CN114100590A - Molybdenum disulfide activated carbon fiber composite adsorbent for deep purification of lead-containing wastewater and preparation method thereof - Google Patents
Molybdenum disulfide activated carbon fiber composite adsorbent for deep purification of lead-containing wastewater and preparation method thereof Download PDFInfo
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- C02F2303/16—Regeneration of sorbents, filters
Abstract
The invention provides a molybdenum disulfide activated carbon fiber composite adsorbent for deeply purifying lead-containing wastewater and a preparation method thereof. The composite adsorbent has a "sandwich" multilayer structure: the activated carbon fiber is used as a carrier, the polydopamine coating is arranged in the middle, and the compact molybdenum disulfide nanosheet is arranged on the outermost layer. The invention solves the technical bottleneck that the nano-grade molybdenum disulfide powder is difficult to separate solid from liquid in practical engineering application, takes the activated carbon fiber with larger specific surface area and length-diameter ratio as a carrier, and combines the activated carbon fiber with molybdenum disulfide nanosheets with excellent adsorption selectivity to lead ions by utilizing the mediation of polydopamine, thereby improving the availability of the molybdenum disulfide nanomaterial. The material has high adsorption capacity to lead ions in water, the adsorption reaction kinetics is rapid, the material can be stably used in a fixed bed flow system, the material with saturated adsorption can be desorbed and regenerated, the aim of repeated use is achieved, and the material has wide application prospect in the advanced treatment of lead-containing wastewater.
Description
Technical Field
The invention belongs to the field of drinking water and industrial wastewater advanced treatment and novel composite adsorption material preparation, and particularly relates to a molybdenum disulfide activated carbon fiber composite adsorbent for deeply purifying lead-containing wastewater and a preparation method thereof.
Background
With the rapid development of the industries such as metallurgy, chemical engineering, coating printing, electroplating and the like in China in recent years, a large amount of wastewater containing heavy metal compounds is discharged into natural waters, so that ecological safety and the health of the masses of people are greatly harmed. Among them, lead, one of the most toxic and harmful heavy metals, is hardly degraded in natural environment, has bio-enrichment property, and can be accumulated layer by layer through food chain in natural environment. How to efficiently and deeply purify lead-containing wastewater is a problem which needs to be solved urgently.
The adsorption technology is one of the most widely used technologies for treating the lead-containing wastewater due to simple operation, high efficiency and low cost, the conventional adsorbents currently applied to the treatment of the lead-containing wastewater comprise porous zeolite, clay, activated carbon and the like, and the adsorbents are widely applied due to low price, easy material obtaining and simple preparation, but have low adsorption quantity and poor selectivity and have limitation on the deep treatment of the lead-containing wastewater.
In recent years, molybdenum disulfide (MoS)2) As a typical layered transition metal sulfide, it is considered to be a promising heavy metal ion adsorbent due to its unique structure and stable physicochemical properties. The molybdenum disulfide has a layered structure, and each layer of the molybdenum disulfide consists of a central Mo atom which is connected with an upper layer S atom and a lower layer S atom through covalent bonds. The particularity of this structure provides a high specific surface area and a large number of exposed sulfur atoms. The exposed sulfur atoms have strong affinity to heavy metal ions, and can selectively remove the heavy metal ions such as lead and the like from the wastewater with complex components, thereby being quickly and quickly applied to the deep purification of the lead-containing wastewater. However, the molybdenum disulfide prepared in the laboratory is usually nano-sized or micron-sized particles, and is easy to agglomerate in practical water treatment application, difficult to separate and recover and applied to practical water treatment applicationThe resistance in the fluid processing systems such as the fixed bed and the like is large, so that the practical application of the fluid processing systems in a large scale is limited. To solve these engineering application short plates, one solution is to combine molybdenum disulfide with magnetic material (application No. CN201610225999.9, a petal-shaped MoS2-Mn3O4The preparation method and the application of the nanowire magnetic composite material), the method for recovering the adsorbent from the liquid phase by utilizing magnetism is an ideal method, but the operation cost is greatly improved by using electromagnetic separation, the wastewater treatment cost is increased, and the metal oxide is easy to run off in the acidic liquid phase to cause secondary pollution.
Another common strategy is to grow nano-sized molybdenum disulfide in situ in the pore channels of the large-sized porous carrier by a precursor introduction-pore nucleation "method. However, this preparation method is liable to cause the carrier pore channel to be blocked, leading to the loss of active sites and the decrease of adsorption kinetics, thereby affecting the adsorption performance of the composite material. To avoid such problems, an effective method is to select a material with a large specific surface area as a carrier (such as biochar, fiber, etc.) and fix molybdenum disulfide on the surface, thereby effectively increasing MoS2Utilization and reaction kinetics. The activated carbon fiber as a carrier material has excellent mechanical strength, stable chemical properties, and extremely large specific surface area and length-diameter ratio, and is an excellent nano adsorbent carrier. However, inorganic MoS2Lack of stable acting force between the activated carbon fiber and the organism, and directly react MoS2The active carbon fibers coated on the active carbon fibers are easy to lose in a fluid system. Polydopamine (PDA) is a material with super-strong adhesion characteristics, and researches show that a polydopamine coating can be formed on the surfaces of various materials by utilizing the reaction mechanism of oxidative autopolymerization of dopamine in an oxygen-containing weak alkaline aqueous solution, and the coating can provide a large number of phenolic hydroxyl active sites for a base material, so that a nano adsorbent is fixed on the surface of a carrier. The research that a layer of molybdenum disulfide nanosheet is fixed on the surface of the activated carbon fiber by utilizing polydopamine to prepare the adsorbent and the adsorbent is used for treating the lead-containing wastewater has not been reported yet. Thus, the use of a polydopamine-like material with superior adhesion to enhance the interaction between the carrier and the nanoparticle adsorbentThe method can provide a scheme for solving the problem of unstable combination between the inorganic nanometer component and the carrier in the nanometer composite adsorbent.
Disclosure of Invention
Aiming at the problems that the existing nano-grade molybdenum disulfide is easy to agglomerate in water and difficult to recover, and cannot be applied to water treatment devices such as fixed beds, and the like, the invention provides a molybdenum disulfide activated carbon fiber composite adsorbent for deeply purifying lead-containing wastewater and a preparation method thereof. The nano-molybdenum disulfide is attached to the surface of the activated carbon fiber through the mediation of polydopamine to prepare a micron-level or even millimeter-level composite material, which is beneficial to recycling. Meanwhile, the composite adsorbent has the advantages of large adsorption capacity, strong selectivity and good adsorption kinetics, and can be used in an advanced treatment system for lead-containing wastewater.
The purpose of the invention is realized by the following technical scheme:
the invention relates to a molybdenum disulfide activated carbon fiber composite adsorbent for deeply purifying lead-containing wastewater, which has a sandwich multilayer structure: the method is characterized in that activated carbon fibers with larger specific surface area and length-diameter ratio are used as carriers, the middle layer is a polydopamine coating, and molybdenum disulfide nanosheets are loaded on the outermost layer through a hydrothermal method under the mediation effect of the polydopamine coating.
Preferably, the surface of the composite adsorbent is uniformly distributed with molybdenum disulfide nanosheet layer spacing of 0.65-0.94nm, and the molybdenum disulfide mass content is 5% -20%.
A preparation method of a molybdenum disulfide activated carbon fiber composite adsorbent for deeply purifying lead-containing wastewater comprises the following specific steps:
(1) cutting the activated carbon fiber into uniform short fiber shape by a pulverizer;
(2) adding the cut activated carbon fiber into a dopamine hydrochloride solution, then placing the mixture into a shaking table, oscillating for 24 hours at the temperature of 25 ℃, alternately washing the product obtained by suction filtration with deionized water and ethanol for at least three times, and then placing the product into a drying oven for drying for 12 hours at the temperature of 60 ℃;
(3) drying the product obtained in the step (2)Adding (NH)4)6Mo7O24·4H2O and CN2H4In the mixed solution of S, oscillating the mixture in a shaking table at the temperature of 25 ℃ for 12-24 h; after the oscillation is finished, transferring the mixture into a stainless steel autoclave with a polytetrafluoroethylene lining, putting the stainless steel autoclave into a high-temperature oven, heating the mixture for 20 hours at 160-220 ℃, and naturally cooling the mixture to room temperature; and (3) alternately washing the product obtained by suction filtration with deionized water and ethanol for at least three times, and then drying the product in a drying oven at 60 ℃ for 12 hours.
Preferably, in the step (2), the dopamine hydrochloride solution is prepared by using a 5-20 mM Tris-HCl buffer solution, and the pH value of the dopamine hydrochloride solution is 7-9 and the concentration of the dopamine hydrochloride solution is 1-5 g/L.
Preferably, the mass ratio of the activated carbon fiber to the dopamine hydrochloride in the step (2) is (0.2-2): 1.
preferably, the activated carbon fiber, (NH) is used in the step (3)4)6Mo7O24·4H2O and CN2H4The mass ratio of the S to the S is (0.2-2) to (0.5-2) to 1.
The molybdenum disulfide activated carbon fiber composite adsorbent is applied to the treatment of lead-containing wastewater.
Preferably, the adsorbent can adsorb 300-500 Mg of lead per gram on average, and the adsorption amount is not influenced by coexisting cations in water such as Ca, Mg (concentration range: 0-2000 Mg/L) and the like.
Preferably, the adsorbent after saturated adsorption can be desorbed and regenerated through 0.005-0.1M EDTA-2Na solution.
Compared with the prior art, the invention has the following beneficial effects:
(1) according to the technical scheme, the activated carbon fiber with high specific surface area and length-diameter ratio is used as a carrier, the polydopamine coating is used for uniformly fixing the molybdenum disulfide nanosheets on the surface of the carrier, and the lead ion adsorption capacity and adsorption selectivity are excellent. Wherein, sulfur atoms on the surface of the molybdenum disulfide adsorb lead through the complexation with lead ions, and polydopamine can also be removed by chelating the lead ions in water through phenolic hydroxyl and amino on the surface.
(2) According to the technical scheme, the adsorbent utilizes the strong adhesion of polydopamine to enhance the acting force between molybdenum disulfide and activated carbon fibers, the load rate of molybdenum disulfide is remarkably improved, the loss of molybdenum disulfide in a composite adsorbent in a fluid system is effectively prevented, and faster adsorption kinetics are brought.
(3) According to the technical scheme, the activated carbon fiber is used as the carrier, and the defects that the micro-nano molybdenum disulfide powder adsorbent is easy to run off, large in fluid resistance, difficult to separate solid from liquid, not beneficial to recycling and the like in practical application are effectively overcome by means of the appearance characteristics and the physicochemical properties of the carrier. Meanwhile, after the adsorbent is used, desorption regeneration can be efficiently carried out by using desorption liquid, and the actual application value of the adsorbent is ensured.
Drawings
FIG. 1: the SEM image and the EDS mapping scanning image of the molybdenum disulfide activated carbon fiber composite adsorbent are shown in the specification. (a) Is a low power SEM picture; (b) high power SEM image; (c) and (d) and (e) are distributions of N, Mo and S elements in the specific region of the adsorbent measured by EDS mapping, respectively.
FIG. 2: the XRD pattern of the molybdenum disulfide activated carbon fiber composite adsorbent is disclosed.
FIG. 3; experimental diagram of dynamic adsorption column of example 7.
Detailed Description
The present invention will be further described in detail with reference to specific examples, which are implemented on the premise of the technical solution of the present invention, but the scope of the present invention is not limited to the following examples.
Example 1
The preparation method of the molybdenum disulfide activated carbon fiber composite adsorbent in the embodiment is as follows:
(1) the active carbon fiber felt is crushed into uniform short fiber shape by a plant crusher, and is washed and dried by deionized water. (2) Adding the treated activated carbon fiber into a dopamine hydrochloride solution with the pH value of 8.4-8.5 and the concentration of 2g/L, wherein the mass ratio of the activated carbon fiber to the dopamine hydrochloride is 1: 1, dopamine hydrochloride solution buffered with 10mM Tris-HClPreparing a solution; then the mixture was put into a shaker, shaken at 25 ℃ for 24h, and the resulting product was washed three times with deionized water and ethanol alternately, and then dried in a drying oven at 60 ℃ for 12 h. (3) Adding the compound obtained in the step (2) into (NH)4)6Mo7O24·4H2O and CN2H4S, wherein activated carbon fiber, (NH)4)6Mo7O24·4H2O and CN2H4The mass ratio of S is 3:2:3.6, and the mixture is oscillated for 12-24h at the temperature of 25 ℃ in a shaking table; and after the oscillation is finished, transferring the mixture into a stainless steel high-pressure autoclave with a polytetrafluoroethylene lining, putting the stainless steel high-pressure autoclave into a high-temperature oven, heating the mixture for 20 hours at 180 ℃, naturally cooling the mixture to room temperature, and cleaning and drying the obtained product to constant weight to obtain the nano composite adsorbent.
From a scanning electron microscope image (figure 1b), a large number of ultrathin nanosheets are uniformly attached to the surface of the activated carbon fiber in flower shapes, and from an EDS image (figures 1c-e), it can be clearly seen that MoS not only exists on the surface of the material2The element Mo and the element S exist, and the element N of the polydopamine exists, so that the surface of the activated carbon fiber is wrapped by the polydopamine coating. Meanwhile, the XRD pattern (fig. 2) of the composite adsorbent can correspond to the (002) (100) (102) and (110) crystal planes of the molybdenum disulfide of the 2H phase. The results show that the activated carbon fiber is successfully loaded with the molybdenum disulfide nanosheet.
Example 2
Preparing Pb with a certain concentration range from 20mg/L to 500mg/L2+Solutions of each 25mg of the composite material to 50mL of Pb at the above different concentrations2+In the solution, oscillating in a shaking table at the temperature of 25 ℃ and the speed of 160r/min for 24 hours until the solution is balanced, taking the supernatant, measuring the concentration of the supernatant when the solution is balanced by using an inductively coupled plasma emission spectrometer (ICP), and calculating the Pb pair of the molybdenum disulfide activated carbon fiber composite material under the condition2+The adsorption capacity of the adsorbent can reach 393 mg/g.
Example 3
2 groups of different competitive ion solutions are prepared to ensure Pb2+The concentration is 100mg/L, wherein Ca2+、Mg2+The concentration is respectively equal to 100mgPb of L2+Are 0, 5, 10, 20, 40, 60, 100, respectively. Respectively adding 25mg of the composite material into 50mL of the different solutions, shaking the solutions in a shaking table at a speed of 160r/min at a temperature of 25 ℃ for 24 hours until the solutions are balanced, taking supernatant, and measuring the concentration of the supernatant at the equilibrium by using ICP. The result analysis shows that the molybdenum disulfide activated carbon fiber composite material keeps stable removal efficiency of lead in the presence of a large amount of calcium and magnesium ions, and shows excellent adsorption selectivity.
Example 4
Preparing 200mg/L Pb2+500mL of the solution is added with 250mg of molybdenum disulfide activated carbon fiber composite material, then mechanical stirring is carried out, timing is started, and the adsorbed solution is taken out at intervals to measure the concentration. Pb measured at various times2+The concentration and the removal rate of lead ions in different time are calculated, the speed of the adsorbent to lead ions is extremely high in the first 60 minutes of adsorption, and the adsorption balance is achieved in 100 minutes.
Example 5
8 portions of 150mg/L Pb are prepared2+50mL of each solution, the pH value of each solution is adjusted to be uniformly distributed between 1 and 7, and 25mg of molybdenum disulfide activated carbon fiber composite material is added into each solution. After 24 hours at 25 ℃ and with shaking at 160r/min in a shaker until equilibrium, the supernatant was taken and its concentration at equilibrium was measured by ICP and its pH at equilibrium was measured. Along with the increase of the pH value of the solution, the adsorption capacity of the composite material is continuously and slowly enhanced, and the adsorbent has excellent adsorption capacity on lead ions in a wide pH range.
Example 6
Preparing 10mg/L Pb2+50mL of the solution was added with 25mg of the composite adsorbent, and after equilibrium of adsorption, desorption was carried out by shaking 50mL of 5mM EDTA-2Na solution in a shaker for 5 hours, and similarly, 5 adsorption-desorption cycles were carried out. And respectively measuring the lead ion concentration in the adsorption solution and the desorption solution, and calculating the adsorption amount and the desorption rate. After 5 times of adsorption-desorption cycles, the adsorption capacity of the composite adsorbent is not obviously reduced, and the desorption rate of lead ions adsorbed on each round of adsorbent is maintained to be more than 90%.
Example 7
Preparing a plurality of liters of simulated wastewater with lead ion concentration of 10mg/L, wherein the solution contains 200mg/L Ca2+And Mg2+Competing ions, simulated wastewater pH 4.5.
The simulated wastewater prepared in this example was passed through an adsorption column packed with the molybdenum disulfide activated carbon fiber composite adsorbent prepared in this example from top to bottom at a flow rate of 50mL/h, and the effluent was continuously collected by an autosampler with the breakthrough point set to 1 mg/L. According to the experimental result, each kilogram of the composite adsorbent can treat 16t of simulated wastewater with the lead ion concentration of 10mg/L until the lead ion concentration is below 1 mg/L.
Claims (10)
1. The utility model provides a molybdenum disulfide activated carbon fiber composite adsorbent for deep purification contains plumbous waste water which characterized in that, composite adsorbent has "sandwich" multilayer structure: the method is characterized in that activated carbon fibers with larger specific surface area and length-diameter ratio are used as carriers, the middle layer is a polydopamine coating, and molybdenum disulfide nanosheets are loaded on the outermost layer through a hydrothermal method under the mediation effect of the polydopamine coating.
2. The molybdenum disulfide activated carbon fiber composite adsorbent of claim 1, wherein the molybdenum disulfide nanosheets are uniformly and densely distributed on the surface of the activated carbon fiber, the interlayer spacing of the nanosheets is 0.65-0.94nm, and the mass content of molybdenum disulfide in the composite adsorbent is 5% -20%.
3. The preparation method of the molybdenum disulfide activated carbon fiber composite adsorbent for deeply purifying lead-containing wastewater according to claim 1, which is characterized by comprising the following steps:
(1) cutting the activated carbon fiber into uniform short fiber shape by a pulverizer;
(2) adding the cut activated carbon fiber into a dopamine hydrochloride solution, then placing the mixture into a shaking table, oscillating for 24 hours at the temperature of 25 ℃, alternately washing the product obtained by suction filtration with deionized water and ethanol for at least three times, and then placing the product into a drying oven for drying for 12 hours at the temperature of 60 ℃;
(3) adding (NH) into the dried product obtained in the step (2)4)6Mo7O24·4H2O and CN2H4In the mixed solution of S, oscillating the mixture in a shaking table at the temperature of 25 ℃ for 12-24 h; after the oscillation is finished, transferring the mixture into a stainless steel autoclave with a polytetrafluoroethylene lining, putting the stainless steel autoclave into a high-temperature oven, heating the mixture for 20 hours at 160-220 ℃, and naturally cooling the mixture to room temperature; and (3) alternately washing the product obtained by suction filtration with deionized water and ethanol for at least three times, and then drying the product in a drying oven at 60 ℃ for 12 hours.
4. The preparation method of the molybdenum disulfide activated carbon fiber composite adsorbent according to claim 3, wherein the molybdenum disulfide activated carbon fiber composite adsorbent with different loading amounts can be prepared by repeating the step (2) and the step (3)2-5 times.
5. The preparation method of the molybdenum disulfide activated carbon fiber composite adsorbent according to claim 3, wherein the dopamine hydrochloride solution in the step (2) is prepared by using 5-20 mM Tris-HCl buffer solution, and the pH value of the dopamine hydrochloride solution is 7-9, and the concentration of the dopamine hydrochloride solution is 1-5 g/L.
6. The preparation method of the molybdenum disulfide activated carbon fiber composite adsorbent according to claim 3, wherein the mass ratio of the activated carbon fiber in the step (2) to the dopamine hydrochloride is 0.2-2: 1.
7. the method for preparing the molybdenum disulfide activated carbon fiber composite adsorbent according to claim 3, wherein the activated carbon fiber (NH) in the step (2)4)6Mo7O24·4H2O and CN2H4The mass ratio of S is 0.2-2: 0.5-2: 1.
8. The use of the molybdenum disulfide activated carbon fiber composite adsorbent of claim 1 in the treatment of lead-containing wastewater.
9. The use according to claim 8, wherein the adsorbent can adsorb 300-500 Mg of lead per gram on average, and the adsorption amount is not affected by coexisting cations in water such as Ca and Mg (concentration range: 0-2000 Mg/L).
10. The use of claim 9, wherein the adsorbent saturated by adsorption can be desorbed and regenerated by 0.005-0.1M EDTA-2Na solution.
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| CN115180739A (en) * | 2022-07-18 | 2022-10-14 | 威海智洁环保技术有限公司 | Method for removing 2-methylisoborneol and geosmin in drinking water |
| CN115475606A (en) * | 2022-10-19 | 2022-12-16 | 辽宁大学 | Modified molybdenum sulfide/charcoal material, preparation method thereof and application thereof in co-adsorption of antibiotics and heavy metal ions |
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| CN115672253A (en) * | 2022-11-07 | 2023-02-03 | 南京工业大学 | High-stability molybdenum disulfide coating composite adsorbent and preparation method and application thereof |
| CN116159574A (en) * | 2023-02-10 | 2023-05-26 | 浙江理工大学 | Preparation method of composite material for mobile treatment of oily wastewater |
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