Detailed Description
The invention is further illustrated below with reference to examples and figures.
Example 1
A preparation method of silver particle-loaded bactericidal biomass charcoal comprises the following steps:
(1) weighing 10g of analytically pure sodium hydroxide solid, dissolving in 100mL of ultrapure water, stirring with a glass rod for 20 minutes at room temperature, and then sonicating in an ultrasonic instrument for 20 minutes; using a 200mL volumetric flask to fix the volume of the completely dissolved sodium hydroxide solution, and completing the preparation of a dilute sodium hydroxide solution with the mass fraction of 5% (w/v); weighing 3g of silver nitrate solid, dissolving the silver nitrate solid in 100mL of ultrapure water, performing ultrasonic treatment for 20 minutes, and then putting the silver nitrate solid into a magnetic stirring device for continuous stirring; to the silver nitrate solution was added a dilute sodium hydroxide solution, the pH was adjusted to 14.5 and maintained over 1 minute without pH jump.
(2) Carrying out solid-water separation on the silver hydroxide precipitate obtained in the step (1) through a suction filtration device, and placing the silver hydroxide precipitate in a clean culture dish for standing; grinding biomass (peanut shells) in a mill and passing through a 200-mesh screen; adding 100g of biomass (peanut shells) into a beaker filled with 500mL of alcohol, and fully stirring for 3 hours in magnetic stirring; adding the silver hydroxide precipitate in the culture dish into a biomass-alcohol system, continuously stirring for 24 hours in a magnetic stirring device, marking as a material with 3 percent of loading capacity, placing the obtained mixture into a heating magnetic stirrer, setting the temperature to be 60 ℃, and continuously stirring until the alcohol in a beaker is completely volatilized, wherein the part which is not volatilized at this time is a uniform mixture of the silver hydroxide precipitate and the biomass.
(3) Putting the mixture of the silver hydroxide precipitate and the biomass into a porcelain boat, and putting the porcelain boat into a tubular furnace; before the tube furnace is opened, firstly evacuating the air in the tube furnace by using a vacuum pump, introducing nitrogen into the tube furnace after confirming that the tube furnace is in a negative pressure closed state, and repeating the operation for three times to ensure that the air in the tube furnace is evacuated; starting the tube furnace, setting the heating rate to be 10 ℃/min, setting the temperature to be 700 ℃, and maintaining the temperature at 700 ℃ for 2 h; and after the firing process of the tubular furnace is finished, the mixture of the biomass and the silver hydroxide is pyrolyzed in the high-temperature oxygen-insulating mode to obtain the bactericidal biochar with the loading capacity of 3% Ag.
According to the preparation method, 1% and 2% Ag-loaded bactericidal biochar is prepared by adding silver nitrate with different masses.
Meanwhile, according to the preparation method, the carbonization temperature in the step (3) is changed to 500 ℃, and the bactericidal biochar with the Ag loading amounts of 1%, 2% and 3% is prepared at the carbonization temperature of 500 ℃.
For the 6 bactericidal biochar prepared in this example, XPS scanning was performed on six biochar-nanoparticles loaded with silver, the distribution of silver within 10nm of the surface of each biochar was monitored, and it can be seen from comparison of XPS scanning of silver-loaded biochar with different metal loading fired at the same pyrolysis temperature in fig. 1 that the total amount of silver loaded at 10nm on the surface of each biochar-nanoparticle was positively correlated with the silver loading when the filler was prepared. In addition, the XPS scanning results show that the silver distributed on the surface of the filler includes silver simple substance and silver oxide, and the total amount of silver and silver in different forms is quantitatively analyzed, and as shown in table 1, the amount of silver simple substance and silver oxide increases in a nearly ascending manner with the increase of the total amount of silver load. Quantitative analysis is carried out on the proportion of the silver with different forms in the total silver on the surface of the filler, and as a result, as shown in fig. 2, the variation trend of the silver with different forms along with the total silver load is influenced by the pyrolysis temperature selected in the preparation of the filler, wherein the silver oxide is approximately reduced along with the increase of the silver load when the firing temperature is 500 ℃, and is approximately reduced along with the increase of the silver load when the firing temperature is 700 ℃; the silver content increases with the silver loading approximately at 500 degrees, and decreases with the silver loading approximately at 700 degrees.
TABLE 1 surface nanoparticle Loading of six materials
Example 2
Preparing 1L water body containing Escherichia coli with sterilized water, and measuring Escherichia coli concentration to 10 by plate counting method6CFU/mL, and adding 0.5g of bactericidal biochar (6 biochar prepared in example 1) into the water body, and carrying out sterilization removal for 3h under magnetic stirring; after 3h of reaction, the removal rate of Escherichia coli was measured by using a plate counting method, and as can be seen from FIG. 3, the percentage of Escherichia coli removed in 3h of the sterilized biochar fired at 700 ℃ was positively correlated with the silver loading (R)20.91), wherein the percentage of escherichia coli removed in 3h of the biochar-nano silver particles with a loading of 3% fired at 700 degrees is higher than 90%, and is 95.46%. The percentage of escherichia coli removed within 3h for 500 degree fired biochar-nanosilver particles is inversely related to the silver loading (R)2-0.88), but the percentage of escherichia coli removal in 3h of the silver-loaded biochar was higher than that of the 500 degree fired pure biochar, wherein the 500 degree fired biochar with a loading of 1% was 95.09% with the percentage of escherichia coli removal in 3h of the nano-silver particles being higher than 90%.
Taking a biochar-nano silver particle reaction solution substrate for 3 hours, and detecting the physiological state and the death rate of escherichia coli in the reaction solution by using a flow cytometer. Fig. 4(a) is a schematic diagram of the analysis result of the flow cytometer for the 700-degree-fired biocarbon with a loading of 1%, namely, the flow cytometer for the nano-silver particles shows that the percentage of the inactivated escherichia coli in 3h is 22.26%, and the analysis data shows that the percentage of the inactivated enterobacter coli in 3h of the 700-degree-fired biocarbon, namely, the nano-silver particles, is increased (22.26% -69.82%) with the increase of the nano-silver loading (1% -3%); the percentage of inactivated escherichia coli in 3h of the 500-degree burnt biochar, namely the nano silver particles, is increased (13.66% -22.09%). According to the ICP test result, the concentration of the silver ions in the reaction liquid for 3h is inconsistent with the change trend of the mortality of the escherichia coli, and the reason that the mechanism that the biological carbon and the nano silver particles kill the enterobacter coli is presumed to be that the biological carbon and the nano silver particles not only release the silver ions into the reaction liquid for sterilization, but also contact the escherichia coli with the nano silver particles loaded on the biological carbon for sterilization.
As can be seen from FIG. 5, the 500 degree calcined charcoal, namely the nano silver particles, react for 3 hours, and the silver ion concentration in the reaction solution is negatively correlated with the load capacity when 24 hours, and the correlation coefficient is-0.91, -0.96; when the silver loading is increased from 1% to 3%, the concentration of silver ions in the reaction liquid is reduced from 0.04146mg/L to 0.03356mg/L when the reaction is carried out for 3h, and the concentration of silver ions in the reaction liquid is reduced from 0.1081mg/L to 0.07243mg/L when the reaction is carried out for 24 h. The silver ion concentration of the biochar, namely nano silver particles, fired at 700 ℃ is negatively related to the load capacity in 3h of reaction liquid, and the correlation coefficient is-0.98 and-0.97. When the silver loading is increased from 1% to 3%, the concentration of silver ions in the reaction liquid is reduced from 0.3228mg/L to 0.1107mg/L when the reaction is carried out for 3h, and the concentration of silver ions in the reaction liquid is reduced from 0.5223mg/L to 0.1932mg/L when the reaction is carried out for 24 h.
Claims (8)
1. A preparation method of bactericidal biochar loaded with silver particles comprises the following steps:
(1) dropwise adding a potassium hydroxide or sodium hydroxide solution into the silver nitrate solution to obtain a silver hydroxide precipitate, and filtering to obtain a silver hydroxide solid;
(2) dispersing biomass powder in ethanol to form a biomass-ethanol system, adding the silver hydroxide solid into the biomass-ethanol system to obtain a mixed system, stirring the mixed system at room temperature for 10-24h, heating to 50-70 ℃, and stopping heating after ethanol is completely volatilized to obtain Ag-biomass;
(3) heating the Ag-biomass to 700 ℃ in the nitrogen atmosphere, maintaining for 2-4h, cooling to room temperature, and taking out to obtain the bactericidal biochar loaded with silver particles and silver monoxide; the heating rate during heating is 10 ℃/min;
the mass ratio of the silver nitrate to the biomass is 1-3: 100.
2. The method of claim 1, wherein the biomass powder is obtained by pulverizing peanut shells and sieving the pulverized peanut shells through a 200-mesh sieve.
3. The preparation method according to claim 1, wherein the mass ratio of the silver nitrate to the biomass is 1: 100.
4. The preparation method according to claim 1, wherein the biomass-ethanol system has a biomass-ethanol mass-to-volume ratio of 1 g: 500 mL.
5. The preparation method according to claim 1, wherein the step (1) comprises the following specific steps:
a1. weighing 10g of analytically pure sodium hydroxide, dissolving in 100mL of ultrapure water, and preparing a dilute sodium hydroxide solution with the mass fraction of 5% (w/v);
a2. weighing 1-3g of silver nitrate solid, dissolving the silver nitrate solid in 100mL of ultrapure water, carrying out ultrasonic treatment for 20 minutes, adding a dilute sodium hydroxide solution into the silver nitrate solution under the stirring condition, adjusting the pH to 14.5, maintaining the pH for 1 minute without jumping, and carrying out solid-water separation by using a suction filtration device to obtain the silver hydroxide solid.
6. The preparation method according to claim 1, wherein the step (3) comprises the following specific steps:
placing the Ag-biomass in a porcelain boat and placing the porcelain boat in a tube furnace; before the tube furnace is opened, firstly evacuating the air in the tube furnace by using a vacuum pump, introducing nitrogen into the tube furnace after confirming that the tube furnace is in a negative pressure closed state, and repeating the operation for three times to ensure that the air in the tube furnace is evacuated; starting the tube furnace, setting the heating rate to be 10 ℃/min, setting the temperature to be 500-700 ℃, and maintaining the peak temperature for 2 h; and after the firing process of the tubular furnace is finished, cooling to room temperature, and taking out to obtain the bactericidal biochar.
7. The method according to any one of claims 1 to 6, wherein the Ag-biomass is heated to 700 ℃ in the step (3).
8. A bactericidal biochar carrying silver particles, characterized by being produced by the production method according to any one of claims 1 to 6.
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| CN111359579A (en) * | 2020-03-31 | 2020-07-03 | 张雨璨 | Preparation method of antibacterial diatomite wall material |
| CN111841496B (en) * | 2020-07-24 | 2022-02-22 | 泉州南京大学环保产业研究院 | Method for rapidly preparing silver-loaded activated carbon |
| CN113457623B (en) * | 2021-06-18 | 2022-09-20 | 广西大学 | Method for adsorbing antibiotics in water by using silver-ytterbium modified charcoal |
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