CN113413875A - Preparation method of modified activated carbon for efficiently removing bacteria in water - Google Patents
Preparation method of modified activated carbon for efficiently removing bacteria in water Download PDFInfo
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- 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
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- 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
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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
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- B01J20/32—Impregnating or coating ; Solid sorbent compositions obtained from processes involving impregnating or coating
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
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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
Abstract
The invention discloses a preparation method of modified activated carbon for efficiently removing bacteria in water, belonging to the field of sewage treatment, wherein conventional activated carbon is used as base carbon, the base carbon is subjected to iron removal treatment, the base carbon is subjected to boiling and washing for three times, silver nitrate solution is added after drying and standing for uniform mixing, ultrasonic auxiliary treatment and vacuum drying are carried out to obtain primary carbon, the primary carbon is added with alkali metal salt solution for uniform mixing, ultrasonic auxiliary treatment and drying are carried out to obtain secondary carbon, and the secondary carbon is put into a muffle furnace for burning treatment to obtain the modified activated carbon. The degerming rate in water is more than 99.99 percent, and the level of the special carbon for removing bacteria is achieved.
Description
Technical Field
The invention belongs to the field of sewage treatment, and particularly relates to a preparation method of modified activated carbon for efficiently removing bacteria in water.
Background
Escherichia coli, also known as Escherichia coli, is a normal colonizing bacterium in the intestinal tract of animals, a small proportion of which causes disease under certain conditions. The serotype of escherichia coli can cause gastrointestinal infections of human or animals, mainly caused by infection with specific pilus antigens, pathogenic toxins and the like, and can cause urinary tract infection, arthritis, meningitis, sepsis type infection and the like besides gastrointestinal tract infection.
Staphylococcus aureus, also known as Staphylococcus aureus, belongs to the genus Staphylococcus, is a representative of gram-positive bacteria, and is a common food-borne pathogenic microorganism. The bacteria have optimum growth temperature of 37 deg.C, pH of 7.4, high salt tolerance, and can grow in environment with salt concentration close to 10%. Staphylococcus aureus is a common food-borne pathogenic bacterium, and is widely found in the natural environment, often parasitizing in the skin, nasal cavity, throat, intestines and stomach, carbuncle, suppurative sore and the like of human and animals, and in the air, sewage and other environments. Under appropriate conditions, staphylococcus aureus can produce enterotoxin, causing food poisoning.
In the prior art, the silver-loaded activated carbon can not only keep the function of adsorbing organic compounds and partial inorganic matters in water, but also effectively inhibit the growth and propagation of escherichia coli and staphylococcus aureus by utilizing the loaded silver, but the problem of silver loss is difficult to solve in the industrial production process of the silver-loaded activated carbon.
Through retrieval, Chinese patent application No. CN201510832329.9 discloses a high-load nano-silver activated carbon and a preparation method thereof, and discloses that nano-silver and pretreated activated carbon are purified and dried after being matched with auxiliary means to reduce silver loss and increase silver load, but the invention does not use experimental data to prove the effect of silver loss, and only uses ICP to measure silver load.
Disclosure of Invention
In order to solve the problem of high silver loss rate of the silver-loaded activated carbon, the invention provides a preparation method of modified activated carbon for efficiently removing bacteria in water.
The specific technical scheme of the invention is as follows:
a preparation method of modified activated carbon for efficiently removing bacteria in water comprises the following steps:
(1) preparing materials:
according to the carbon base: silver nitrate: the mass ratio of the alkali metal salt is 100: 0.1-0.5: 0.05-0.3 preparing base carbon, silver nitrate and alkali metal salt;
(2) loading:
measuring the saturated adsorption water quantity M of the base carbon, and taking deionized water which is 1-1.5 times of the saturated adsorption water quantity M; dissolving silver nitrate in the step (1) in the deionized water, adding base carbon, uniformly mixing, performing auxiliary treatment for 10-60 minutes by using ultrasonic waves of 20-40 kHz, and performing vacuum drying for 0.5-2 hours at the temperature of 50-80 ℃ to obtain primary carbon;
dissolving the alkali metal salt in the step (1) in deionized water which is 1-1.5 times of the saturated adsorption water quantity M, uniformly mixing the alkali metal salt with the primary carbon, performing auxiliary treatment for 10-60 minutes by using ultrasonic waves of 20-40 kHz, and drying for 0.5-3 hours at the temperature of 50-150 ℃ to obtain secondary carbon;
(3) fixing:
and (3) putting the secondary carbon into a muffle furnace, and burning for 1-5 hours at the temperature of 150-295 ℃ to obtain the modified activated carbon.
Further, the base carbon in the step (1) is conventional activated carbon.
Further, the conventional activated carbon is one or more of coal-based activated carbon, wood-based activated carbon, shell activated carbon and coconut shell activated carbon.
Further, the conventional activated carbon is one or more of granular, powdery, lamellar or amorphous.
Further, carrying out iron removal treatment on the base carbon in the step (1), washing and boiling for three times, and drying.
Further, the alkali metal salt in the step (1) is a soluble salt containing one metal ion of Li, Na, K and Rb.
Further, the soluble salt is one or more of acid salt, sulfate, nitrate, carbonate and bicarbonate.
Further, the saturated adsorbed water amount M in the step (2) is measured by the following operations: weighing 1Kg of base carbon to be detected, adding water, metering M0, stirring uniformly to realize full adsorption, then weighing the mass M1 of filtrate after suction filtration, deducting the mass to obtain the adsorbed water quantity Mn, namely Mn = M0-M1, repeatedly measuring for several times, and taking the average value of Mn to obtain the saturated adsorption water quantity M of the base carbon to be detected.
Has the advantages that:
according to the invention, silver nitrate is selected as a raw material for first loading of the base carbon, is easy to dissolve in water, has the effects of etching and killing germs, and has a very good actual convergence effect, but the loading rate of silver is not high when the silver is loaded on the surface of the active carbon.
In all alkali solutions, it was found that sodium carbonate solution increased the silver loading better than the other solutions, and the second loading of sodium carbonate reacted with the first silver nitrate loading on the carbon surface to form silver carbonate, which was insoluble in water and chemically stable at room temperature and in air, but the silver loss rate from the modified activated carbon surface was still rather high over multiple uses, leading to increased costs and secondary pollution.
In the face of the problem of high loss rate, the silver carbonate is melted and decomposed at 218 ℃ by adopting a physical burning method to process, so that silver oxide and carbon dioxide are generated. Experiments show that the silver oxide is not easy to lose on the surface of the active carbon, the silver oxide is firmly bonded with functional groups on the surface of the active carbon, but the silver oxide is decomposed into simple substance silver and oxygen when heated to more than 300 ℃, the loss condition of the simple substance silver on the surface of the active carbon is obviously improved compared with the silver oxide, and other alkali metal salts are not changed when added at the temperature, so that the fixed burning temperature is controlled to be 150-295 ℃.
Treatment with suitable ultrasound during loading can enhance the stability of silver on the surface of activated carbon, increase the loading of silver and reduce the silver leaching rate.
The modified activated carbon for removing bacteria in water is safe in raw material, low in price, low in cost, simple and convenient in method, easy to operate and easy for industrial expanded production; the method combining chemical reaction and physical fixation has obvious effect of removing bacteria in water, is safe and stable, does not produce secondary pollution because of low silver loss rate and stable substances after reaction, and is convenient to use. The degerming rate in water is more than 99.99 percent, and the level of the special carbon for removing bacteria is achieved.
Drawings
FIG. 1 is an experimental flow chart of a preparation method of modified activated carbon for efficiently removing bacteria in water.
Detailed Description
Example 1
(1) Preparing materials:
taking 100g of granular coal-based activated carbon of 5-10 meshes as base carbon, knowing that the saturated adsorption water quantity of the coal-based activated carbon is M =600g/Kg, carrying out iron removal treatment on the base carbon by using a magnetic separator through a magnetic separation method, carrying out three times of boiling and drying; weighing silver nitrate with the mass of 0.1 percent of the base carbon; weighing lithium chloride with the mass of 0.05 percent of the base carbon.
(2) Loading:
dissolving the silver nitrate in the step (1) in deionized water which is 1.2 times of the saturated adsorption water quantity M, adding the base carbon, uniformly mixing, carrying out auxiliary treatment for 10 minutes by using 20KHz ultrasonic wave, turning over the base carbon to ensure that the solution is fully and uniformly absorbed by the base carbon, and then carrying out vacuum drying for 0.5 hour at 80 ℃ to obtain primary carbon; dissolving the lithium chloride in the step (1) in deionized water which is 1.2 times of the saturated adsorption water quantity M, uniformly mixing the lithium chloride with primary carbon, carrying out auxiliary treatment for 20 minutes by using 25KHz ultrasonic waves, turning over the lithium chloride once every 10 minutes to ensure that the solution is fully and uniformly absorbed by the primary carbon, and then drying the lithium chloride for 0.5 hour at the temperature of 150 ℃ to obtain secondary carbon.
(3) Fixing:
and (3) putting the secondary carbon into a muffle furnace, and burning for 1 hour at the temperature of 295 ℃ to obtain the modified activated carbon.
Example 2
(1) Preparing materials:
taking 100g of granular wood activated carbon of 40-60 meshes as base carbon, knowing that the saturated adsorption water quantity of the coal activated carbon is M =900g/Kg, carrying out iron removal treatment on the base carbon by using a magnetic separator through a magnetic separation method, carrying out three times of boiling and drying; weighing silver nitrate with the mass of 0.3 percent of the base carbon; sodium bicarbonate with the mass of 0.1 percent of the base carbon is weighed.
(2) Loading:
dissolving the silver nitrate in the step (1) in deionized water which is 1.4 times of the saturated adsorption water quantity M, adding base carbon, uniformly mixing, carrying out auxiliary treatment for 40 minutes by using 25KHz ultrasonic, turning over the base carbon every 10 minutes to ensure that the solution is fully and uniformly absorbed by the base carbon, and then carrying out vacuum drying for 1 hour at 70 ℃ to obtain primary carbon; and (2) dissolving the sodium bicarbonate in the step (1) in deionized water which is 1.4 times of the saturated adsorption water quantity M, uniformly mixing the sodium bicarbonate with the primary carbon, performing auxiliary treatment for 30 minutes by using 30KHz ultrasonic waves, turning over the sodium bicarbonate once every 10 minutes to ensure that the solution is fully and uniformly absorbed by the primary carbon, and drying the mixture for 1.2 hours at the temperature of 140 ℃ to obtain secondary carbon.
(3) Fixing:
and (3) putting the secondary carbon into a muffle furnace, and burning for 2 hours at 290 ℃ to obtain the modified activated carbon.
Example 3
(1) Preparing materials:
taking 100g of 8-30-mesh lamellar shell activated carbon as base carbon, knowing that the saturated adsorption water quantity of the shell activated carbon is M =720g/Kg, carrying out iron removal treatment on the base carbon by using a magnetic separator through a magnetic separation method, boiling for three times, and drying; weighing silver nitrate accounting for 0.4 percent of the mass of the base carbon, and weighing potassium nitrate accounting for 0.3 percent of the mass of the base carbon;
(2) loading:
dissolving the silver nitrate in the step (1) in deionized water which is 1.5 times of the saturated adsorption water quantity M, adding base carbon, uniformly mixing, performing auxiliary treatment for 60 minutes by using 40KHz ultrasonic, turning over the base carbon every 10 minutes to ensure that the solution is fully and uniformly absorbed by the base carbon, and then performing vacuum drying for 2 hours at 50 ℃ to obtain primary carbon; dissolving the potassium nitrate in the step (1) in deionized water which is 1.5 times of the saturated adsorption water quantity M, uniformly mixing the potassium nitrate with primary carbon, carrying out auxiliary treatment for 50 minutes by using 35KHz ultrasonic waves, turning over the mixture once every 10 minutes to ensure that the solution is fully and uniformly absorbed by the primary carbon, and then drying the solution at the temperature of 110 ℃ for 1.8 hours to obtain secondary carbon.
(3) Fixing:
and (3) putting the secondary carbon into a muffle furnace, and burning for 2.5 hours at the temperature of 280 ℃ to obtain the modified activated carbon.
Example 4
(1) Preparing materials:
taking 100g of 8-30-mesh lamellar coconut shell activated carbon as base carbon, knowing that the saturated adsorption water quantity of the coconut shell activated carbon is M =830g/Kg, carrying out iron removal treatment on the base carbon by using a magnetic separator through a magnetic separation method, boiling for three times, and drying; weighing silver nitrate with the mass of 0.5 percent of the base carbon; weighing sodium carbonate with the mass of 0.2 percent of the base carbon;
(2) loading:
dissolving the silver nitrate in the step (1) in deionized water which is 1.1 times of the saturated adsorption water quantity M, adding base carbon, uniformly mixing, carrying out auxiliary treatment for 50 minutes by using 35KHz ultrasonic, turning over the base carbon every 10 minutes to ensure that the solution is fully and uniformly absorbed by the base carbon, and then carrying out vacuum drying for 1.5 hours at the temperature of 60 ℃ to obtain primary carbon; dissolving the sodium carbonate in the step (1) in deionized water which is 1.1 times of the saturated adsorption water quantity M, uniformly mixing the sodium carbonate with primary carbon, carrying out auxiliary treatment for 60 minutes by using 40KHz ultrasonic waves, turning over the mixture once every 10 minutes to ensure that the solution is fully and uniformly absorbed by the primary carbon, and then drying the mixture for 2 hours at the temperature of 120 ℃ to obtain secondary carbon.
(3) Fixing:
and (3) putting the secondary carbon into a muffle furnace, and burning for 5 hours at the temperature of 250 ℃ to obtain the modified activated carbon.
Example 5
(1) Preparing materials:
taking 100g of powdered coconut shell activated carbon with the particle size of less than 8 meshes and 5-10 meshes of coal activated carbon in a mass ratio of 1:1 as base carbon, knowing that the saturated adsorption water amount of the mixed activated carbon is M =1000g/Kg, carrying out iron removal treatment on the base carbon by using a magnetic separation method through a magnetic separator, carrying out three times of boiling and drying; weighing silver nitrate with the mass of 0.5 percent of the base carbon; weighing rubidium sulfate with the mass of 0.2 percent of the base carbon;
(2) loading:
dissolving the silver nitrate in the step (1) in deionized water which is 1 time of the saturated adsorption water quantity M, adding base carbon, uniformly mixing, performing auxiliary treatment for 50 minutes by using 10KHz ultrasonic, turning over the base carbon every 10 minutes to ensure that the solution is fully and uniformly absorbed by the base carbon, and then performing vacuum drying for 1.5 hours at the temperature of 60 ℃ to obtain primary carbon; dissolving the rubidium sulfate in the step (1) in deionized water which is 1 time of the saturated adsorption water quantity M, uniformly mixing the rubidium sulfate with primary carbon, carrying out auxiliary treatment for 10 minutes by using 20KHz ultrasonic waves, turning the rubidium sulfate once every 10 minutes to ensure that the solution is fully and uniformly absorbed by the primary carbon, and then drying the rubidium sulfate for 3 hours at the temperature of 50 ℃ to obtain secondary carbon.
(3) Fixing:
and (3) putting the secondary carbon into a muffle furnace, and burning for 1 hour at the temperature of 150 ℃ to obtain the modified activated carbon.
Example 6
(1) Preparing materials:
100g of 8-30 mesh layered coconut shell activated carbon is used as base carbon, and M =830g/Kg of saturated adsorption water amount of the coconut shell activated carbon is known as a blank control.
(2) Loading: is free of
(3) Fixing: is free of
Example 7
The preparation method of the modified activated carbon with high efficiency degerming in water is the same as that in example 4 except that sodium carbonate is replaced by sodium bicarbonate to be loaded with base carbon in the step (2).
The method comprises the following specific steps of (1) preparing materials:
taking 100g of 8-30-mesh lamellar coconut shell activated carbon as base carbon, knowing that the saturated adsorption water quantity of the coconut shell activated carbon is M =830g/Kg, carrying out iron removal treatment on the base carbon by using a magnetic separator through a magnetic separation method, boiling for three times, and drying; weighing silver nitrate with the mass of 0.5 percent of the base carbon; weighing sodium bicarbonate with the mass of 0.2 percent of the base carbon;
(2) loading:
dissolving the silver nitrate in the step (1) in deionized water which is 1.1 times of the saturated adsorption water quantity M, adding base carbon, uniformly mixing, carrying out auxiliary treatment for 50 minutes by using 35KHz ultrasonic, turning over the base carbon every 10 minutes to ensure that the solution is fully and uniformly absorbed by the base carbon, and then carrying out vacuum drying for 1.5 hours at the temperature of 60 ℃ to obtain primary carbon; and (2) dissolving the sodium bicarbonate in the step (1) in deionized water which is 1.1 times of the saturated adsorption water quantity M, uniformly mixing the sodium bicarbonate with the primary carbon, performing auxiliary treatment for 60 minutes by using 40KHz ultrasonic waves, turning over the sodium bicarbonate once every 10 minutes to ensure that the solution is fully and uniformly absorbed by the primary carbon, and drying the sodium bicarbonate at the temperature of 120 ℃ for 2 hours to obtain secondary carbon.
(3) Fixing:
and (3) putting the secondary carbon into a muffle furnace, and burning for 5 hours at the temperature of 250 ℃ to obtain the modified activated carbon.
Comparative example 1
The procedure was as in example 4 except that the fixation in step (3) was not performed.
The method comprises the following specific steps:
(1) preparing materials:
taking 100g of 8-30-mesh lamellar coconut shell activated carbon as base carbon, knowing that the saturated adsorption water quantity of the coconut shell activated carbon is M =830g/Kg, carrying out iron removal treatment on the base carbon by using a magnetic separator through a magnetic separation method, boiling for three times, and drying; weighing silver nitrate with the mass of 0.5 percent of the base carbon; weighing sodium carbonate with the mass of 0.2 percent of the base carbon;
(2) loading:
dissolving the silver nitrate in the step (1) in deionized water which is 1.1 times of the saturated adsorption water quantity M, adding base carbon, uniformly mixing, carrying out auxiliary treatment for 50 minutes by using 35KHz ultrasonic, turning over the base carbon every 10 minutes to ensure that the solution is fully and uniformly absorbed by the base carbon, and then carrying out vacuum drying for 1.5 hours at the temperature of 60 ℃ to obtain primary carbon; and (2) dissolving the sodium carbonate in the step (1) in deionized water which is 1.1 times of the saturated adsorption water quantity M, uniformly mixing the sodium carbonate with primary carbon, performing auxiliary treatment for 60 minutes by using 40KHz ultrasonic waves, turning the mixture once every 10 minutes to ensure that the solution is fully and uniformly absorbed by the primary carbon, and drying the solution at the temperature of 120 ℃ for 2 hours to obtain secondary carbon, namely the modified activated carbon of the comparative example.
(3) Fixing: does not perform the process
Comparative example 2
The procedure was as in example 4 except that the secondary loading of the base carbon with sodium carbonate was not carried out in step (2).
The method comprises the following specific steps:
(1) preparing materials:
taking 100g of 8-30-mesh lamellar coconut shell activated carbon as base carbon, knowing that the saturated adsorption water quantity of the coconut shell activated carbon is M =830g/Kg, carrying out iron removal treatment on the base carbon by using a magnetic separator through a magnetic separation method, boiling for three times, and drying; weighing silver nitrate with the mass of 0.5 percent of the base carbon; weighing sodium carbonate with the mass of 0.2 percent of the base carbon;
(2) loading:
dissolving the silver nitrate in the step (1) in deionized water which is 1.1 times of the saturated adsorption water quantity M, adding base carbon, uniformly mixing, carrying out auxiliary treatment for 50 minutes by using 35KHz ultrasonic, turning over the base carbon every 10 minutes to ensure that the solution is fully and uniformly absorbed by the base carbon, and then carrying out vacuum drying for 1.5 hours at the temperature of 60 ℃ to obtain primary carbon;
(3) fixing:
and (3) putting the primary carbon into a muffle furnace, and burning for 5 hours at the temperature of 250 ℃ to obtain the modified activated carbon.
Comparative example 3
The procedure was as in example 4 except that the secondary loading of the base carbon with sodium carbonate and the fixing in step (3) were not carried out in step (2).
The method comprises the following specific steps:
(1) preparing materials:
taking 100g of 8-30-mesh lamellar coconut shell activated carbon as base carbon, knowing that the saturated adsorption water quantity of the coconut shell activated carbon is M =830g/Kg, carrying out iron removal treatment on the base carbon by using a magnetic separator through a magnetic separation method, boiling for three times, and drying; weighing silver nitrate with the mass of 0.5 percent of the base carbon; weighing sodium carbonate with the mass of 0.2 percent of the base carbon;
(2) loading:
dissolving the silver nitrate in the step (1) in deionized water which is 1.1 times of the saturated adsorption water quantity M, adding base carbon, uniformly mixing, performing auxiliary treatment for 50 minutes by using 35KHz ultrasonic, turning over the base carbon every 10 minutes to ensure that the solution is fully and uniformly absorbed by the base carbon, and then performing vacuum drying for 1.5 hours at 60 ℃ to obtain primary carbon, namely the modified activated carbon of the comparative example;
(3) fixing: this process is not performed.
Comparative example 4
The procedure was as in example 4 except that the ultrasound-assisted treatment of step (2) was not performed.
(1) Preparing materials:
taking 100g of 8-30-mesh lamellar coconut shell activated carbon as base carbon, knowing that the saturated adsorption water quantity of the coconut shell activated carbon is M =830g/Kg, carrying out iron removal treatment on the base carbon by using a magnetic separator through a magnetic separation method, boiling for three times, and drying; weighing silver nitrate with the mass of 0.5 percent of the base carbon; weighing sodium carbonate with the mass of 0.2 percent of the base carbon;
(2) loading:
dissolving the silver nitrate in the step (1) in deionized water which is 1.1 times of the saturated adsorption water quantity M, adding base carbon, uniformly mixing, turning over the base carbon every 10 minutes to ensure that the solution is fully and uniformly absorbed by the base carbon, and then drying in vacuum at 60 ℃ for 1.5 hours to obtain primary carbon; and (2) dissolving the lithium chloride in the step (1) in deionized water which is 1.1 times of the saturated adsorption water quantity M, uniformly mixing the lithium chloride with the primary carbon, turning the lithium chloride once every 10 minutes to ensure that the solution is fully and uniformly absorbed by the primary carbon, and drying the lithium chloride for 2 hours at the temperature of 120 ℃ to obtain secondary carbon.
(3) Fixing:
and (3) putting the secondary carbon into a muffle furnace, and burning for 5 hours at the temperature of 250 ℃ to obtain the modified activated carbon.
Comparative example 5
The procedure was as in example 4 except that the firing in step (3) was carried out at 320 ℃.
The method comprises the following steps:
(1) preparing materials:
taking 100g of 8-30-mesh lamellar coconut shell activated carbon as base carbon, knowing that the saturated adsorption water quantity of the coconut shell activated carbon is M =830g/Kg, carrying out iron removal treatment on the base carbon by using a magnetic separator through a magnetic separation method, boiling for three times, and drying; weighing silver nitrate with the mass of 0.5 percent of the base carbon; weighing sodium carbonate with the mass of 0.2 percent of the base carbon;
(2) loading:
dissolving the silver nitrate in the step (1) in deionized water which is 1.1 times of the saturated adsorption water quantity M, adding base carbon, uniformly mixing, carrying out auxiliary treatment for 50 minutes by using 35KHz ultrasonic, turning over the base carbon every 10 minutes to ensure that the solution is fully and uniformly absorbed by the base carbon, and then carrying out vacuum drying for 1.5 hours at the temperature of 60 ℃ to obtain primary carbon; dissolving the lithium chloride in the step (1) in deionized water which is 1.1 times of the saturated adsorption water quantity M, uniformly mixing the lithium chloride with primary carbon, carrying out auxiliary treatment for 60 minutes by using 40KHz ultrasonic waves, turning over the lithium chloride once every 10 minutes to ensure that the solution is fully and uniformly absorbed by the primary carbon, and then drying the lithium chloride for 2 hours at the temperature of 120 ℃ to obtain secondary carbon.
(3) Fixing:
and (3) putting the secondary carbon into a muffle furnace, and burning for 5 hours at the temperature of 295 ℃ to obtain the modified activated carbon.
Comparative example 6
According to the experiment of example 1 in Chinese patent 'a high-load nano silver activated carbon and preparation method thereof' (Chinese patent application No. CN 201510832329.9), the specific steps are as follows:
taking 1kg of freshly prepared flaky coconut shell activated carbon, grinding, sieving with a 80-mesh sieve, and washing with 5 kg of pure water for multiple times until a washing solution is clear and colorless; drying at 100-140 ℃ to constant weight, cooling to room temperature in a dryer, and recording as coconut shell activated carbon AC-0; adding 1kg of coconut shell activated carbon into 30% hydrogen peroxide under stirring at 180rpm, maintaining stirring at room temperature for 5-8 hours, and filtering out the activated carbon; repeatedly pumping and washing 5 kg of pure water in batches until the washing liquid is colorless and neutral, wherein the conductivity of the washing liquid is low and the washing liquid is dried by 20.0 mu s/cm; drying the modified coconut shell activated carbon at 100-140 ℃ to constant weight, cooling to room temperature in a dryer, and recording as coconut shell activated carbon AC-1.
Preparing 20nm nano silver particles by taking a silver-ammonia solution as a precursor, maltose as a reducing agent and a glucan protective agent in an environment of 40-50 ℃; performing high-speed centrifugation, washing with pure water for 5 times, and washing with anhydrous ethanol for 5 times; then, re-dispersing the nano-silver material in pure water under stirring, adding 5% dextran, performing ultrasonic intensity of 0.5W/mL (ultrasonic 10 seconds, intermittent 5 seconds), stirring at a rotating speed of 200rpm, dispersing for 2 hours, and controlling the temperature not to exceed 40 ℃ in the whole process; finally, obtaining uniform nano silver colloid solution as a nano silver medium A.
The following tests were carried out on the activated modified carbons of examples 1 to 5, example 7, and comparative examples 1 to 5, the base carbon of example 6, and the nano silver colloidal solution of comparative example 6, and the obtained results were shown in the following table.
The test methods of the above examples and comparative examples are as follows:
silver loading rate: the content of silver in the modified activated carbon is detected by ICP-MC, and the unit is accurate to ppm.
The silver loss rate was measured as follows:
taking 80g of the product (modified activated carbon, base carbon or nano silver colloidal solution) finally obtained in the specific embodiment, and taking 20g as A1; boiling and washing the rest 60g of charcoal for 2 times and washing for 4 times, (boiling and washing for 1 time, washing for 2 times, boiling and washing for 1 time and washing for 2 times), and drying at 120 ℃, and taking 20g of charcoal as A2; boiling and washing the rest 40g of charcoal for 2 times and washing for 4 times, (boiling and washing for 1 time, washing for 2 times, boiling and washing for 1 time, washing for 2 times) drying at 120 ℃, and taking 20g of charcoal as A3; the remaining 20g of charcoal was boiled and washed 2 times and 4 times, (boiled and washed 1 time, washed 2 times, boiled and washed 1 time, washed 2 times) and dried at 120 ℃ as A4.
The silver content of A1-A4 was measured by ICP-MC, respectively, and the leaching rate was calculated by the following formula. (where n.gtoreq.1, An is the silver content of sample An, where stream n is the silver loss rate from the washing of one time. n =4 in the present embodiment)
Stream n = (An-An +1)/An × 100%
The sample loss rate = (stream 1+ … + stream n)/n.
And (4) calculating the removal rate of total coliform bacteria and the removal rate of staphylococcus aureus (viable count) according to MOH (Standard for evaluating health safety and function of water quality processors for domestic Drinking Water) and GB/T5750.12-2006 Standard test method for domestic Drinking Water microbial standards.
From the data in the above table, it is seen that in example 4, the silver loading amount of the modified activated carbon is decreased and the silver leaching rate is greatly increased compared to comparative example 1 in which comparative example 1 is not fixed.
Compared with the comparative example 2, the comparative example 2 does not carry out secondary loading, namely, does not add alkali metal salt for treatment, and the loading amount of the modified activated carbon silver is greatly reduced. As can be seen from example 4 and comparative example 2, the secondary loading treatment with sodium carbonate reacted with the silver nitrate loaded on the carbon surface at the primary loading to produce silver carbonate, which was insoluble in water and quite stable at room temperature and in air, but the leaching rate on the activated carbon surface was still quite high.
Compared with the comparative example 3, the comparative example 3 does not carry out fixation or add alkali metal salt for treatment, the loading amount of the modified activated carbon silver is greatly reduced, and the loss rate of the silver is greatly increased. As can be seen from examples 1 to 4 and comparative example 3, silver nitrate has the effects of etching and killing germs and has a very good convergence effect, but the loss rate of silver loaded on the surface of modified activated carbon is very high, which leads to cost increase and secondary pollution.
Example 4 compared to comparative example 4, comparative example 4 did not perform the ultrasonic assist and the silver loading was reduced. As can be seen from example 4 and comparative example 4, treatment with suitable ultrasound in the loading can enhance the stability of silver on the surface of activated carbon, increase the loading amount of silver and reduce the leaching rate of silver.
Example 4 compared with comparative example 5, the burning temperature in comparative example 5 was 320 ℃, and the silver loss rate was increased above the range of claims. Experiments show that the silver oxide is firmly bonded with functional groups on the surface of the active carbon and is not easy to run off, but the silver oxide is decomposed into simple substance silver and oxygen when being heated to more than 300 ℃, and the firmness of the simple substance silver on the surface of the active carbon is obviously reduced compared with that of the silver oxide.
Example 4 compared with comparative example 6, in comparative example 6, the experiment of example 1 using "a highly loaded nano-silver activated carbon and a method for preparing the same" (application number: CN 201510832329.9) significantly increased the silver loss rate of comparative example 6.
As is clear from examples 4 and 7, the secondary loading of sodium carbonate can improve the loading rate of silver as compared with the use of other alkali metal solutions.
Claims (8)
1. A preparation method of modified activated carbon for efficiently removing bacteria in water is characterized by comprising the following steps: the method comprises the following steps:
preparing materials:
according to the carbon base: silver nitrate: the mass ratio of the alkali metal salt is 100: 0.1-0.5: 0.05-0.3 preparing base carbon, silver nitrate and alkali metal salt;
loading:
measuring the saturated adsorption water quantity M of the base carbon, and taking deionized water which is 1-1.5 times of the saturated adsorption water quantity M; dissolving silver nitrate in the step (1) in the deionized water, adding base carbon, uniformly mixing, performing auxiliary treatment for 10-60 minutes by using ultrasonic waves of 20-40 kHz, and performing vacuum drying for 0.5-2 hours at the temperature of 50-80 ℃ to obtain primary carbon;
dissolving the alkali metal salt in the step (1) in deionized water which is 1-1.5 times of the saturated adsorption water quantity M, uniformly mixing the alkali metal salt with the primary carbon, performing auxiliary treatment for 10-60 minutes by using ultrasonic waves of 20-40 kHz, and drying for 0.5-3 hours at the temperature of 50-150 ℃ to obtain secondary carbon;
fixing:
and (3) putting the secondary carbon into a muffle furnace, and burning for 1-5 hours at the temperature of 150-295 ℃ to obtain the modified activated carbon.
2. The preparation method of the modified activated carbon for efficiently removing bacteria in water according to claim 1, which is characterized by comprising the following steps: the base carbon in the step (1) is conventional activated carbon.
3. The preparation method of the modified activated carbon for efficiently removing bacteria in water according to claim 2, which is characterized by comprising the following steps: the conventional activated carbon is one or more of coal activated carbon, wood activated carbon, shell activated carbon and coconut shell activated carbon.
4. The preparation method of the modified activated carbon for efficiently removing bacteria in water according to claim 2, which is characterized by comprising the following steps: the conventional activated carbon is one or more of granular, powdery, lamellar or amorphous.
5. The preparation method of the modified activated carbon for efficiently removing bacteria in water according to claim 1, which is characterized by comprising the following steps: and (2) carrying out iron removal treatment on the base carbon in the step (1), washing and boiling for three times, and drying.
6. The preparation method of the modified activated carbon for efficiently removing bacteria in water according to claim 1, which is characterized by comprising the following steps: the alkali metal salt in the step (1) is soluble salt containing one metal ion of Li, Na, K and Rb.
7. The preparation method of the modified activated carbon for efficiently removing bacteria in water according to claim 6, which is characterized by comprising the following steps: the soluble salt is one or more of acid salt, sulfate, nitrate, carbonate and bicarbonate.
8. The preparation method of the modified activated carbon for efficiently removing bacteria in water according to claim 1, which is characterized by comprising the following steps: the saturated adsorbed water amount M in the step (2) is measured according to the following operations: weighing 1Kg of base carbon to be detected, adding water, metering M0, stirring uniformly to realize full adsorption, then weighing the mass M1 of filtrate after suction filtration, deducting the mass to obtain the adsorbed water quantity Mn, namely Mn = M0-M1, repeatedly measuring for several times, and taking the average value of Mn to obtain the saturated adsorption water quantity M of the base carbon to be detected.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114618473A (en) * | 2022-03-25 | 2022-06-14 | 北京林业大学 | Preparation method of modified activated carbon used as ester polymerization catalyst |
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