KR101029090B1 - Capacitive Deionization Electrode using ion-exchangeable engineering plastic and Its Manufacturing Method Thereof - Google Patents
Capacitive Deionization Electrode using ion-exchangeable engineering plastic and Its Manufacturing Method Thereof Download PDFInfo
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- KR101029090B1 KR101029090B1 KR1020090073808A KR20090073808A KR101029090B1 KR 101029090 B1 KR101029090 B1 KR 101029090B1 KR 1020090073808 A KR1020090073808 A KR 1020090073808A KR 20090073808 A KR20090073808 A KR 20090073808A KR 101029090 B1 KR101029090 B1 KR 101029090B1
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Abstract
The present invention comprises the steps of: a) preparing a slurry by mixing engineering plastics, an electrode active material and an organic solvent having an ion exchange functional group; b) applying the slurry to a current collector; And c) drying the current collector to which the slurry is applied; It relates to a method for producing a capacitive desalination electrode, including a. In addition, the present invention is a negative electrode electrode coated with a current collector slurry of engineering plastics, an electrode active material and an organic solvent having a cation exchanger; Anode electrode which apply | coated the slurry which mixed the engineering plastics, an electrode active material, and organic solvent which have an anion exchanger to an electrical power collector; Or the cathode electrode and the anode electrode; It relates to a capacitive desalination remover provided.
The present invention has the advantage of high adsorption and desorption efficiency of ions during the process operation while increasing the adsorption capacity of the electrode, and the manufacturing process is simple as a stable electrode in water without crosslinking reaction.
Sulfonated Engineering Plastics, Capacitive Desalting Electrodes, CDI Electrodes, Desalting
Description
The present invention relates to a capacitive desalination electrode (CDI electrode) having an ion exchange functional group and stable in water without crosslinking reaction, and a method of manufacturing the same.
In particular, the present invention provides a capacitive desalination electrode and a method of manufacturing the electrode having a high adsorption capacity and a high efficiency of adsorption and desorption of ions in the process of operation, stable in water without crosslinking reaction, and a simple electrode manufacturing process. Specifically, in the process of desorption of the adsorbed ions, ions of opposite charges move to the electrode to reduce the adsorption efficiency, and provide a stable capacitive desalination electrode (CDI electrode) in water without a crosslinking process and a manufacturing method thereof. It is.
In the production of domestic and industrial water, desalination technology plays an important role in determining human health, process efficiency and product performance.
Long-term drinking of water containing heavy metals, nitrate nitrogen, and fluoride ions can have a devastating effect on health. In addition, hard water, such as the number of boilers containing hard materials, can cause scale in boilers or heat exchangers, which can greatly reduce the efficiency of the process. It is an important factor in determining this.
Currently, ion exchange methods using ion exchange resins are widely used to remove ionic substances in aqueous solutions. Although this method can effectively separate most ionic materials, a large amount of acid or basic materials are used in the process of regenerating the ion exchanged resin, and a large amount of waste liquid is generated in the regeneration process.
Another method of removing ionic substances is separation membrane technology such as reverse osmosis or electrodialysis. However, problems such as reduced treatment efficiency due to membrane fouling, cleaning of contaminated membranes, and periodic membrane replacement Holding it.
Recently, in order to solve the problems of the existing desalination techniques, capacitive desalination techniques using the principle of electric double layer have been studied and applied to the desalination process.
Capacitive desalination operates at low electrode potentials (about 1 to 2 V) because it utilizes the adsorption reaction of ions by electrical attraction in the electrical double layer formed on the electrode surface when potential is applied to the electrode, resulting in energy consumption. Compared with other desalination technology, it is evaluated as the next generation desalination technology with low energy consumption.
In the CDI process, when an electrode potential of 1 to 2 volts (V) is applied, ionic substances in the influent are removed by an adsorption reaction in an electric double layer formed on the electrode surface. When the adsorbed ions reach the capacitance of the electrode, the electrode potential is changed to zero volts (0 V), or the opposite potential, and the adsorbed ions are desorbed to regenerate the electrode.
However, in the case of CDI electrode without ion selectivity, when adsorption and desorption occurs, the sudden change of electrode potential causes ions adsorbed on the electrode and ions of opposite charge to move to the electric double layer, so that the adsorbed ions do not desorb and remain on the electrode surface. This causes a problem of reducing the adsorption efficiency of the electrode. In order to solve this problem, when the electrode is manufactured by adhering the cation exchange membrane and the anion exchange membrane to the anode, the absorption and desorption efficiency can be reduced, but the manufacturing cost of the electrode is too high.
In addition, an electrode may be manufactured using an ion exchange resin binder solution to prepare a CDI electrode having ion selectivity. However, to produce a CDI electrode having ion selectivity and high electrical conductivity, it must have a sufficiently high ion exchange capacity. If the ion exchange capacity is high, the crosslinking reaction is deteriorated due to poor safety in water, and if the value of the ion exchange capacity is small, the conductivity value is lowered and the selectivity of the ions and the electrode efficiency are lowered.
As a result of much research in order to further maximize the above-mentioned advantages and to solve the disadvantages, the present invention provides a capacitive electrode prepared by preparing a slurry mixed with an engineering plastic having an ion exchange functional group and coating a current collector. The present invention has been accomplished by increasing the adsorption capacity of the electrode as a desalination electrode (CDI electrode), thereby making it possible to manufacture a stable CDI electrode in water without high cross-linking reaction and adsorption and desorption efficiency of ions in the process of operation.
Accordingly, the present invention provides a CDI electrode and a method of manufacturing the same, which is used in a capacitive desalination apparatus having a very good desorption efficiency in living water or industrial water, because the adsorption efficiency of ions is very good.
In addition, the present invention is a new CDI electrode having a very good desorption efficiency of ions when the ions adsorbed on the electrode having an ion exchange functional group reaches the storage capacity of the electrode, when the adsorbed ions are desorbed to regenerate the electrode, and a method of manufacturing the same To provide.
The present invention also relates to a CDI electrode having a ion selectivity and capable of efficiently separating and removing cations and anions and a method of manufacturing the same.
The present invention relates to a method for producing a slurry by mixing an electrode active material with an engineering plastic having an ion exchange functional group, and coating and drying the electrode active material on a current collector to produce a capacitive desalination electrode (CDI electrode) having excellent desalination and regeneration efficiency. In addition, the prepared electrode is stable in water without crosslinking reaction.
In addition, the present invention is to prepare a slurry by mixing the electrode active material and the conductive material (conductive material) with the engineering plastic having an ion exchange functional group, and applying and drying it to the current collector to produce a CDI electrode excellent in desalting efficiency and regeneration efficiency. It also relates to a method for producing a CDI electrode by adding an electrolyte also belongs to the scope of the present invention. Capacitive desalination electrode (CDI electrode) according to the present invention is stable in water without additional crosslinking reaction and excellent in the electrical conductivity of the electrode, has the advantage of improving the selectivity, adsorption, desorption efficiency of ions.
Hereinafter, a method of manufacturing a CDI electrode according to the present invention will be described in detail.
The present invention comprises the steps of: a) preparing a slurry by mixing engineering plastics, an electrode active material and an organic solvent having an ion exchange functional group;
b) applying the slurry to a current collector; And
c) drying the current collector to which the slurry is applied;
The present invention relates to a method for manufacturing a capacitive desalination electrode that is prepared, and also to a capacitive desalination removal apparatus including the prepared electrode.
Engineering plastics having ion exchange functional groups are engineering plastics suitable for structural and mechanical parts, and are plastics mainly intended for metal replacement, or plastics used in industrial applications such as automobile parts, mechanical parts, electrical parts, and electronic parts. By means of the tensile strength, flexural modulus, heat resistance and means a polymer capable of ion exchange containing an ion exchange functional group in the polymer that can be used for a long time at high temperatures.
The engineering plastic in step a) is made of polyimide, polyamide, polyarylethersulfone, polysulfone, polyethersulfone, polyetherketone, polyetheretherketone, polysulfoneketone, polyphenylene oxide and polyphenylene sulfide Preference is given to using one or two or more mixtures selected from the group, more preferably one or two or more mixtures selected from the group consisting of polyarylethersulfones, polyetheretherketones and polyetherketones. .
In the step a), the engineering plastic having an ion exchange functional group preferably contains 1 to 30 wt% based on the total solid content of the slurry, and when the content of the engineering plastic having the ion exchange functional group is less than 1 wt%, the slurry is an electrode Not fully binding the active material particles (binding), not only the durability of the produced electrode is lowered, but the applied slurry may be difficult to adhere firmly to the current collector. When it exceeds 30% by weight, the electrical conductivity from the current collector to the electrode active material is lowered, so that the selectivity of the ions and the adsorption power of the ions are lowered.
The slurry prepared in step a) may be mixed with water as a solvent, and thus it is preferable to use a polar organic solvent that is eluted in water. The polar organic solvent may be selected and used according to the type of engineering plastic, and more preferred examples thereof include dimethylformamide, dimethylacetamide, N-methyl-2-pyrrolidone, acetone, chloroform, dichloromethane, and trichloro. Any one or a mixture of two or more selected from ethylene, ethanol, methanol and normal hexane can be used, but is not limited thereto. The slurry is not particularly limited to the total composition, but the total solid content is preferably 1 to 60% by weight, preferably 10 to 40% by weight. When the solids content is less than 1% by weight, the viscosity of the slurry is low to improve flowability, thereby making the electrode surface uniform.However, when the thickness of the electrode is difficult to control, and when it exceeds 60% by weight, the flowability is increased by increasing the viscosity of the slurry. As a result, the thickness of the electrode can be easily adjusted, but the electrode surface may not be uniform. If the solid content is out of the range may not be easy to apply the slurry.
And the electrode active material that can be used in step a) may be an activated carbon-based material or a metal oxide-based material, more specifically, an activated carbon-based material having a high specific surface area, activated carbon powder, activated carbon fiber Any one or a mixture of two or more selected from carbon nanotubes and carbon aerogels may be used, and it is more preferable to use in powder form. And as the metal oxide-based material, preferably any one or a mixture of two or more selected from RuO 2 , Ni (OH) 2 , MnO 2 , PbO 2 , TiO 2 can be used. The electrode active material is not particularly limited, but a particle average particle diameter of 10 nm to 10 μm is preferred because it can increase the specific surface area and capacitance of the electrode. Although the content of the electrode active material is not particularly limited, it is preferable to include 100 to 1100 parts by weight based on 100 parts by weight of the engineering plastic having an exchange functional group, and to produce an electrode having high storage capacity while exhibiting ion selectivity.
The present invention, the ion exchange functional group in step a) sulfonic acid group (-SO 3 H), carboxyl group (-COOH), phosphonic group (-PO 3 H 2 ), phosphonic group (-HPO 2 H) , Abu sonic group (-AsO 3 H 2), cell Reno nikgi least one from the group consisting of (-SeO 3 H) selected cation exchanger; Or ammonium base (-NH 4 ), primary to tertiary amine group (-NH 2 , -NHR, -NR 2 ), quaternary phosphonium group (-PR 4 ), tertiary sulfonium group (-SR 3 ) Anion exchanger selected from the group consisting of at least one; In the present invention, a CDI electrode using a slurry made of a mixture of engineering plastics having a cation exchanger may be used as a negative electrode, and in the case of having an anion exchanger, it may be used as a positive electrode.
In step a), the slurry may be further mixed with the conductive agent, and the conductive material may serve to increase the adsorption and desorption rate of the ions as well as to increase the adsorption of the ions. The conductive agent may be used without limitation as long as it is a conductive material having a low electrical resistance. More specifically, the conductive agent may be acetylene black, ketjen black, superconductive (XCF) carbon, semi-reinforced furnace (SRF). Semi Reinforcing Furnace) One or more mixtures of carbon, conductive polymer, LiCl, NaCl and KCl may be used. The conductive agent is preferably in the form of a powder having an average particle diameter of 10nm ~ 10㎛, it is possible to increase the electrical conductivity of the electrode in the above range. In addition, including 1 to 250 parts by weight based on 100 parts by weight of engineering plastic is good for increasing the electrical conductivity and storage capacity of the desalination electrode according to the present invention, more preferably using 1 to 30 parts by weight based on 100 parts by weight of the electrode active material It is good.
In the step b), it is preferable that the current collector has excellent conductivity so that the electric field can be uniformly distributed on the electrode surface when the current is supplied to the capacitive desalination electrode manufactured through the power supply device. More specific examples may use sheet form, thin film form or plain weave mesh form comprising one or more mixtures from the group consisting of aluminum, nickel, copper, titanium, iron, stainless steel and graphite. The method of applying the slurry in the present invention is not limited by spraying, dip coating, knife casting, doctor blade, spin coating, etc., and the coating thickness is in the range of 50 to 300 μm while reducing the electrical resistance of the electrode while desalting It is preferable to increase the efficiency, but is not limited thereto. In addition, if necessary, by repeating step b) one or more times, a specific thickness electrode may be manufactured. In the present invention, the capacitive desalination electrode prepared after step c) may be processed into an appropriate form.
In step c), the drying is preferably performed at 50 to 150 ° C. after the first drying at room temperature to 110 ° C., which has a good surface smoothness and economical benefits in drying at different temperature ranges. If the drying is less, the electrode surface is not uniform due to sticking during the press work after drying, and the electrode may be damaged. If it is dried too much, it becomes difficult to obtain a constant thickness electrode having a uniform electrode surface during press operation after drying.
In addition, the present invention may further comprise a step of pressing as necessary for the smoothness of the surface after step c). In the pressing step, the compression ratio is about 0.001 to 30% of the thickness of the coating layer dried in step c). It is preferable to compress. When the compressibility exceeds 30%, the density of the electrode surface and the electrode active material is good, but becomes hard and brittle, thus making it difficult to handle. Preferably, the compression ratio of 1 to 25% makes the surface of the electrode uniform and the density of the electrode active material sufficient, so that the reproducibility of the electrode characteristics is excellent. In addition, after the step c) may further comprise the step of applying and drying the slurry prepared in step a), it may be repeatedly applied to ensure a constant thickness of the coating.
The present invention relates to a capacitive desalination removing apparatus employing the prepared capacitive desalination electrode. The desalination cell employing the electrode according to the invention belongs to the category of capacitive desalination removal apparatus. More specifically, the present invention provides a negative electrode electrode coated with a current collector slurry of engineering plastics, an electrode active material and an organic solvent having a cation exchanger; Anode electrode which apply | coated the slurry which mixed the engineering plastics, an electrode active material, and organic solvent which have an anion exchanger to an electrical power collector; Or the cathode electrode and the anode electrode; It relates to a capacitive desalination remover provided. In the capacitive desalination electrode according to the present invention, the engineering plastics, the electrode active material, the conductive agent, the cation exchanger, and the current collector are the same as those used in the capacitive desalination electrode according to the present invention.
The capacitive desalination electrode according to the present invention can be used only in one of the electrodes selected from the positive electrode or the negative electrode, and even if an electrode having no selectivity of ions is employed as the counter electrode, adsorption and desorption of ions can be achieved. Preferably, by employing both the cathode and the anode, the storage capacity is high, and the adsorption and desorption of ions can be facilitated during the operation of the process.
The present invention has the advantage of high adsorption and desorption efficiency of ions during the process operation while increasing the adsorption capacity of the electrode, and the manufacturing process is simple as a stable electrode in water without crosslinking reaction. In addition, since engineering plastics containing aromatics in the main chain are used as binders for electrode active materials, they have high electrical conductivity even at low ion exchange capacity, and are extremely safe for water, so they do not require crosslinking reaction by crosslinking agent. Capacitive desalination electrode (CDI electrode) with durability has the advantage that can be manufactured, and the process can be simplified to reduce the manufacturing cost.
Hereinafter, the present invention will be described in detail with reference to the following examples. However, the present invention is not limited to the following examples.
[Production Example 1]
Cathode manufacturing
Polyethersulfone (PES; Victrex) having a weight average molecular weight of 70,000 to 100,000 is placed in a vacuum oven and dried at 70 ° C. for 24 hours. In a 1 L three-necked flask, 20 g of PES was dissolved in 100 ml of methyl sulfate, 800 ml of 97% aqueous sulfuric acid solution was added, diluted in a nitrogen atmosphere, and reacted at 50 ° C. for 72 hours. Sulfonated PES (S-PES) is precipitated with
After dissolving 1 g of the synthesized S-PES in 20 g of dimethylacetamide (DMAc), 10 g of activated carbon (P-60: Kuraray Chemical. Co., Ltd., Specific surface area; 1600 m 2 / g), carbon black (super -p: Timcal Co., the average particle diameter = 40nm) 1.5g was mixed to prepare a slurry for cation selective electrode coating.
The slurry thus prepared was coated on a conductive graphite sheet (thickness: 130 μm, Dongbang Carbon Co., Ltd., Cat. No. F02511C) with a doctor blade so that the thickness of the coating layer on one side was 220 μm, and then at room temperature. After drying for 3 hours and hot-air drying at 70 ℃ for 30 minutes and roll pressing at 70 ℃ so that the thickness of the coating layer to 200 ㎛ to prepare a negative electrode having a cation selectivity.
[Production Example 2]
Anode manufacturing
Polyethersulfone (PES) (20 g), paraformaldehyde (PFA) (13.56 g), chlorotrie while slowly passing nitrogen gas through a 2 L reactor equipped with a stirrer, nitrogen injector, temperature controller and reflux condenser. Methylsilane (CTMS) (49.2 g) and Tin (IV) chloride (TC) (2.356 g) were added to chloroform (CF) (660 mL), reacted for 72 hours, precipitated in methanol and washed several times with distilled water. Dried.
The dried chloromethylated polyethersulfone (PES) was dissolved in DMAc solvent to make 500 mL of 12% solution, and then 100 g of trimethylamine (TMA), a tertiary amine, and N, N, N ', N'-tetramethyl A mixture of 33.3 g of hexamethylene diamine (TMHDA) was subjected to an amination reaction at 30 ° C. for 48 hours, precipitated in methanol, washed and dried to obtain aminated polyether sulfone (A-PES). At this time, the ion exchange capacity was measured by an acid salt titration method, and was 1.5 meq / g.
After dissolving 1 g of the synthesized aminated polyether sulfone (A-PES) in 20 g of dimethylacetamide (DMAc), activated carbon (P-60: Kuraray Chemical. Co., Ltd., Specific surface area = 1600 m 2 / g) 10g, carbon black (super-p: Timcal Co., carbon black, average particle diameter = 40nm) by mixing 1.5g to prepare a slurry for anion-selective electrode coating.
The slurry thus prepared was coated on a conductive graphite sheet (thickness: 130 μm, Dongbang Carbon Co., Ltd., Cat. No. F02511C) with a doctor blade so that the thickness of the coating layer on one side was 220 μm, and then at room temperature. After drying for 3 hours and heat-treated at 70 ℃ for 30 minutes and roll pressing at 70 ℃ so that the thickness of the coating layer is 200 ㎛ to prepare a positive electrode having an anion selectivity.
[Manufacture example 3]
Preparation of coating solution for cation selective electrode
The prepared S-PES was prepared in 15% DMAc solution to prepare a solution for cation selective electrode coating.
[Production Example 4]
Preparation of Coating Solution for Anion Selective Electrode
The prepared A-PES was prepared in 15% DMAc solution to prepare an anion-selective electrode coating solution.
[Production Example 5]
The electrode prepared in Preparation Example 1 was dip-coated in the coating solution of Preparation Example 3 to prepare a negative electrode having cation selectivity.
Production Example 6
The electrode prepared in Preparation Example 2 was dip coated on the coating solution of Preparation Example 4 to prepare a positive electrode having anion selectivity.
Example 1
The desalination cell was prepared using the electrode prepared in Preparation Example 1 as the cathode, and using the electrode prepared in Preparation Example 2 as the anode.
The prepared electrode was cut into 10 × 10 cm 2 and then equipped with a spacer (200mesh, polyamide) having a thickness of 100 μm to allow fluid to pass therethrough while preventing the two electrodes from contacting between the anode and the cathode. A 1 cm hole was drilled in the center of the electrode to allow the solution to exit the center through the spacer on the slope of the electrode. A 15 x 15 cm 2 sized acrylic plate was placed on the outside of the positive electrode and the negative electrode and bolted to form a single cell for capacitive desalination.
100 mg / L NaCl solution was supplied at a rate of 30 mL / min while the electrode potential was constantly applied at 1.5 V to the desalting cell prepared in Example 1 above. The desalination efficiency was analyzed by measuring the electrical conductivity of the effluent. After adsorbing for 3 minutes, the electrode potential was changed to 0.0 V and desorbed for 2 minutes. Desalting experiments were carried out with the prepared cells as shown in FIGS. 1 and 2.
Figure 1 shows the removal rate (%) of the salt which is the water treatment rate of Example 1 (S-PES / A-SPES).
2 shows changes in current value and voltage value with time during repeated adsorption and desorption of Example 1 (S-PES electrod vs. A-PES electrod).
[Example 2]
The same process as in Example 1, except that the electrode prepared in Preparation Example 5 was used as the cathode, and the electrode prepared in Preparation Example 6 was used as the anode, and the rest was the same as in Example 1. Prepared.
100 mg / L NaCl solution was supplied at a rate of 30 mL / min while the electrode potential of the desalting cell prepared in Example 2 was constantly applied at 1.5 V. The desalination efficiency was analyzed by measuring the electrical conductivity of the effluent. After adsorbing for 3 minutes, the electrode potential was changed to 0.0 V and desorbed for 2 minutes. Desalting experiments were carried out with the prepared cells as shown in FIGS. 1 and 3.
Figure 1 below shows the removal rate (%) of the salt which is the water treatment rate of Example 2 (Recoated S-PES / A-SPES).
3 shows changes in current value and voltage value with time during repeated adsorption and desorption of Example 2 (S-PES recoating vs. A-PES recoating).
As shown in FIG. 1, the desalination cell prepared in Example 1 showed excellent salt removal rate (82%) in aqueous solution, and the desalination cell prepared in Example 2 had excellent salt removal rate (84% in aqueous solution). Can be seen.
As shown in FIGS. 2 and 3, the desalination cells prepared in Examples 1 and 2 have a constant current change with respect to the applied voltage when adsorption and desorption are repeated with time. It can be seen that the adsorption amount and the desorption amount are almost constant and thus have a uniform performance.
Figure 1 shows the removal rate (%) of salt which is the water treatment rate of Example 1 (S-PES / A-SPES), Example 2 (Recoated S-PES / A-SPES).
Figure 2 shows the change of the current value and the voltage value with time during repeated adsorption and desorption of Example 1 (S-PES electrod vs. A-PES electrod).
Figure 3 shows the change of the current value and the voltage value with time during repeated adsorption and desorption of Example 2 (S-PES recoating vs. A-PES recoating).
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| WO2013147380A1 (en) * | 2012-03-29 | 2013-10-03 | 공주대학교 산학협력단 | Specific ion-selective composite carbon electrode for capacitive deionization, and preparation method thereof |
| KR101317472B1 (en) | 2013-04-04 | 2013-10-11 | 주식회사 죽암기계 | Capacitive deionization electrode and manufacturing method thereof |
| WO2013183973A1 (en) * | 2012-06-08 | 2013-12-12 | Sion Tech Co., Ltd | Method of manufacturing capacitive deionization electrode having ion selectivity and cdi electrode module including the same |
| US9758391B2 (en) | 2013-12-24 | 2017-09-12 | Samsung Electronics Co., Ltd. | Capacitive deionization electrodes, capacitive deionization apparatuses including the same, and production methods thereof |
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| WO2013147380A1 (en) * | 2012-03-29 | 2013-10-03 | 공주대학교 산학협력단 | Specific ion-selective composite carbon electrode for capacitive deionization, and preparation method thereof |
| KR101621270B1 (en) | 2012-03-29 | 2016-05-17 | 공주대학교 산학협력단 | Method for manufacturing of specific ion selective composite carbon electrode for capacitive deionization |
| WO2013183973A1 (en) * | 2012-06-08 | 2013-12-12 | Sion Tech Co., Ltd | Method of manufacturing capacitive deionization electrode having ion selectivity and cdi electrode module including the same |
| US10584043B2 (en) | 2012-11-29 | 2020-03-10 | Samsung Electronics Co., Ltd. | Capacitive deionization apparatus and methods of treating fluid using the same |
| KR101317472B1 (en) | 2013-04-04 | 2013-10-11 | 주식회사 죽암기계 | Capacitive deionization electrode and manufacturing method thereof |
| US10023479B2 (en) | 2013-06-12 | 2018-07-17 | Samsung Electronics Co., Ltd. | Capacitive deionization apparatus and methods of treating a fluid using the same |
| US9758391B2 (en) | 2013-12-24 | 2017-09-12 | Samsung Electronics Co., Ltd. | Capacitive deionization electrodes, capacitive deionization apparatuses including the same, and production methods thereof |
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| KR20110016213A (en) | 2011-02-17 |
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