CN114105320B - Method for inhibiting electrode surface scaling by utilizing nano/micro-bubble induced scaling substance liquid-phase nucleation - Google Patents
Method for inhibiting electrode surface scaling by utilizing nano/micro-bubble induced scaling substance liquid-phase nucleation Download PDFInfo
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- 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
- C02F1/4602—Treatment of water, waste water, or sewage by electrochemical methods for prevention or elimination of deposits
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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/24—Treatment of water, waste water, or sewage by flotation
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- 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
- C02F1/46104—Devices therefor; Their operating or servicing
- C02F1/46109—Electrodes
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- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F5/00—Softening water; Preventing scale; Adding scale preventatives or scale removers to water, e.g. adding sequestering agents
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- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
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- 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
- C02F1/46104—Devices therefor; Their operating or servicing
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- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/03—Pressure
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- C02F2209/06—Controlling or monitoring parameters in water treatment pH
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- C02F2209/44—Time
Abstract
The invention belongs to the technical field of water treatment, and discloses a method for inhibiting electrode surface scaling by utilizing nano/micro-bubble induced scaling substance liquid-phase nucleation, which comprises the following steps: constructing an electrode with continuous multiple channels and a nano tip covering surface; size regulation and control of generated nanometer and micro bubbles; and controlling the nucleation of the scale forming substances in the liquid phase. The nano-scale and micro-bubble are generated by adding constant current voltage on a multi-channel cathode with a nano-tip structure, and the nano-scale and micro-bubble play double roles, can be used as a nucleation site of scale and a transport carrier of the scale, then form a gas-liquid-solid mixed phase containing scale particles, converge to a liquid-phase surface layer, and separate from the solution along with the mixed phase of the flowing scale of the solution. The method discovers the bubble nucleation principle in the electrochemical process for the first time, realizes the anti-scaling function of the electrode in the water softening process by the electrochemical technology, and ensures that the electrochemical reaction is continuously carried out.
Description
Technical Field
The invention belongs to the technical field of water treatment, and particularly relates to a method for inhibiting electrode surface scaling by utilizing nano/micro-bubble induced scaling substance liquid-phase nucleation.
Background
The scaling phenomenon is very common in circulating water systems with heat exchangers, conveying pipelines and cooling pumps. It can block the pipeline, reduce the heat transfer efficiency of the heat exchange equipment, cause the corrosion of the equipment and waste energy. Therefore, a series of technologies for softening water bodies are developed and include mechanical methods, physical methods, chemical methods, ultrasonic methods, electrochemical methods and the like. The electrochemical technology is considered as a 'green' water softening technology, because no additional reagent is required to be added into the water in the reaction process, no by-product is generated to cause secondary pollution of the water, and the technology is not influenced by treatment environment and conditions, and can be widely used in various occasions.
The main principle of electrochemical water softening is that a certain voltage is applied to an electrode, a large amount of hydroxyl ions are generated at the interface of a cathode and water, bicarbonate ions are promoted to be converted into carbonate ions, and calcium carbonate and magnesium hydroxide near the cathode are supersaturated and precipitated. The precipitation is divided into two parts of nucleation and crystal growth, and the nucleation generally occurs on the surface of the electrode, so that calcium carbonate and magnesium hydroxide are precipitated and then attached to the surface of the electrode. The invention discloses a method for softening a water body and synchronously preparing calcium carbonate whiskers by adopting electrochemistry in a Chinese patent application number of 202110431015.3, and the purpose of softening the water body is achieved by staged electrolysis. Also, the Multi-media coated performance of electrochemical water sensing system in the reference achieves the same objective by controlling the electrode form and optimizing the parameters. However, the above works are to bind the scale on the surface of the electrode, and although the water is successfully softened, the scale deposited on the electrode is not conductive, which affects the performance and service life of the electrode, increases the energy consumption and even completely blocks the electrochemical reaction. In order to solve the problem, various descaling methods have been studied, and chinese patent No. 200620032114.5 discloses an electrochemical reactor operating in an inverted manner, which makes the cathode scale fall off in the inverted manner; the invention discloses a circulating water electrolysis descaling device with the application number of 200910059929.0 and a descaling method, wherein ultrasonic waves are adopted for automatic descaling and cleaning; in addition, the Chinese patent with the application number of 202110581157.8 is a rotary electrochemical continuous descaling device, and the Chinese patent with the application number of 202110715978.6 is an electrochemical water treatment device with a descaling function, and a scraper is used for physically removing scale on the surface of an electrode.
The essence of the methods is that the scale covered on the surface of the electrode is removed, the method does not have the self-descaling capability, and the scale generated on the surface of the cathode after the method is used for a period of time can only be added with additional equipment for descaling, or the scale layer is cleaned by adopting a physical method or a manual mode after the device is stopped. This also makes the use of electrochemical techniques cumbersome, adds additional processing costs, and limits their use.
Disclosure of Invention
The invention aims to provide a method for inhibiting the electrode surface from scaling by utilizing liquid-phase nucleation of a nano/micro-bubble induced scaling substance. The method overcomes the problem of electrode scaling in the traditional electrochemical technology water softening process, utilizes the nanometer tip structure of the multi-channel electrode to control the bubbles generated by the cathode in nanometer and micron sizes, and the nanometer and micro bubbles are continuously released from the surface of the electrode, thereby preventing the scale from nucleating on the surface of the electrode on the one hand, and preventing the nanometer and micro bubbles which are diffused to the solution from being taken as the nucleation sites of the scale on the other hand, so that the nucleation is far away from the surface of the electrode instead of being attached to the surface of the electrode. And moreover, the nano-scale and micro-bubble are used as nucleation sites, and formed scale crystals are difficult to grow, are easy to adhere to the bubbles and float to the water surface, and can be separated from the solution in an overflow mode. The method realizes the anti-scaling function of the electrode in the water softening process by the electrochemical technology for the first time, and ensures that the electrochemical reaction is continuously carried out.
A method for inhibiting electrode surface scaling by utilizing nano/micro-bubble induced scaling substance liquid-phase nucleation, which comprises the following steps:
(1) Constructing an electrode with continuous multiple channels and a nano tip covering surface;
preparing an electrode covered with a nanometer tip structure on the surface of a material with a continuous channel structure inside on the basis of the material, and then preparing the electrode on the surface of the material by etching, anodic oxidation, a template method, spraying or an electrophoresis method;
the newly constructed electrochemical water treatment device can directly adopt an electrode with continuous multiple channels and a nano tip covering surface; for the existing electrochemical water treatment device, the electrode can be directly replaced by an electrode with continuous multiple channels and a nano tip covering surface;
(2) Size regulation of generated nanometer and micro-bubble;
the size regulating diameter range of the generated nanometer and micro-bubble is 0.001-300 mu m, and the corresponding current density is 1-120 mA/cm 2 ；
(3) Controlling the nucleation of the scale forming substances in the liquid phase;
decomposing water and hydrogen ion consumption in water solution through cathode electrochemical process, regulating the nucleation environment of scale forming matter in the solution to be alkaline, controlling the pH value of the solution to be 7-14, and controlling the corresponding current density to be 1～120mA/cm 2 ；
The surface tension of the solution is less than 0.0728N/m under the action of bubbles and water, the solution passes through an electrode channel in a continuous flow state, and at the moment, a solid-scale forming substance, liquid-water, gas-hydrogen/carbon dioxide mixed phase is suspended on the surface layer of the solution in a mist form, so that the liquid-phase nucleation of the scale forming substance induced by nano-micro-bubbles is realized.
The material with the continuous channel structure can be a wire mesh, and the aperture range of the wire mesh is 0.001-2 mm; or foam carbon, porous carbon and nano carbon with a multi-channel structure, wherein the equivalent diameter of the channel is 0.001-2 mm.
The metal wire mesh is made of iron, copper, aluminum, titanium, zinc, nickel, stainless steel, various alloys and the like.
The diameter of the metal wire mesh is smaller than 2mm.
The foam carbon, the porous carbon and the nano carbon can be cellulose, lignin, carbon nano tubes, carbon nano rods, glass fibers, calcined biomass materials and the like.
The effective diameter of the nano tip structure is 1-500 nm, and the length is less than 100 mu m.
Compared with the prior art, the method for inhibiting the electrode surface from scaling by utilizing the liquid-phase nucleation of the nano and micro bubble induced scaling substance has the characteristics that:
(1) The nanometer tip porous electrode can generate a large amount of nanometer and micro bubbles;
(2) The nanometer and the micro-bubble play double roles, and can be used as a nucleation site of the scale and a transportation carrier of the scale;
(3) When water is softened by an electrochemical method, the scale formation on the surface of the electrode is inhibited, so that the continuous proceeding of the electrochemical reaction is ensured.
Drawings
FIG. 1 is a method and schematic diagram for inhibiting the scaling on the surface of an electrode by using nano/micro-bubble induced liquid-phase nucleation of a scaling substance according to the present invention.
Figure 2 is a scanning electron microscope image of a multi-channel nanotip cathode.
FIG. 3 shows the presence of scale according to the invention.
Fig. 4 shows the voltage variation trend of the nano-copper mesh and the copper plate during the long-term operation.
Detailed Description
In order to further illustrate the present invention, the following examples are given in detail, but they should not be construed as limiting the scope of the present invention.
Example 1
The preparation method of the multi-channel nanometer tip cathode comprises the following steps:
(1) Pretreatment of the copper wire mesh substrate: and (3) putting the copper wire mesh with the aperture of 1mm into 0.5mol/L hydrochloric acid to remove an apparent oxide layer, then carrying out ultrasonic treatment in an ethanol solution for 10min, and then soaking in 1mol/L sodium hydroxide solution for 30min to remove pollutants on the surface of the material.
(2) Anodic oxidation: then controlling the current density to be 15mA/cm in 2mol/L sodium hydroxide electrolyte at the constant temperature of 40 DEG C 2 And oxidizing the anode for 10min to obtain the cathode with the nanometer tip, as shown in figure 2.
The average length of the prepared nanotip structures was about 23 μm and the effective diameter was about 150nm.
Then, taking the multichannel nanotip as a cathode, taking a material of a ruthenium iridium titanium loaded active layer with a titanium wire mesh as a substrate as an anode, continuously enabling cooling circulating water with the hardness of 1500mg/L to pass through the multichannel nanotip cathode, and adjusting the current density to 10mA/cm 2 At this time, dense bubbles are generated on the surface of the multi-channel nanotip cathode and in the solution, the average particle size of 89% of the bubbles is less than 6.9 μm measured by a laser particle size analyzer, after a period of time, the pH value of the solution rises from the initial 5.6 to 13.5, at this time, a solid-liquid-gas mixed phase separated from the surface of the cathode appears in the solution, and the solid-liquid-gas mixed phase floats to the surface of the solution to generate agglomeration, as shown in fig. 3. And drying the mixed phase, performing XPS and EDS characterization to obtain main elements of Ca, mg, C and O of the substance, and judging that the main components of the scale are calcium carbonate of calcite crystals and aragonite crystals through XRD analysis. After 30min reaction, the removal rate of hardness in effluent is 55%.
As shown in FIG. 4, at the same current density, 10mA/cm 2 Comparing the voltage change in the process of treating the cooling circulating water by the copper plate and the nano-tip copper mesh, the voltage of the nano-copper mesh electrode is stabilized at 4.8V along with the reaction, and the fluctuation is small. While the copper plate electrode had a significant increase in voltage after 12h of operation and increased to 6.5V after 24h, the electrode surface was heavily fouled.
Claims (3)
1. A method for inhibiting electrode surface scaling by utilizing nano/micro-bubble induced scaling substance liquid phase nucleation is characterized by comprising the following three conditions:
(1) Constructing an electrode with continuous multiple channels and a nano tip covering surface;
preparing an electrode covered with a nanometer tip structure on the surface of a material with a continuous channel structure inside by etching, anodic oxidation, a template method, spraying or an electrophoresis method;
for the newly constructed electrochemical water treatment device, an electrode with continuous multiple channels and a nano tip covering surface is directly adopted; for the existing electrochemical water treatment device, the electrode is directly replaced by an electrode with continuous multiple channels and a nano tip covering surface;
the material with the continuous channel structure is a wire mesh, and the aperture range of the wire mesh is 0.001 to 2mm; or the composite material contains foam carbon, porous carbon and nano carbon with a multi-channel structure, and the equivalent diameter of the channel is 0.001 to 2mm;
the diameter of the metal wire mesh is less than 2mm;
the effective diameter of the nano tip structure is 1 to 500nm, and the length of the nano tip structure is less than 100 mu m;
(2) Size regulation and control of generated nanometer and micro bubbles;
regulating and controlling the current density to be 1 to 120mA/cm 2 Controlling the size of generated nano micro bubbles to regulate and control the diameter range to be 0.001 to 300 mu m;
(3) Controlling the nucleation of the scale forming substances in the liquid phase;
regulating and controlling the current density to be 1 to 120mA/cm 2 By cathodic electrochemical processes for the decomposition of hydrogen ions in water and aqueous solutionsRegulating the nucleation environment of a scale forming substance of the solution to be alkaline, and controlling the pH value range of the solution to be 7 to 14;
the surface tension of the solution is less than 0.0728N/m under the action of bubbles and water, the solution passes through an electrode channel in a continuous flow state, and at the moment, a solid-scale forming substance, liquid-water, gas-hydrogen gas/carbon dioxide mixed phase is suspended on the surface layer of the solution in a mist form, so that the liquid-phase nucleation of the scale forming substance induced by nano-micro-bubbles is realized.
2. The method of claim 1, wherein the wire mesh is iron, copper, aluminum, titanium, zinc, nickel, stainless steel, or an alloy.
3. The method according to claim 1 or 2, wherein the carbon foam, porous carbon, nanocarbon is cellulose, lignin, carbon nanotubes, carbon nanorods, glass fibers, or calcined biomass material.
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Citations (4)
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| GB1484974A (en) * | 1974-02-01 | 1977-09-08 | Swift & Co | Purification by bubble floatation of water containing suspended and or dissolved impurities |
| CN102396093A (en) * | 2009-02-17 | 2012-03-28 | 麦卡利斯特技术有限责任公司 | Apparatus and method for controlling nucleation during electrolysis |
| CN113549943A (en) * | 2021-08-16 | 2021-10-26 | 中国石油化工股份有限公司 | Water electrolysis hydrogen production device and method with fractal reinforced surface |
| CN113716658A (en) * | 2021-09-27 | 2021-11-30 | 大连理工大学 | Preparation method of ruthenium, iridium and titanium ternary metal mesh electrode containing nano tip structure |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6884866B2 (en) * | 2001-10-19 | 2005-04-26 | Avant Immunotherapeutics, Inc. | Bulk drying and the effects of inducing bubble nucleation |
| CN2586689Y (en) * | 2002-10-15 | 2003-11-19 | 上海同济建设科技有限公司 | Electrical flotation waste water treatment apparatus |
| JP2007075674A (en) * | 2005-09-12 | 2007-03-29 | Matsushita Electric Ind Co Ltd | Microbubble generator and sanitary washing device equipped with it |
| CN205892793U (en) * | 2016-07-08 | 2017-01-18 | 福建方明环保科技股份有限公司 | Take bubble generating device's air supporting device |
| FI128091B (en) * | 2018-04-22 | 2019-09-13 | Timo Korpela | Combiflotation for purification and disinfection of waste water |
| CN113772787B (en) * | 2021-09-27 | 2022-10-21 | 大连理工大学 | Electrochemical filter for removing total nitrogen in water |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1484974A (en) * | 1974-02-01 | 1977-09-08 | Swift & Co | Purification by bubble floatation of water containing suspended and or dissolved impurities |
| CN102396093A (en) * | 2009-02-17 | 2012-03-28 | 麦卡利斯特技术有限责任公司 | Apparatus and method for controlling nucleation during electrolysis |
| CN113549943A (en) * | 2021-08-16 | 2021-10-26 | 中国石油化工股份有限公司 | Water electrolysis hydrogen production device and method with fractal reinforced surface |
| CN113716658A (en) * | 2021-09-27 | 2021-11-30 | 大连理工大学 | Preparation method of ruthenium, iridium and titanium ternary metal mesh electrode containing nano tip structure |
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