CN111285445B - Method for removing halogenated organic pollutants in water by utilizing zero-valent aluminum and copper oxide - Google Patents
Method for removing halogenated organic pollutants in water by utilizing zero-valent aluminum and copper oxide Download PDFInfo
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- CN111285445B CN111285445B CN202010230652.XA CN202010230652A CN111285445B CN 111285445 B CN111285445 B CN 111285445B CN 202010230652 A CN202010230652 A CN 202010230652A CN 111285445 B CN111285445 B CN 111285445B
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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
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/467—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction
- C02F1/4676—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction by electroreduction
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/36—Organic compounds containing halogen
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Abstract
The invention relates to a method for removing halogenated organic pollutants in water by utilizing zero-valent aluminum and copper oxide, belonging to the technical field of water pollution treatment. The method comprises the following steps: s1, mixing the zero-valent aluminum powder and the copper oxide powder according to the mass ratio of (5-500) to 1, and filling the mixed powder into a fixed bed reactor; s2, adding electrolyte into water containing halogenated organic pollutants to obtain a mixed solution, pumping the mixed solution into a reactor from the bottom of the fixed bed reactor, and discharging the treated solution through a water outlet at the upper end of the reactor; the technical scheme of the invention utilizes the principle that zero-valent aluminum and copper oxide form galvanic corrosion in the presence of electrolyte, and strengthens the reduction activity of the zero-valent aluminum on halogenated organic matters by adding the copper oxide and the electrolyte, so that the method can effectively remove the halogenated organic pollutants in water, the elution amount of aluminum ions and copper ions in the treated water is very low, secondary pollution cannot be generated, the method is efficient, the operation is simple, and the used medicines are cheap and easy to obtain.
Description
Technical Field
The invention belongs to the technical field of water treatment, and particularly relates to a method for removing halogenated organic pollutants in water by utilizing zero-valent aluminum and copper oxide.
Background
The use and discharge of a large amount of halogenated organic matters cause the pollution of the halogenated organic matters in the water body to be increasingly serious, and threaten the ecological safety and the human health. Moreover, halogenated organic pollutants have the characteristics of environmental persistence, difficult biodegradation, bioaccumulation, high toxicity, long-distance migration capability and the like, and how to effectively solve the problem of halogenated pollutants is always the focus of attention in the environmental field.
The zero-valent aluminum has lower oxidation-reduction potential, higher reduction capability and rich resources, and can be used for dehalogenation of halogenated pollutants in water and reduce the toxicity of halogenated organic pollutants. However, since the zero-valent aluminum is very easily oxidized by oxygen in the air, the aluminum oxide film formed on the surface is very dense and non-conductive and is very stable in the range of pH4-9, thereby inhibiting the reactivity of the zero-valent aluminum in practical application.
Disclosure of Invention
In view of the above, the present invention provides a method for removing halogenated organic pollutants in water by using a combination of zero-valent aluminum and copper oxide, wherein the method uses the formation of galvanic corrosion of zero-valent aluminum and copper oxide in the presence of an electrolyte, thereby solving the problem of low reaction activity of zero-valent aluminum under a neutral condition and realizing efficient removal of halogenated organic matters in water.
In order to realize the purpose of the invention, the technical scheme provided by the invention is that the method for removing the halogenated organic pollutants in water by utilizing the zero-valent aluminum and the copper oxide comprises the following steps:
s1, mixing the zero-valent aluminum powder and the copper oxide powder according to the mass ratio of (5-500) to 1, and filling the mixed powder into a fixed bed reactor;
s2, adding chloride ion-containing salt serving as electrolyte into water containing halogenated organic pollutants, adding the chloride ion-containing salt to the water to obtain a mixed solution with the concentration of 0.01-1.0mmol/L, pumping the mixed solution into a fixed bed reactor, keeping the mixed solution for 0.1-1 hour, and discharging the treated solution through a water outlet of the reactor.
The method for removing the halogenated organic pollutants in the water by utilizing the zero-valent aluminum and the copper oxide further comprises the following technical scheme:
preferably, the particle size of the zero-valent aluminum powder in the step S1 is 100-200 meshes, and the particle size of the copper oxide powder is 1-5 microns.
Preferably, the halogenated organic pollutant in step S2 is one or a mixture of two or more of chlorinated organic compound, brominated organic compound and iodo organic compound.
Preferably, the halogenated organic contaminant is 2, 4-dichlorophenol or sodium diatrizoate.
Preferably, the electrolyte in step S2 is sodium chloride, and is added to a concentration of 0.1 mmol/L.
Compared with the prior art, the invention has the beneficial effects that:
1) the technical scheme of the invention utilizes the principle that zero-valent aluminum and copper oxide form galvanic corrosion in the presence of electrolyte, and strengthens the reduction activity of the zero-valent aluminum on halogenated organic matters by adding the copper oxide and the electrolyte. The addition of the copper oxide enables the anode and the cathode in the system to be separated, the migration distance of aluminum ions generated near the anode and hydroxide ions generated near the cathode is increased, hydroxide precipitates are more easily generated in a solution instead of on the surface of the zero-valent aluminum, the generation of a passivation layer on the surface of the zero-valent aluminum is relieved, the reaction activity of the zero-valent aluminum is improved, and meanwhile, chloride ions in the electrolyte can generate a pitting action on the surface of the zero-valent aluminum, so that the corrosion of the surface of the zero-valent aluminum is further promoted.
2) The invention provides a method for treating halogenated organic pollutants, which can effectively remove the halogenated organic pollutants in water, and the treated water has low leaching amount of aluminum ions and copper ions and cannot generate secondary pollution. The method has the advantages of high efficiency, simple operation and low price and easy obtainment of used medicines.
3) The detection of the wastewater before and after the treatment by the method disclosed by the invention shows that the removal rate of 2, 4-dichlorophenol or sodium diatrizoate after the treatment by the method disclosed by the invention is over 90 percent and can reach 100 percent at most.
Drawings
FIG. 1 is a schematic view of a fixed bed reactor used in the treatment method of the present invention;
FIG. 2 is a graph showing the removal rate of 2, 4-dichlorophen by the treatment method of the present invention at different NaCl concentrations;
FIG. 3 is a graph showing the removal rate of sodium diatrizoate at different mass ratios of zerovalent aluminum to copper oxide according to the treatment method of the present invention;
FIG. 4 is an SEM image of zero valent aluminum and copper oxide before and after reaction in the treatment method of the present invention;
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more clearly understood, the present invention is further described in detail below with reference to the accompanying drawings and embodiments, and all other embodiments obtained by a person of ordinary skill in the art based on the embodiments of the present invention without creative efforts belong to the protection scope of the present invention.
In the following examples, the concentration of 2, 4-dichlorophenol or sodium diatrizoate was measured by high performance liquid chromatography.
Example 1
The reactor used in the technical scheme of the invention is not limited to a fixed bed reactor, and in principle any reactor capable of realizing reaction effect can be used. The water inlet and outlet of the fixed bed reactor are not limited to two ends of the reactor shell.
The structure of the fixed bed reactor used in the treatment method of the present invention is shown in FIG. 1. The main body of the fixed bed reaction device is a cylindrical reactor shell, the lower part of the reactor shell is provided with a water inlet and a water distribution plate, the middle of the reactor shell is filled with a mixture of zero-valent aluminum powder and copper oxide powder in a certain mass ratio as a filler, and the upper end of the reactor shell is provided with a water outlet. A mixed solution containing halogenated organic matters and electrolytes with certain concentration is prepared in a water inlet tank, the mixed solution is pumped into a water distributor at the bottom of a reactor through a peristaltic pump and enters a packing layer for treatment, and the treated solution flows out of a water outlet at the upper part of the reactor and enters a water outlet tank.
Examples 2 to 4
S1, mixing the zero-valent aluminum powder and the copper oxide powder according to the mass ratio of 50:1, and filling the mixed powder into a fixed bed reactor;
s2, preparing an aqueous solution containing 5umol/L2, 4-dichlorophenol, dividing into three parts, and respectively adding NaCl until the concentration is 1mmol/L, 0.1mmol/L and 0.01mmol/L to obtain mixed solutions 1, 2 and 3; pouring the mixed solution 1 into a water inlet tank of the fixed bed reactor, opening a peristaltic pump at a water inlet, slowly pumping the solution in the water inlet tank into the reactor from the bottom of the fixed bed reactor, treating the solution by the uniformly mixed zero-valent aluminum powder and copper oxide powder in the packing layer, discharging the solution from a water outlet at the top end of the fixed bed reactor, and collecting effluent to a water outlet tank; treating the mixed solution 2 and 3 in turn by the same method;
the effluent of the mixed solutions 1, 2 and 3 was filtered through a 0.45 μm filter membrane, and the residual amount of 2, 4-dichlorophenol in the effluent of the three mixed solutions was measured by HPLC, respectively, as shown in FIG. 2, in which the unit mM represents mmol/L. The removal rate of 2, 4-dichlorophen in the treated effluent of the mixed solution 1 reaches 100 percent, the removal rate of 2, 4-dichlorophen in the treated effluent of the mixed solution 2 reaches 100 percent, and the removal rate of 2, 4-dichlorophen in the treated effluent of the mixed solution 3 reaches 92.4 percent; indicating that the increased electrolyte concentration facilitates the removal of halogenated organics by the zero-valent aluminum/copper oxide combination.
Example 5
S1, filling the zero-valent aluminum powder into the fixed bed reactor;
s2, preparing an aqueous solution containing 5umol/L of diatrizoic acid sodium, pouring the aqueous solution into a water inlet tank of the fixed bed reactor, opening a peristaltic pump at the water inlet, slowly pumping the solution in the water inlet tank into the reactor from the bottom of the fixed bed reactor, treating the solution by the zero-valent aluminum powder and the copper oxide powder which are uniformly mixed in the packing layer, discharging the solution from a water outlet at the top end of the fixed bed reactor, and collecting effluent to a water outlet tank;
and (3) filtering the effluent through a 0.45-micron filter membrane, and detecting the residual quantity of the diatrizoic acid sodium in the water by adopting high performance liquid chromatography, wherein the removal rate of the diatrizoic acid sodium reaches 50%.
Example 6
S1, mixing the zero-valent aluminum powder and the copper oxide powder according to the mass ratio of 25:1, and filling the mixed powder into a fixed bed reactor;
s2, preparing an aqueous solution containing 5umol/L of diatrizoic acid sodium, pouring the aqueous solution into a water inlet tank of the fixed bed reactor, opening a peristaltic pump at the water inlet, slowly pumping the solution in the water inlet tank into the reactor from the bottom of the fixed bed reactor, treating the solution by the zero-valent aluminum powder and the copper oxide powder which are uniformly mixed in the packing layer, discharging the solution from a water outlet at the top end of the fixed bed reactor, and collecting effluent to a water outlet tank;
and (3) filtering the effluent through a 0.45-micron filter membrane, and detecting the residual quantity of the diatrizoic acid sodium in the water by adopting high performance liquid chromatography, wherein the removal rate of the diatrizoic acid sodium reaches 92.8%.
Example 7
S1, mixing the zero-valent aluminum powder and the copper oxide powder according to the mass ratio of 50:1, and filling the mixed powder into a fixed bed reactor;
s2, preparing an aqueous solution containing 5umol/L of diatrizoic acid sodium, pouring the aqueous solution into a water inlet tank of the fixed bed reactor, opening a peristaltic pump at the water inlet, slowly pumping the solution in the water inlet tank into the reactor from the bottom of the fixed bed reactor, treating the solution by the zero-valent aluminum powder and the copper oxide powder which are uniformly mixed in the packing layer, discharging the solution from a water outlet at the top end of the fixed bed reactor, and collecting effluent to a water outlet tank;
and (3) filtering the effluent through a 0.45-micron filter membrane, and detecting the residual quantity of the diatrizoic acid sodium in the water by adopting high performance liquid chromatography, wherein the removal rate of the diatrizoic acid sodium reaches 93.2%.
Example 8
S1, mixing the zero-valent aluminum powder and the copper oxide powder according to the mass ratio of 100:1, and filling the mixed powder into a fixed bed reactor;
s2, preparing an aqueous solution containing 5umol/L of diatrizoic acid sodium, pouring the aqueous solution into a water inlet tank of the fixed bed reactor, opening a peristaltic pump at the water inlet, slowly pumping the solution in the water inlet tank into the reactor from the bottom of the fixed bed reactor, treating the solution by the zero-valent aluminum powder and the copper oxide powder which are uniformly mixed in the packing layer, discharging the solution from a water outlet at the top end of the fixed bed reactor, and collecting effluent to a water outlet tank;
and (3) filtering the effluent through a 0.45-micron filter membrane, and detecting the residual quantity of the diatrizoic acid sodium in the water by adopting high performance liquid chromatography, wherein the removal rate of the diatrizoic acid sodium reaches 94%.
FIG. 3 shows the removal rate of sodium diatrizoate after treatment in the fixed bed reactor in examples 5, 6, 7 and 8, and the effect of the mixed mass ratio of different zero-valent aluminum and copper oxide on the removal effect is examined, wherein the removal rate of zero-valent aluminum on sodium diatrizoate after copper oxide is added can reach more than 90%, while the removal rate of zero-valent aluminum on sodium diatrizoate in the control group example without copper oxide is only 50%.
FIG. 4 shows SEM images of zero-valent aluminum powder and copper oxide powder before and after the reaction, FIG. 4(a) represents zero-valent aluminum powder amplified by 500 times before the reaction, FIG. 4(b) represents zero-valent aluminum powder amplified by 5000 times before the reaction, FIG. 4(c) represents copper oxide powder amplified by 500 times before the reaction, FIG. 4(d) represents copper oxide powder amplified by 5000 times before the reaction, FIG. 4(e) represents mixture of zero-valent aluminum powder and copper oxide powder amplified by 500 times after the reaction, and FIG. 4(f) represents mixture of zero-valent aluminum powder and copper oxide powder amplified by 5000 times after the reaction; as can be seen from the figure, the surfaces of the unreacted zero-valent aluminum powder and the copper oxide powder are smooth, and the surfaces of the reacted zero-valent aluminum powder and the copper oxide powder which are in contact with each other are corroded. The addition of the copper oxide is illustrated to separate the anode and the cathode in the system, so that the migration distance of aluminum ions generated near the anode and hydroxyl ions generated near the cathode is increased, hydroxide precipitates are more easily generated in a solution instead of on the surface of the zero-valent aluminum, the generation of a passivation layer is relieved, the reaction activity of the zero-valent aluminum is improved, meanwhile, chloride ions in the electrolyte can generate a pitting action on the surface of the zero-valent aluminum, the corrosion of the surface of the zero-valent aluminum is further promoted, and the reduction activity of the zero-valent aluminum on halogenated organic matters can be enhanced by adding the copper oxide and the electrolyte.
It should be understood by those skilled in the art that the foregoing is only illustrative of several embodiments of the invention, and not of all embodiments. It should be noted that many variations and modifications are possible to those skilled in the art, and all variations and modifications that do not depart from the gist of the invention are intended to be within the scope of the invention as defined in the appended claims.
Claims (4)
1. A method for removing halogenated organic pollutants in water by utilizing zero-valent aluminum and copper oxide is characterized by comprising the following steps:
s1, mixing zero-valent aluminum powder and copper oxide powder according to the mass ratio of (25-500) to 1, filling the mixed powder into a fixed bed reactor, wherein the particle size of the zero-valent aluminum powder is 100-200 meshes, and the particle size of the copper oxide powder is 1-5 microns;
s2, adding sodium chloride as electrolyte into water containing halogenated organic pollutants, adding the electrolyte into the water with the concentration of 0.01-1.0mmol/L to obtain a mixed solution, pumping the mixed solution into a fixed bed reactor, keeping the mixed solution for 0.1-1 hour, and discharging the treated solution through a water outlet of the reactor.
2. The method for removing halogenated organic pollutants in water by using zero-valent aluminum and copper oxide according to claim 1, wherein the halogenated organic pollutants in the step S2 are one or a mixture of two or more of chlorinated organic compounds, brominated organic compounds and iodo organic compounds.
3. The method for removing halogenated organic pollutants in water by using zero-valent aluminum and copper oxide according to claim 2, wherein the halogenated organic pollutants are 2, 4-dichlorophenol or sodium diatrizoate.
4. The method for removing halogenated organic pollutants in water by utilizing zero-valent aluminum and copper oxide according to claim 1, wherein the electrolyte sodium chloride is added in the step S2 at a concentration of 0.1 mmol/L.
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