CN110075802B - Iron oxide loaded activated carbon and synthesis method and application thereof - Google Patents
Iron oxide loaded activated carbon and synthesis method and application thereof Download PDFInfo
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Abstract
The invention belongs to the field of water treatment, and discloses iron oxide loaded activated carbon and a synthesis method and application thereof. The synthesis method comprises the following steps: and (3) dipping the activated carbon in an aqueous solution of an iron source, carrying out ultrasonic treatment, then evaporating to dryness and roasting to obtain the iron oxide loaded activated carbon. The synthesis method brings Fe load, Fe-O-C bond generation and fiber filamentous structure formation in the pore channel; the active carbon has large specific surface area, organic pollutants are more fully adsorbed in the pore canal of the active carbon, the extracellular electron transfer rate of the attached and growing microorganism is accelerated, and the formation of a biological film is promoted. The invention not only reduces the disinfection by-products and pathogenic microorganisms in the factory water, but also has the function of inhibiting the generation of the disinfection by-products and the regrowth of the pathogenic microorganisms in the subsequent tap water pipe network.
Description
Technical Field
The invention belongs to the field of water treatment, and particularly relates to iron oxide loaded activated carbon and a synthesis method and application thereof.
Background
In recent years, the microbiological problem of drinking water networks has been receiving social attention. Generally, tap water of residential users has significantly deteriorated water quality due to the regrowth of microorganisms in the pipe network, as compared with the outgoing water of water works. To reduce this hazard, chlorine disinfectants were introduced in the 20 th century because of their lower cost and continued disinfection by maintaining a certain residual chlorine concentration throughout the network. However, chlorine disinfectants can react with natural organic materials in the water to produce a series of harmful disinfection by-products such as trihalomethanes and haloacetic acids, which are carcinogenic to humans.
Recently, the large number of growth of opportunistic pathogens such as Mycobacterium avium, Legionella pneumoniae and Hartmanella vermiformis in drinking water networks has become a new focus of public attention. Unlike intestinal microorganisms which are easily killed by chlorine disinfectants, conditionally pathogenic bacteria can survive well in the network, amplify and reproduce even at very high disinfectant concentrations, as they have a range of advantages including ease of biofilm formation, production of large amounts of extracellular polymers, anti-oligotrophism, etc.
In order to improve the quality of drinking water, the ozone-biological activated carbon combined process is widely applied as an advanced treatment means of a drinking water plant. Ozone has been proved to oxidize and disinfect the precursor of the by-product, remove odor substances, inactivate pathogenic microorganisms and improve the biodegradability of organic matters, and simultaneously, the ozone plays a role in promoting the microbial metabolic activity of the subsequent biological activated carbon. The biological activated carbon can obviously remove organic pollutants and disinfection by-product precursors, and simultaneously entrap most pathogenic bacteria.
However, the ozone-biological activated carbon combined technology has certain defects, such as the process of ozone oxidation of organic matters can form new precursors of disinfection byproducts. While the biological activated carbon can effectively remove organic pollutants, the fallen biological membrane and soluble microbial metabolites can also be used as precursors of disinfection byproducts, and the latter can cause harm to human bodies. In addition, the fallen biological membrane contains a large amount of pathogenic microorganisms, and the mature biological membrane structure plays a role in protecting the microorganisms, is difficult to inactivate by a chlorine disinfectant after entering the pipe network and can be regrown. Although most microorganisms in tap water are inactivated after chlorination, pathogenic microorganisms in tap water are not effectively controlled after the tap water is transported and distributed through a pipe network, and disinfection byproducts are generated continuously. If the transition metal oxide can be loaded on the surface of the active carbon for modification, the metal oxygen bond is formed to enhance the complexation of organic matters and the extracellular electron transfer rate of microorganisms, the structure of the biological membrane on the surface of the active carbon is more excellent, the organic matters, the form of the biological membrane and the structure of microbial communities in the effluent of the active carbon are improved, and the water quality stability in a subsequent pipe network is further ensured, so that the problems of disinfection by-products and pathogenic microorganisms of tap water can be solved simultaneously.
Disclosure of Invention
In order to overcome the disadvantages and shortcomings of the prior art, the invention provides a method for synthesizing iron oxide-supported activated carbon. The method takes common activated carbon as a matrix, and synthesizes the target novel activated carbon through three steps of dipping into an iron source, evaporating and calcining.
The invention also aims to provide the iron oxide-loaded activated carbon prepared by the method, and the synthesis method brings about the loading of Fe, the generation of Fe-O-C bonds and the formation of fibrous filiform structures in the pore channels; the active carbon has large specific surface area, organic pollutants are more fully adsorbed in the pore canal of the active carbon, the extracellular electron transfer rate of the attached and growing microorganism is accelerated, and the formation of a biological film is promoted.
Still another object of the present invention is to provide the use of the above-mentioned iron oxide-loaded activated carbon for inhibiting disinfection by-products and pathogenic microorganisms in the outlet water of a tap water pipe network, which is not possessed by the activated carbon with a conventional inhibiting effect.
The purpose of the invention is realized by the following scheme:
a synthetic method of iron oxide supported activated carbon comprises the following steps: and (3) dipping the activated carbon in an aqueous solution of an iron source, carrying out ultrasonic treatment, then evaporating to dryness and roasting to obtain the iron oxide loaded activated carbon.
The activated carbon is one of coconut shell activated carbon, coal activated carbon, wood activated carbon and bamboo activated carbon, and is preferably coconut shell activated carbon;
the diameter of the activated carbon is 0.5-3 mm, and preferably 1.2 mm;
the iron source is ferric chloride hexahydrate (FeCl)3·6H2O) and ferric nitrate nonahydrate (FeNO)3·9H2O), preferably hexahydrateFerric chloride (FeCl)3·6H2O)；
The concentration of the iron source water solution is 15-25 g/L, and preferably 20 g/L.
The dosage of the active carbon and the iron source water solution meets the following requirements: soaking every 1g of activated carbon in (2-4) mL of iron source aqueous solution correspondingly, preferably soaking every 1g of activated carbon in 3mL of iron source aqueous solution correspondingly;
the ultrasonic treatment is ultrasonic treatment at 300W power for 0.5-1.5 hours, preferably ultrasonic treatment at 300W power for 1 hour. The ultrasonic treatment mainly promotes iron salt to be dispersed in developed pores of the active carbon, is beneficial to the formation of fiber filamentous iron oxide in the pore canal, is indispensable in structure, remarkably enhances the sites of organic matter adsorption and microorganism attachment growth, and improves the extracellular electron transfer rate of the microorganism.
The drying by distillation refers to drying by distillation at 75-95 ℃;
the temperature rise rate of the roasting is less than 20 ℃/min, and preferably 5 ℃/min; the roasting temperature is 200-400 ℃, and preferably 300 ℃; the roasting time is 0.5-2 h, preferably 1 h;
the method is characterized in that the activated carbon further comprises a pretreatment step before being dipped into an aqueous solution of an iron source, wherein the pretreatment aims at removing impurities and activating surface groups of the activated carbon, so that a surface carbon material and iron oxide are bonded in a synthesis process, and Fe-O-C bonds are indispensable. The pretreatment step specifically comprises the following steps: sequentially dipping the activated carbon in an alkaline aqueous solution and an acidic aqueous solution, washing with water, and drying for later use;
the alkaline aqueous solution is preferably 50-150 g/L sodium hydroxide aqueous solution, and is preferably 100g/L sodium hydroxide aqueous solution; the time for soaking in the alkaline aqueous solution is 0.5-2 h; after soaking in the alkaline aqueous solution, the water is preferably used for washing, and then the soaking is carried out in the acidic aqueous solution.
The acidic aqueous solution is preferably HNO with the concentration of 5-15% (v/v)3An aqueous solution, preferably 10% (v/v) HNO3An aqueous solution; the soaking time in the acidic aqueous solution isIs 0.5 to 2 hours;
the drying is preferably performed at 100-200 ℃, and is preferably performed at 160 ℃.
An iron oxide-loaded activated carbon prepared by the method. The iron oxide-loaded activated carbon prepared by the method is still black solid particles, and the appearance of the activated carbon is not different from that of common activated carbon; the microstructure is formed by forming a filamentous iron oxide structure in a pore canal developed by active carbon. The iron enters into the structural framework on the surface of the active carbon to form Fe-O-C bonds. The iron oxide loaded active carbon has larger specific surface area, organic pollutants are more fully adsorbed in the pore canal of the active carbon, and the extracellular electron transfer rate of the microorganism attached and grown is accelerated.
The iron oxide loaded active carbon is applied to inhibiting disinfection byproducts and pathogenic microorganisms in drinking water and tap water pipe network outlet water.
The disinfection by-products may include trihalomethanes and haloacetic acids; the pathogenic microorganism comprises legionella pneumophila, mycobacterium avium, and formica furiosa.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) the iron oxide-loaded activated carbon has higher removal rate on the precursor of the disinfection by-product.
(2) The active carbon has a more excellent pore structure and a large specific surface area, a fibrous filamentous structure is formed in a pore channel, active components of the active carbon are greatly exposed on the surface of the active carbon, and adsorption sites of organic matters are greatly increased.
(3) The invention can not generate heavy metal pollution in the using process.
(4) The microbial metabolism activity of the surface of the active carbon is higher, and the structure of a biological membrane is more developed.
(5) The activated carbon of the invention releases fewer microorganisms during biodegradation of organic pollutants and has a smaller scale of biofilm.
(6) The iron oxide-loaded active carbon effluent has fewer organic matters and disinfection by-product precursors, and a suspended biological film in an effluent water body has smaller size and is easier to inactivate by a disinfectant. Therefore, the invention not only reduces the disinfection by-products and pathogenic microorganisms in the factory water, but also has the function of inhibiting the generation of the disinfection by-products and the regrowth of the pathogenic microorganisms in the subsequent tap water pipe network.
Drawings
FIG. 1 is an SEM picture of Fe/CAC prepared in example 1 and of the raw material CAC.
FIG. 2 is the Fe/CAC prepared in example 1 and the N of the raw material CAC2Adsorption and desorption isotherms.
FIG. 3 is an XRD spectrum of Fe/CAC prepared in example 1 and of the starting material CAC.
FIG. 4 is an infrared spectrum of Fe/CAC prepared in example 1 and of the raw material CAC.
FIG. 5 is the O1s XPS spectra of the Fe/CAC prepared in example 1 and the feedstock CAC.
FIG. 6 is a graph of the formation of trihalomethanes and haloacetic acids in simulated tube-network effluent using Fe/CAC prepared in example 1 and a control activated carbon support (plain CAC).
FIG. 7 is a graph of conditioned pathogen conditions simulating the tapping of a pipe network under Fe/CAC prepared in example 1 and a control activated carbon support (plain CAC).
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the embodiments of the present invention are not limited thereto.
The reagents used in the examples are commercially available without specific reference.
Example 1
The invention relates to a synthesis method of iron oxide loaded coconut shell activated carbon Fe/CAC, which comprises the following steps:
(1) immersing coconut shell activated carbon (CAC) having an average particle size of 1.2mm in 100g/L sodium hydroxide solution (NaOH) for 1 hour;
(2) the coconut shell activated carbon was taken out and washed with deionized water, and then immersed in a 10 vol% nitric acid aqueous solution (HNO)3)1 hour;
(3) and taking out the coconut shell activated carbon, repeatedly washing the coconut shell activated carbon with deionized water for 5 times, and drying the coconut shell activated carbon in an oven at 160 ℃ for later use.
(4) Ferric chloride hexahydrate (FeCl)3·6H2O) dissolving the mixture into deionized water to form a solution A with the concentration of 20 g/L;
(5) mixing the solution A and pretreated coconut shell activated carbon in a ratio of 3mL to 1.0g, carrying out ultrasonic treatment at 300W power for 1 hour, and heating in a water bath at 85 ℃ until the liquid is evaporated to dryness;
(6) and roasting the coconut shell activated carbon subjected to water bath evaporation for 1 hour at 300 ℃ in a muffle furnace, and naturally cooling to obtain the final iron oxide loaded novel coconut shell activated carbon Fe/CAC.
FIG. 1 is an SEM picture of Fe/CAC prepared in example 1 and of the raw material CAC. The Fe/CAC has the grain diameter of about 1-2 mm, a developed pore structure and a fiber-like structure in a pore channel.
FIG. 2 is the Fe/CAC prepared in example 1 and the N of the raw material CAC2Adsorption and desorption isotherm, the specific surface area of the CAC of the raw material is 641.09m as determined by BET2g-1The Fe/CAC has a larger specific surface area of about 680m2g-1. By EDS spectroscopy, the Fe/CAC has a surface Fe content of 3.33 wt% and a bulk iron content of about 1.25 wt%, indicating that a large number of Fe sites are exposed on the activated carbon surface.
FIG. 3 is an XRD spectrum of Fe/CAC prepared in example 1 and of the starting material CAC. It can be seen from the figure that the Fe/CAC surface-supported iron oxide is mainly Fe2O3The carbon substance exists mainly in the form of graphitized carbon.
FIG. 4 is an infrared spectrum of Fe/CAC prepared in example 1 and of the raw material CAC, which shows 544cm after the coconut shell activated carbon is surface-loaded with iron-1And 474cm-1Two new peaks of Fe2O3The characteristic peak of Fe-O bond in (1) is in accordance with the above XRD results.Furthermore, 1701cm newly appeared-1Characteristic peaks, representing C-O bonds in carboxylic acid and ketone structures. Represents CH22924cm for asymmetric and symmetric stretching vibration-1And 2860cm-1The peak intensity is reduced, which shows that the C-O-H bond on the surface of the activated carbon is increased. 3480cm-1The hydroxyl group moves to 3425cm-1It is shown that iron loading introduces Fe-O-H in addition to C-O-H, thus causing a shift in hydroxyl peak.
FIG. 5 is the O1s XPS spectra of the Fe/CAC prepared in example 1 and the feedstock CAC. From the figure it can be seen that the iron species of the Fe/CAC surface are bound to the activated carbon surface by Fe-O-C bonds and the presence of Fe-O-Fe and Fe-O-H is further confirmed.
Application examples
The effluent from the sand filter was taken from a waterworks and first treated with ozone and then passed into a fixed bed loaded with activated carbon for a retention time of 30 minutes. After the water body is treated by the activated carbon loaded by the iron oxide, chlorination disinfection is carried out, the disinfectant is sodium hypochlorite, and then the water body enters a chlorine reaction tank for 4 hours. The effluent of the chlorine reaction tank enters a simulated tap water pipe network. (the process conditions of ozone treatment and active carbon treatment are parameters commonly used in actual waterworks, the adding dose of ozone is 1.0mg/L, and the retention time and the filtration rate of active carbon are respectively 30 minutes and 10 meters per hour.)
FIG. 6 is a graph of the formation of trihalomethanes and haloacetic acids (test methods are all U.S. EPA standard methods) for simulated tube-network effluent using Fe/CAC prepared in example 1 and a control activated carbon support (plain CAC). As shown in FIG. 6, the simulated ductwork effluent had trihalomethane concentrations of 8.46ug/L and 2.15ug/L, respectively, and haloacetic acid concentrations of 28.45ug/L and 10.55ug/L, respectively, with the use of CAC and Fe/CAC. Obviously, the active carbon loaded with the iron oxide prepared by the method obviously inhibits trihalomethane and haloacetic acid in the outlet water of a pipe network, and reduces the risk of disinfection byproducts in tap water.
FIG. 7 is a graph of conditioned pathogen conditions simulating the tapping of a pipe network under Fe/CAC prepared in example 1 and a control activated carbon support (plain CAC). As shown in fig. 7, prepared using example 1In the case of Fe/CAC, the gene copy numbers of Legionella, Mycobacterium and Gliaca are respectively reduced to 1.18 log, 0.97 log and 0 log per milliliter of water body on the genus level. And legionella pneumophila, mycobacterium avium and formica furiosa were inactivated at the species level determined to be pathogenic. In addition, the Fe/CAC iron release was very low throughout the reaction, below 0.1mg L-1And the iron itself is non-toxic and harmless. Therefore, the Fe/CAC effectively inhibits disinfection byproducts and pathogenic microorganisms in a pipe network and ensures the water quality safety of the tap water.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (8)
1. The application of the iron oxide loaded activated carbon in inhibiting disinfection byproducts and pathogenic microorganisms in drinking water and tap water pipe network outlet water is characterized in that the iron oxide loaded activated carbon is prepared by the following steps: and (3) dipping the activated carbon in an aqueous solution of an iron source, carrying out ultrasonic treatment, then evaporating to dryness and roasting to obtain the iron oxide loaded activated carbon.
2. The use of the iron oxide-loaded activated carbon of claim 1 for inhibiting disinfection by-products and pathogenic microorganisms in drinking water and tap water pipe network effluent, wherein:
the active carbon is one of coconut shell active carbon, coal active carbon, wood active carbon and bamboo active carbon;
the iron source is one of ferric chloride hexahydrate and ferric nitrate nonahydrate.
3. The use of the iron oxide-loaded activated carbon of claim 1 for inhibiting disinfection by-products and pathogenic microorganisms in drinking water and tap water pipe network effluent, wherein:
the active carbon is coconut shell active carbon;
the iron source is ferric chloride hexahydrate.
4. The use of the iron oxide-loaded activated carbon of claim 1 or 2 for inhibiting disinfection by-products and pathogenic microorganisms in drinking water and tap water pipe network effluent, characterized in that:
the concentration of the iron source water solution is 15-25 g/L;
the dosage of the active carbon and the iron source water solution meets the following requirements: every 1g of activated carbon is correspondingly soaked in (2-4) mL of iron source water solution.
5. The use of the iron oxide-loaded activated carbon of claim 1 or 2 for inhibiting disinfection by-products and pathogenic microorganisms in drinking water and tap water pipe network effluent, characterized in that:
the concentration of the iron source water solution is 20 g/L;
the dosage of the active carbon and the iron source water solution meets the following requirements: each 1g of the activated carbon was soaked in 3mL of an aqueous iron source solution.
6. The use of the iron oxide-loaded activated carbon of claim 1 or 2 for inhibiting disinfection by-products and pathogenic microorganisms in drinking water and tap water pipe network effluent, characterized in that:
the ultrasonic treatment is ultrasonic treatment at 300W power for 0.5-1.5 hours;
the drying by distillation refers to drying by distillation at 75-95 ℃;
the temperature rise rate of the roasting is less than 20 ℃/min; the roasting temperature is 200-400 ℃; the roasting time is 0.5-2 h.
7. The use of the iron oxide-loaded activated carbon of claim 1 for inhibiting disinfection by-products and pathogenic microorganisms in drinking water and tap water pipe network effluent, wherein:
before the activated carbon is immersed in the aqueous solution of the iron source, the activated carbon further comprises a pretreatment step, and the pretreatment step specifically comprises the following steps: sequentially dipping the activated carbon in an alkaline aqueous solution and an acidic aqueous solution, washing with water, and drying for later use;
the alkaline aqueous solution is 50-150 g/L sodium hydroxide aqueous solution, and the time for soaking in the alkaline aqueous solution is 0.5-2 h;
the acidic aqueous solution is HNO with the volume concentration of 5-15 percent3The water solution is soaked in the acidic water solution for 0.5-2 hours;
the drying is drying at 100-200 ℃.
8. The use of the iron oxide-loaded activated carbon of claim 1 for inhibiting disinfection by-products and pathogenic microorganisms in drinking water and tap water pipe network effluent, wherein:
the disinfection by-products comprise trihalomethane and haloacetic acid; the pathogenic microorganism comprises legionella pneumophila, mycobacterium avium and formica furiosa.
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| CN113262758A (en) * | 2021-06-02 | 2021-08-17 | 重庆交通大学 | Preparation method and application of trivalent manganese modified biomass charcoal |
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