CN114014414A - Copper ion treatment method - Google Patents

Copper ion treatment method Download PDF

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CN114014414A
CN114014414A CN202111171694.1A CN202111171694A CN114014414A CN 114014414 A CN114014414 A CN 114014414A CN 202111171694 A CN202111171694 A CN 202111171694A CN 114014414 A CN114014414 A CN 114014414A
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mesoporous carbon
carbon material
copper
adsorption
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CN114014414B (en
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余皓
蒋梦瑶
曹永海
黄江南
王红娟
彭峰
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South China University of Technology SCUT
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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
    • C02F1/469—Treatment of water, waste water, or sewage by electrochemical methods by electrochemical separation, e.g. by electro-osmosis, electrodialysis, electrophoresis
    • C02F1/4691—Capacitive deionisation
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/28—Treatment of water, waste water, or sewage by sorption
    • C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
    • 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
    • C02F2101/10—Inorganic compounds
    • C02F2101/20—Heavy metals or heavy metal compounds
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2209/00—Controlling or monitoring parameters in water treatment
    • C02F2209/05—Conductivity or salinity
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

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Abstract

The invention discloses a copper ion treatment method, which comprises the following steps: treating the copper ion solution by adopting an electric adsorption device; mesoporous carbon materials are filled between the anode and the cathode of the electric adsorption device. The raw materials required by the electro-adsorption are wide in source and low in price, the treatment process is controllable, and the mass preparation of products is easy to realize.

Description

Copper ion treatment method
Technical Field
The invention belongs to the technical field of water treatment, and particularly relates to a copper ion treatment method.
Background
Copper ion (Cu)2+) Is a common pollutant in industrial wastewater of electroplating, printed circuit boards, semiconductors and the like. Copper is a trace element essential to the human body. However, excessive copper in the body can lead to various diseases, and when the intake of copper exceeds the maximum limit, copper causes irreparable damage to the eyes, liver and central nervous system, resulting in alzheimer's disease and parkinson's disease, and even death. On the other hand, copper is also an important industrial raw material, and it is valuable to remove and recover copper from water.
Various techniques including chemical precipitation, membrane separation, electrodeposition, ion exchange, cementation and adsorption have been used to remove Cu from wastewater2+Adsorption is one of the common methods for removing metal ions. For Cu in wastewater2+The adsorption treatment method comprises electro-adsorption and reverse osmosis. The electro-adsorption technology (also called as capacitive deionization technology) has the advantages of low pressure, normal temperature, low energy consumption, low cost, no secondary pollution, easy regeneration and the like, can be used for removing salts or metal ions (copper, arsenic, mercury, chromium, lead and the like) in water, is a promising emerging water heavy metal treatment technology, effectively avoids using chemical reagents and prevents secondary pollution by adopting electric energy as a driving force, and has good industrial application prospect. However, the electro-adsorption technology used in the industry at present has low adsorption efficiency, complex preparation of the adsorption material, long time for treating copper-containing wastewater and unsuitability for large-scale use. The application of electro-adsorption to treat copper-containing wastewater is facing dilemma.
Disclosure of Invention
In order to solve the problem of poor effect of removing copper ions by electro-adsorption in the prior art, the invention aims to provide a copper ion treatment method which has good effect of removing copper ions.
Due to the unique structural characteristics of the mesoporous carbon material, such as high specific surface area, low density, high conductivity, low resistance, controllable aperture, easy recovery and recycling, the mesoporous carbon material has unique advantages in practical use. The mesoporous carbon material is used as an adsorbent, the copper-containing wastewater is efficiently treated by applying voltage, the copper-adsorbing mesoporous carbon material can be effectively regenerated, the wastewater is circularly adsorbed and treated, and the mesoporous carbon material has a very good industrial application prospect.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a copper ion treatment method comprises the following steps: treating the copper ion solution by adopting an electric adsorption device; mesoporous carbon materials are filled between the anode and the cathode of the electric adsorption device.
Preferably, in the copper ion treatment method, the copper ion solution comprises one or more of a copper nitrate solution, a copper chloride solution and a copper sulfate solution; further preferably, the copper ion solution is a copper nitrate solution.
Preferably, in the copper ion treatment method, the copper ion concentration of the copper ion solution is 5-1500 mg/L; further preferably, the copper ion concentration of the copper ion solution is 8-1200 mg/L; still further preferably, the copper ion concentration of the copper ion solution is 9-1100 mg/L; still more preferably, the copper ion concentration of the copper ion solution is 10 to 1000 mg/L.
Preferably, in the copper ion treatment method, the pH of the copper ion solution is 1-7; further preferably, the pH of the copper ion solution is 2-6; still further preferably, the pH of the copper ion solution is 4 to 6; still more preferably, the pH of the copper ion solution is 5.
Preferably, in the copper ion treatment method, the flow rate of the copper ion solution passing through the electric adsorption device is 0.5-80 mL/min; further preferably, the flow rate of the copper ion solution passing through the electro-adsorption device is 0.8-50 mL/min; still further preferably, the flow rate of the copper ion solution passing through the electro-adsorption device is 0.9-10 mL/min; still more preferably, the flow rate of the copper ion solution through the electro-adsorption device is 1-2 mL/min.
Preferably, in the copper ion treatment method, the applied voltage of the positive electrode and the negative electrode of the electric adsorption device is 0-8.0V; further preferably, the applied voltage of the positive electrode and the negative electrode of the electric adsorption device is 0-6.0V; still further preferably, the applied voltage of the positive and negative electrodes of the electro-adsorption device is 0-5.0V; further preferably, the applied voltage of the positive and negative electrodes of the electro-adhesion device is 0.5-1V.
Preferably, in the copper ion treatment method, the electro-adsorption time of the copper ion solution is 0.1-5 h; further preferably, the electro-adsorption time of the copper ion solution is 0.1-4 h; still more preferably, the electro-adsorption time of the copper ion solution is 1-4 h.
Preferably, in the copper ion treatment method, the preparation method of the mesoporous carbon material includes the following steps:
1) mixing phenols, a template agent and an ethanol solution for reaction, and then adding a curing agent for reaction; adding formaldehyde solution to react to obtain a mixture;
2) solidifying the mixture obtained in the step 1) to obtain a solid reactant;
3) carbonizing the solid reactant in the step 2) to obtain the mesoporous carbon material.
More preferably, in the step 1) of the method for preparing a mesoporous carbon material, the phenol is at least one of resorcinol and phenol; still more preferably, the phenol is resorcinol.
Further preferably, in the step 1) of the preparation method of the mesoporous carbon material, the template is at least one of polyether F127, Pluronic P123 and mesoporous silica; still further preferably, the template agent is at least one of polyether F127 and Pluronic P123; still more preferably, the templating agent is polyether F127.
Further preferably, in the preparation method of the mesoporous carbon material, in step 1), the curing agent is at least one of 1, 6-hexanediamine, toluene and 1,3, 5-trimethylbenzene; still more preferably, the curing agent is at least one of 1, 6-hexanediamine and toluene; still more preferably, the curing agent is 1, 6-hexanediamine.
Further preferably, in the step 1) of the preparation method of the mesoporous carbon material, the mass ratio of the template, the phenols, the ethanol, the curing agent and the formaldehyde is as follows: 1: (2-3): (6-8): (0.06-0.1): (3-4); still further preferably, the mass ratio of the template agent, the phenols, the ethanol, the curing agent and the formaldehyde is as follows: 1: (2.3-2.5): (6.5-7.5): (0.07-0.09): (3.5-3.6).
Further preferably, in the step 1) of the preparation method of the mesoporous carbon material, the phenols, the template agent and the ethanol solution are mixed and reacted for 10-20 min; still further preferably, the mixing reaction time of the phenols, the template agent and the ethanol solution is 14-16 min; more preferably, the mixing reaction time of the phenols, the template agent and the ethanol solution is 15 min.
Further preferably, in the step 1) of the preparation method of the mesoporous carbon material, the curing agent is added for reaction for 40-50 min; still more preferably, the time for adding the curing agent to react is 43-48 min; more preferably, the time for adding the curing agent is 45 min.
Further preferably, in the step 1) of the preparation method of the mesoporous carbon material, the formaldehyde solution is added for reaction for 10-30 min; further preferably, the time for adding the formaldehyde solution to react is 15-25 min; more preferably, the time for adding the formaldehyde solution for reaction is 20 min.
Further preferably, in step 2), the mesoporous carbon material is cured in an oven.
Further preferably, in the step 2) of the preparation method of the mesoporous carbon material, the curing condition is that the mesoporous carbon material is cured for 18 to 22 hours at the temperature of between 45 and 55 ℃, cured for 26 to 30 hours at the temperature of between 55 and 65 ℃ and cured for 2 to 4 hours at the temperature of between 95 and 105 ℃; still further preferred; the curing condition is that the curing is carried out for 19 to 21 hours at the temperature of between 48 and 52 ℃, for 27 to 29 hours at the temperature of between 58 and 62 ℃, and for 2.5 to 3.5 hours at the temperature of between 98 and 102 ℃; even more preferred; the curing condition is that the curing is carried out for 20 hours at 50 ℃, 28 hours at 60 ℃ and 2.5-3 hours at 100 ℃.
Further preferably, in the step 3) of the method for producing a mesoporous carbon material, carbonization is performed in a tube furnace.
Further preferably, in the step 3) of the method for producing a mesoporous carbon material, the carbonization is performed in an Ar atmosphere; still more preferably, the flow rate of Ar is 250-350 mL/min; more preferably, the flow rate of Ar is 300 mL/min.
Further preferably, in the step 3) of the preparation method of the mesoporous carbon material, the temperature is raised to 9000-1100 ℃ at the speed of 1-3 ℃/min and then the obtained product is carbonized for 1-3 h; further preferably, the mixture is carbonized for 1 to 3 hours after being heated to 1000 ℃ at the speed of 2 ℃/min; more preferably, the mixture is carbonized for 2 hours after being heated to 1000 ℃ at a rate of 2 ℃/min.
Preferably, in the copper ion treatment method, the diameter of the mesoporous carbon material is 1-6 nm; further preferably, the diameter of the mesoporous carbon material is 2-5 nm; still more preferably, the diameter of the mesoporous carbon material is 3-4.5 nm; still more preferably, the diameter of the mesoporous carbon material is 3.5 to 4.3 nm; more preferably, the diameter of the mesoporous carbon material is 3.93 nm.
Preferably, in the copper ion treatment method, the specific surface area of the mesoporous carbon material is more than or equal to 500m2(ii)/g; more preferably, the mesoporous carbon material has a specific surface area≥600m2(ii)/g; still more preferably, the mesoporous carbon material has a specific surface area of 700m or more2(ii)/g; still more preferably, the mesoporous carbon material has a specific surface area of 700-800m2(ii)/g; more preferably, the mesoporous carbon material has a specific surface area of 750-760m2(ii)/g; the specific surface area is obtained by the BET test.
Preferably, in the copper ion treatment method, the electric adsorption device comprises an upper die, a middle die and a lower die; the upper die and the middle die are detachably connected; the upper die and the lower die are respectively provided with a conductor.
More preferably, in the electric absorption device, a mesoporous carbon material is arranged at the connecting part of the middle die and the upper die; still more preferably, the mesoporous carbon material is in contact with the electrical conductor in the upper mold.
Further preferably, in the electric absorption device, the edges of the upper die, the middle die and the lower die are connected in a sealing manner; still further preferably, movable polytetrafluoroethylene cutting sleeves are adopted among the upper die, the middle die and the lower die for sealing.
Further preferably, in the electric adsorption device, the electric conductor is a titanium sheet and/or a titanium wire; still further preferably, the electric conductor is a titanium sheet and a titanium wire; the titanium sheet is positioned inside the electric adsorption device; the titanium wire is positioned outside the electric adsorption device.
More preferably, in the electric absorption device, the thickness of the titanium sheet is 2-3 mm; still more preferably, the titanium plate has a thickness of 2.3 mm.
More preferably, in the electric absorption device, the diameter of the titanium sheet is more than or equal to 10 mm; still further preferably, the diameter of the titanium sheet in the upper die is 10-1000 mm; still further preferably, the diameter of the titanium sheet in the upper die is 10-100 mm; more preferably, the diameter of the titanium sheet in the upper die is 10-50 mm; still more preferably, the titanium sheet in the upper die has a diameter of 30 mm.
Further preferably, in the electric absorption device, the diameter of the titanium sheet in the lower die is 10-1000 mm; still further preferably, the diameter of the titanium sheet in the lower die is 10-100 mm; still further preferably, the diameter of the titanium sheet in the lower die is 10-30 mm; still more preferably, the diameter of the titanium sheet in the lower die is 20 mm.
More preferably, in the electric absorption device, the diameter of the titanium wire is 0.3-0.8 mm; further preferably, the diameter of the titanium wire is 0.4-0.6 mm; still more preferably, the diameter of the titanium wire is 0.5 mm.
Preferably, the method for treating copper ions further comprises a step of regenerating the mesoporous carbon material, which comprises the following steps: after the mesoporous carbon material adsorbs copper ions, the electrodes of the electric adsorption device are reversely connected, and then the salt solution passes through the electric adsorption device to realize desorption and regeneration of the mesoporous carbon material.
Preferably, in the step of regenerating the mesoporous carbon material, the salt solution is one or more of a sodium sulfate solution, a sodium chloride solution, a potassium chloride solution and a sodium nitrate solution; still further preferably, the salt solution is one of a sodium sulfate solution and a sodium chloride solution; still more preferably, the salt solution is a sodium sulfate solution.
Further preferably, in the step of regenerating the mesoporous carbon material, the temperature of the salt solution is 50-100 ℃; still further preferably, the temperature of the salt solution is 60-100 ℃; even more preferably, the temperature of the salt solution is 80-90 ℃.
Further preferably, in the regeneration step of the mesoporous carbon material, the concentration of the salt solution is 1-30 g/L; still further preferably, the concentration of the salt solution is 1.5-25 g/L; even more preferably, the concentration of the salt solution is 2-20 g/L.
Preferably, in the step of regenerating the mesoporous carbon material, the flow rate of the salt solution is 5-30 mL/min; still further preferably, the flow rate of the solvent is 8-25 mL/min; even more preferably, the flow rate of the salt solution is 10-20 mL/min.
Further preferably, in the regeneration step of the mesoporous carbon material, the desorption time is 0.5-5 h; still further preferably, the desorption time is 0.5-3 h; even more preferably, the desorption time is between 0.5 and 2 h.
Further preferably, in the regeneration step of the mesoporous carbon material, the desorption voltage is 0-8.0V; still further preferably, the desorption voltage is 0-6.0V; even more preferably, the desorption voltage is 0-5.0V.
The invention has the beneficial effects that:
the raw materials required by the electro-adsorption are wide in source and low in price, the treatment process is controllable, and the mass preparation of products is easy to realize.
The treatment method is simple and easy to implement, the requirement on required equipment is low, and the electric adsorption effect on the copper ions in the water is good under the condition of low voltage.
The mesoporous carbon material for adsorbing copper ions can be effectively regenerated, realizes cyclic adsorption treatment of wastewater, and has a very good industrial application prospect.
Drawings
FIG. 1 is a schematic diagram of a mesoporous carbon material prepared in example 1.
Fig. 2 is a schematic view of an electro-adhesion device.
Fig. 3 is a physical diagram of the electro-adhesion device.
FIG. 4 is a graph showing the adsorption effect of the mesoporous carbon material after adsorption regeneration in example 32.
The attached figure 2 marks:
310-upper die, 311-water outlet, 320-middle die, 330-lower die, 331-water inlet, 340-electric adsorption material, 350-electric conductor, 351-titanium sheet and 352-titanium wire.
Detailed Description
The present invention will be described in further detail with reference to specific examples. The starting materials or apparatuses used in the examples and comparative examples were obtained from conventional commercial sources or may be obtained by a method of the prior art, unless otherwise specified. Unless otherwise indicated, the testing or testing methods are conventional in the art.
Example 1
The preparation method of the mesoporous carbon material comprises the following steps:
adding 45g of resorcinol and 18.75g of block polyether F127 into 300mL of 50 wt% ethanol solution, stirring for 15min, adding 1.56g of 1,6 hexamethylene diamine, continuing stirring for 45min, adding 61.5mL of 37 wt% formaldehyde solution, stirring for 20min, putting the mixture into a container, curing for 20h at 50 ℃, curing for 28h at 60 ℃ and curing for 3h at 100 ℃ in an oven to obtain the solid reactant phenolic resin. And (3) putting the solid reactant into a tube furnace, heating to 1000 ℃ at the speed of 2 ℃/min under the Ar atmosphere of 300mL/min, and carbonizing for 2h to obtain the mesoporous carbon material for electro-adsorption of copper ions, wherein a physical diagram of the mesoporous carbon material is shown in figure 1.
Examples 2-32 below electroadsorption experiments were performed using the electroadsorption apparatus shown in fig. 2, which is shown in fig. 3. The electric adsorption device consists of an upper die, a middle die and a lower die, wherein electric conductors are arranged in the upper die and the lower die, mesoporous carbon materials are arranged in the electric adsorption device and are in contact with the electric conductors in the upper die, the middle die and the lower die are sealed by movable polytetrafluoroethylene clamping sleeves, a water inlet is formed in one end of the lower die, and a water outlet is formed in one end of the upper die; the inner diameters of the upper die and the lower die are both 50mm, and the inner diameter of the middle lower part of the middle die is 18 mm; the electric conductor is a titanium sheet and a titanium wire, the titanium sheet is positioned inside the electric adsorption device, the titanium wire is positioned outside the electric adsorption device, the thickness of the titanium sheet is 2.3mm, the diameter of the titanium sheet in the upper die is 30mm, the diameter of the titanium sheet in the lower die is 20mm, and the diameter of the titanium wire is 0.5 mm.
And the copper ion solution enters the electric adsorption device through a water inlet of the lower die, sequentially passes through the lower die, the middle die and the upper die of the electric adsorption device and is discharged from a water outlet of the upper die, and the copper in the copper ion solution is adsorbed by the mesoporous carbon material in the electric adsorption device to realize the removal of the copper ions. The electrochemical workstation is connected with the titanium wires in the upper die and the lower die and provides voltage for the electro-adsorption device. The mesoporous carbon materials according to examples 2 to 32 below were prepared by the method for preparing the mesoporous carbon material according to example 1.
Example 2
1.0565g of mesoporous carbon material is used as an adsorbent, a copper nitrate solution with the initial concentration of 200mg/L is selected as an adsorption solution, and an experiment for removing copper ions by adsorption is started under the conditions that the solution flow is 2mL/min, the initial pH value is 5.2 and no voltage exists. After the copper nitrate solution is adsorbed for 2 hours, the concentration change of the copper nitrate solution is measured by a conductivity meter, and the electric adsorption quantity of the copper nitrate solution is 7.46mg/g according to the analysis result.
Example 3
0.9998g of mesoporous carbon material is used as an adsorbent, a copper nitrate solution with the initial concentration of 200mg/L is selected as an adsorption solution, and an experiment of removing copper ions by electro-adsorption is started under the conditions that the solution flow is 2mL/min, the initial pH value is 5.2, and 0.5V voltage is applied. After absorbing for 2h, measuring the concentration change of the copper nitrate solution by a conductivity meter, and analyzing to obtain the electro-absorption amount of 68.85mg/g of the copper nitrate solution.
Example 4
1.0912g of mesoporous carbon material was used as an adsorbent, a copper nitrate solution with an initial concentration of 200mg/L was selected as an adsorption solution, and an experiment for removing copper ions by electro-adsorption was started under the conditions that the solution flow rate was 2mL/min, the initial pH value was 5.2, and a voltage of 5.0V was applied. After the copper nitrate solution is adsorbed for 2 hours, the concentration change of the copper nitrate solution is measured by a conductivity meter, and the electric adsorption quantity of the copper nitrate solution is 20.33mg/g according to the analysis result.
Example 5
1.1744g of mesoporous carbon material was used as an adsorbent, a copper nitrate solution with an initial concentration of 10mg/L was selected as an adsorption solution, and an experiment for removing copper ions by electro-adsorption was started under the conditions that the solution flow rate was 2mL/min, the initial pH value was 5.2, and a voltage of 0.5V was applied. After adsorbing for 2h, the concentration change of the copper nitrate solution is measured by a conductivity meter, and the electric adsorption quantity of the copper nitrate solution is 8.23mg/g according to the analysis result.
Example 6
1.2104g of mesoporous carbon material was used as an adsorbent, a copper nitrate solution with an initial concentration of 1000mg/L was selected as an adsorption solution, and an experiment for removing copper ions by electro-adsorption was started under the conditions that the solution flow rate was 2mL/min, the initial pH value was 5.2, and a voltage of 0.5V was applied. After absorbing for 2h, measuring the concentration change of the copper nitrate solution by a conductivity meter, and analyzing the result to obtain the electro-absorption amount of the copper nitrate solution of 56.79 mg/g.
Example 7
1.2271g of mesoporous carbon material was used as an adsorbent, a copper nitrate solution with an initial concentration of 200mg/L was selected as an adsorption solution, and an experiment for removing copper ions by electro-adsorption was started under the conditions that the solution flow rate was 1mL/min, the initial pH value was 5.2, and a voltage of 0.5V was applied. After adsorbing for 2h, measuring the concentration change of the copper nitrate solution by a conductivity meter, and analyzing the result to obtain the electro-adsorption quantity of the copper nitrate solution reaching 50.12 mg/g.
Example 8
1.2621g of mesoporous carbon material was used as an adsorbent, a copper nitrate solution with an initial concentration of 200mg/L was selected as an adsorption solution, and an experiment for removing copper ions by electro-adsorption was started under the conditions that the solution flow rate was 50mL/min, the initial pH value was 5.2, and a voltage of 0.5V was applied. After the copper nitrate solution is adsorbed for 2 hours, the concentration change of the copper nitrate solution is measured by a conductivity meter, and the electric adsorption quantity of the copper nitrate solution is 23.88mg/g according to the analysis result.
Example 9
1.2096g of mesoporous carbon material is used as an adsorbent, a copper nitrate solution with the initial concentration of 200mg/L is selected as an adsorption solution, and HNO is used at the solution flow rate of 2mL/min3The experiment for removing copper ions by electro-adsorption was started under the conditions that the pH of the copper nitrate solution was adjusted to 2 and 0.5V was applied. After adsorbing for 2h, the relationship between the luminosity and the concentration is measured by a flame atomic absorption spectrophotometer, and the result of analysis shows that the electro-adsorption quantity of the copper nitrate solution reaches 5.77 mg/g.
Example 10
1.3165g of mesoporous carbon material was used as an adsorbent, a copper nitrate solution with an initial concentration of 200mg/L was selected as an adsorption solution, and an experiment for removing copper ions by electro-adsorption was started under the conditions that the solution flow rate was 2mL/min, the pH of the copper nitrate solution was adjusted to 6 using NaOH, and a voltage of 0.5V was applied. After adsorbing for 2h, the relationship between the luminosity and the concentration is measured by a flame atomic absorption spectrophotometer, and the result of analysis shows that the electro-adsorption quantity of the copper nitrate solution reaches 38.65 mg/g.
Example 11
1.2241g of mesoporous carbon material is used as an adsorbent, copper sulfate solution with the initial concentration of 200mg/L is selected as adsorption solution, and the experiment of removing copper ions by electro-adsorption is started under the conditions that the solution flow is 2mL/min, the initial pH value is 5.2 and 0.5V voltage is applied. After adsorbing for 2h, the concentration change of the copper sulfate solution is measured by a conductivity meter, and the electric adsorption quantity of the copper sulfate solution is 26.37mg/g according to the analysis result.
Example 12
1.2606g of mesoporous carbon material is used as an adsorbent, a copper chloride solution with the initial concentration of 200mg/L is selected as an adsorption solution, and an experiment of removing copper ions by electro-adsorption is started under the conditions that the solution flow is 2mL/min, the initial pH value is 5.2, and 0.5V voltage is applied. After the absorption is carried out for 2 hours, the concentration change of the copper chloride solution is measured by a conductivity meter, and the electric absorption amount of the copper chloride solution is 38.46mg/g according to the analysis result.
Example 13
1.2422g of mesoporous carbon material was used as an adsorbent, a copper nitrate solution with an initial concentration of 200mg/L was selected as an adsorption solution, and an experiment for removing copper ions by electro-adsorption was started under the conditions that the solution flow rate was 2mL/min, the initial pH value was 5.2, and a voltage of 0.8V was applied. After the copper nitrate solution is adsorbed for 2 hours, the concentration change of the copper nitrate solution is measured by a conductivity meter, and the electric adsorption quantity of the copper nitrate solution is up to 29.56mg/g according to the analysis result.
Example 14
1.4255g of mesoporous carbon material was used as an adsorbent, a copper nitrate solution with an initial concentration of 200mg/L was selected as an adsorption solution, and an experiment for removing copper ions by electro-adsorption was started under the conditions that the solution flow rate was 2mL/min, the initial pH value was 5.2, and a voltage of 1.0V was applied. After the copper nitrate solution is adsorbed for 2 hours, the concentration change of the copper nitrate solution is measured by a conductivity meter, and the electric adsorption quantity of the copper nitrate solution is up to 29.00mg/g according to the analysis result.
Example 15
1.3546g of mesoporous carbon material was used as an adsorbent, a copper nitrate solution with an initial concentration of 200mg/L was selected as an adsorption solution, and an experiment for removing copper ions by electro-adsorption was started under the conditions that the solution flow rate was 2mL/min, the initial pH value was 5.2, and a voltage of 0.5V was applied. After the copper nitrate solution is adsorbed for 0.1 hour, the concentration change of the copper nitrate solution is measured by a conductivity meter, and the electric adsorption quantity of the copper nitrate solution is 11.79mg/g according to the analysis result.
Example 16
1.2969g of mesoporous carbon material was used as an adsorbent, a copper nitrate solution with an initial concentration of 200mg/L was selected as an adsorption solution, and an experiment for removing copper ions by electro-adsorption was started under the conditions that the solution flow rate was 2mL/min, the initial pH value was 5.2, and a voltage of 0.5V was applied. After 4 hours of adsorption, the concentration change of the copper nitrate solution is measured by a conductivity meter, and the electric adsorption quantity of the copper nitrate solution is 33.47mg/g according to the analysis result.
Example 17
1.2715g of mesoporous carbon material was used as an adsorbent, a copper nitrate solution with an initial concentration of 50mg/L was selected as an adsorption solution, and an experiment for removing copper ions by electro-adsorption was started under the conditions that the solution flow rate was 2mL/min, the initial pH value was 5.2, and a voltage of 0.5V was applied. After the copper nitrate solution is adsorbed for 2 hours, the concentration change of the copper nitrate solution is measured by a conductivity meter, and the electric adsorption quantity of the copper nitrate solution is 16.00mg/g according to the analysis result.
Example 18
1.2519g of mesoporous carbon material was used as an adsorbent, a copper nitrate solution with an initial concentration of 500mg/L was selected as an adsorption solution, and an experiment for removing copper ions by electro-adsorption was started under the conditions that the solution flow rate was 2mL/min, the initial pH value was 5.2, and a voltage of 0.5V was applied. After the copper nitrate solution is adsorbed for 2 hours, the concentration change of the copper nitrate solution is measured by a conductivity meter, and the electric adsorption quantity of the copper nitrate solution is 33.35mg/g according to the analysis result.
Example 19
1.2765g of mesoporous carbon material is used as an adsorbent, a copper nitrate solution with the initial concentration of 200mg/L is selected as an adsorption solution, and HNO is used at the solution flow rate of 2mL/min3The experiment for removing copper ions by electro-adsorption was started under the conditions that the pH of the copper nitrate solution was adjusted to 3 and 0.5V was applied. After adsorbing for 2h, the relationship between luminosity and concentration is measured by a flame atomic absorption spectrophotometer, and the result of analysis shows that the electro-adsorption quantity of the copper nitrate solution reaches 15.34 mg/g.
Example 20
1.3035g of mesoporous carbon material was used as an adsorbent, a copper nitrate solution with an initial concentration of 200mg/L was selected as an adsorption solution, and an experiment for removing copper ions by electro-adsorption was started under the conditions that the solution flow rate was 6mL/min, the initial pH value was 5.2, and a voltage of 0.5V was applied. After adsorbing for 2h, the concentration change of the copper nitrate solution is measured by a conductivity meter, and the electric adsorption quantity of the copper nitrate solution is up to 30.73mg/g according to the analysis result.
Example 21
1.6237g of mesoporous carbon material was used as an adsorbent, a copper nitrate solution with an initial concentration of 200mg/L was selected as an adsorption solution, and an experiment for removing copper ions by electro-adsorption was started under the conditions that the solution flow rate was 2mL/min, the initial pH value was 5.2, and a voltage of 0.5V was applied. After the absorption is carried out for 1 hour, the concentration change of the copper nitrate solution is measured by a conductivity meter, and the electric absorption amount of the copper nitrate solution is 30.42mg/g according to the analysis result.
Example 22
1.3931g of mesoporous carbon material was used as an adsorbent, a copper nitrate solution with an initial concentration of 200mg/L was selected as an adsorption solution, and an experiment for removing copper ions by electro-adsorption was started under the conditions that the solution flow rate was 2mL/min, the initial pH value was 5.2, and a voltage of 3.0V was applied. After the copper nitrate solution is adsorbed for 2 hours, the concentration change of the copper nitrate solution is measured by a conductivity meter, and the electric adsorption quantity of the copper nitrate solution is 25.80mg/g according to the analysis result.
Example 23
1.2838g of mesoporous carbon material was used as an adsorbent, a copper nitrate solution with an initial concentration of 200mg/L was selected as an adsorption solution, and an experiment for removing copper ions by electro-adsorption was started under the conditions that the solution flow rate was 20mL/min, the initial pH value was 5.2, and a voltage of 0.5V was applied. After absorbing for 2h, measuring the concentration change of the copper nitrate solution by a conductivity meter, and analyzing the result to obtain the electro-absorption amount of the copper nitrate solution of 29.88 mg/g.
Example 24
1.2141g of mesoporous carbon material is used as an adsorbent, a copper nitrate solution with the initial concentration of 200mg/L is selected as an adsorption solution, and HNO is used at the solution flow rate of 2mL/min3The experiment for removing copper ions by electro-adsorption was started under the conditions that the pH of the copper nitrate solution was adjusted to 5 and 0.5V was applied. After adsorbing for 2h, the relationship between the luminosity and the concentration is measured by a flame atomic absorption spectrophotometer, and the result of analysis shows that the electro-adsorption quantity of the copper nitrate solution reaches 53.76 mg/g.
Example 25
1.4004g of mesoporous carbon material was used as an adsorbent, a copper nitrate solution with an initial concentration of 200mg/L was selected as an adsorption solution, and an experiment for removing copper ions by electro-adsorption was started under the conditions that the solution flow rate was 2mL/min, the initial pH value was 5.2, and a voltage of 2.0V was applied. After the copper nitrate solution is adsorbed for 2 hours, the concentration change of the copper nitrate solution is measured by a conductivity meter, and the electric adsorption quantity of the copper nitrate solution is 27.32mg/g according to the analysis result.
Example 26
1.2794g of mesoporous carbon material is used as an adsorbent, a copper nitrate solution with the initial concentration of 200mg/L is selected as an adsorption solution, and HNO is used at the solution flow rate of 2mL/min3The experiment for removing copper ions by electro-adsorption was started under the conditions that the pH of the copper nitrate solution was adjusted to 4 and 0.5V was applied. After adsorbing for 2h, the relationship between the luminosity and the concentration is measured by a flame atomic absorption spectrophotometer, and the result of analysis shows that the electro-adsorption quantity of the copper nitrate solution reaches 39.08 mg/g.
Example 27
1.4255g of mesoporous carbon material was used as an adsorbent, a copper nitrate solution with an initial concentration of 200mg/L was selected as an adsorption solution, and an experiment for removing copper ions by electro-adsorption was started under the conditions that the solution flow rate was 2mL/min, the initial pH value was 5.2, and a voltage of 4.0V was applied. After adsorbing for 2h, measuring the concentration change of the copper nitrate solution by a conductivity meter, and analyzing the result to obtain the electro-adsorption quantity of the copper nitrate solution reaching 22.50 mg/g.
Example 28
1.3235g of mesoporous carbon material was used as an adsorbent, a copper nitrate solution with an initial concentration of 100mg/L was selected as an adsorption solution, and an experiment for removing copper ions by electro-adsorption was started under the conditions that the solution flow rate was 2mL/min, the initial pH value was 5.2, and a voltage of 0.5V was applied. After the copper nitrate solution is adsorbed for 2 hours, the concentration change of the copper nitrate solution is measured by a conductivity meter, and the electric adsorption quantity of the copper nitrate solution is up to 24.33mg/g according to the analysis result.
Example 29
1.2006g of mesoporous carbon material was used as an adsorbent, a copper nitrate solution with an initial concentration of 300mg/L was selected as an adsorption solution, and an experiment for removing copper ions by electro-adsorption was started under the conditions that the solution flow rate was 2mL/min, the initial pH value was 5.2, and a voltage of 0.5V was applied. After the copper nitrate solution is adsorbed for 2 hours, the concentration change of the copper nitrate solution is measured by a conductivity meter, and the electric adsorption quantity of the copper nitrate solution is 31.90mg/g according to the analysis result.
Example 30
1.2736g of mesoporous carbon material was used as an adsorbent, a copper nitrate solution with an initial concentration of 200mg/L was selected as an adsorption solution, and an experiment for removing copper ions by electro-adsorption was started under the conditions that the solution flow rate was 10mL/min, the initial pH value was 5.2, and a voltage of 0.5V was applied. After the copper nitrate solution is adsorbed for 2 hours, the concentration change of the copper nitrate solution is measured by a conductivity meter, and the electric adsorption quantity of the copper nitrate solution is up to 32.52mg/g according to the analysis result.
Example 31
1.2061g of mesoporous carbon material was used as an adsorbent, a copper nitrate solution with an initial concentration of 200mg/L was selected as an adsorption solution, and an experiment for removing copper ions by electro-adsorption was started under the conditions that the solution flow rate was 30mL/min, the initial pH value was 5.2, and a voltage of 0.5V was applied. After the copper nitrate solution is adsorbed for 2 hours, the concentration change of the copper nitrate solution is measured by a conductivity meter, and the electric adsorption quantity of the copper nitrate solution is 27.03mg/g according to the analysis result.
Example 32
1.1605g of mesoporous carbon material is used as an adsorbent, copper sulfate solution with the initial concentration of 200mg/L is selected as adsorption solution, and the experiment of removing copper ions by electro-adsorption is started under the conditions that the solution flow is 2mL/min, the initial pH value is 5.2 and 0.5V voltage is applied. After adsorbing for 2h, Na with the concentration of 10g/L is selected2SO4The solution is used as a solvent in the desorption process, the temperature is 80-90 ℃, the electric desorption experiment is carried out on the copper ions adsorbed by the mesoporous carbon material under the conditions that the solution flow is 20mL/min and the working voltage of 2.0V is reversely connected, and the electric adsorption is carried out again after the desorption is carried out for 1.5 h. After four times of cyclic adsorption and desorption experiments, as shown in fig. 4, the regeneration rate is kept at about 90%, and the cyclic use of the carbon adsorbent is realized, which shows that the material has high regeneration performance.
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 (10)

1. A copper ion treatment method is characterized by comprising the following steps: treating the copper ion solution by adopting an electric adsorption device; mesoporous carbon materials are filled between the positive electrode and the negative electrode of the electric adsorption device.
2. The method according to claim 1, wherein the copper ion concentration of the copper ion solution is 5 to 1500 mg/L.
3. The method according to claim 1, wherein the pH of the copper ion solution is 1 to 7.
4. The method according to claim 1, wherein the flow rate of the copper ion solution passing through the electro-adsorption apparatus is 0.5 to 80 mL/min.
5. The method according to claim 1, wherein the applied voltage of the positive and negative electrodes of the electro-adsorption device is 0 to 8.0V.
6. The method for treating copper ions according to claim 1, wherein the method for preparing the mesoporous carbon material comprises the steps of:
1) mixing phenols, a template agent and an ethanol solution for reaction, and then adding a curing agent for reaction; adding formaldehyde solution to react to obtain a mixture;
2) solidifying the mixture obtained in the step 1) to obtain a solid reactant;
3) carbonizing the solid reactant in the step 2) to obtain the mesoporous carbon material.
7. The copper ion treatment method according to claim 1, wherein the electric adsorption device comprises an upper die, a middle die and a lower die; the upper die and the middle die are detachably connected, and the middle die and the lower die are detachably connected; and the upper die and the lower die are respectively provided with a conductor.
8. The method of claim 7, wherein a mesoporous carbon material is provided at a connecting portion between the middle mold and the upper mold in the electro-adsorption device.
9. The method for treating copper ions according to claim 8, wherein the mesoporous carbon material is in contact with the electric conductor in the upper mold in the electric adsorption device.
10. The method for treating copper ions according to claim 1, further comprising a step of regenerating the mesoporous carbon material, specifically as follows: after the mesoporous carbon material adsorbs copper ions, the electrodes of the electric adsorption device are reversely connected, and then the salt solution passes through the electric adsorption device to realize desorption and regeneration of the mesoporous carbon material.
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