CN111362368A - Preparation method of iron-carbon micro-electrolysis ball - Google Patents
Preparation method of iron-carbon micro-electrolysis ball Download PDFInfo
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- CN111362368A CN111362368A CN202010169770.4A CN202010169770A CN111362368A CN 111362368 A CN111362368 A CN 111362368A CN 202010169770 A CN202010169770 A CN 202010169770A CN 111362368 A CN111362368 A CN 111362368A
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/46104—Devices therefor; Their operating or servicing
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
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- General Chemical & Material Sciences (AREA)
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Abstract
The invention discloses a preparation method of an iron-carbon micro-electrolysis ball, which comprises the following steps: mixing iron powder, active carbon, fluxing agent sodium hexafluoroaluminate and pore-forming agent sodium chloride according to a certain proportion; ball milling the mixture; heating and melting at high temperature under the protection of nitrogen, and keeping the temperature for 2-5 hours; the molten mass flows out from the aperture of 5mm, the fluid is broken and cooled by spraying from the side surface, and the lower part is cooled by cold water in a flash manner; and soaking in tap water for 1-5 days to obtain the iron-carbon micro-electrolysis ball. The invention utilizes high-temperature melting energy to uniformly mix iron and carbon, greatly increases the number of formed micro batteries, and is beneficial to the degradation of organic matters in wastewater, particularly benzene ring-containing organic matters; rapidly cooling and shrinking the lower surface of the free falling body of the molten mass to form small particle ellipsoids; the pore-forming agent sodium chloride is dissolved in the water to form a plurality of pores, and the longer the service time is, the more the pores are, the better the wastewater degradation effect is. The invention has low requirement on equipment precision, can be produced in large scale, does not use and produce harmful substances and is environment-friendly.
Description
Technical Field
The invention belongs to the field of environmental pollution treatment, and particularly relates to a preparation method of an iron-carbon micro-electrolysis ball, which is used for degrading high-concentration organic sewage.
Background
High-concentration organic wastewater, especially benzene ring-containing organic wastewater, is difficult to reach the national discharge standard by using Fenton oxidation and microbial degradation. With the application of novel technology, the iron-carbon micro-electrolysis method better solves the problem and is gradually applied to the pharmaceutical and chemical industries.
Iron-carbon micro-electricityThe principle of degrading water pollutants is the electric adsorption of iron filings to flocs and the catalytic action of iron filings to reaction. Coagulation of reaction products of countless iron-carbon micro-batteries, adsorption of new flocs, filtration of bed layers and the like. The main functions of the system are oxidation reduction and electric adsorption, the main components of the scrap iron are iron and carbon, when the scrap iron is immersed in electrolyte solution, a countless micro-battery system can be formed due to the 1.2V electrode potential difference between Fe and C, an electric field is formed in the action space, and a large amount of Fe is generated by anode reaction2+Enters the wastewater and is further oxidized into Fe3+So as to form the flocculant with higher adsorption flocculation activity. Cathodic reaction producing large quantities of nascent state [ H ]]And [ O]Under the condition of weak acidity, the active components can generate oxidation-reduction reaction with many components in the waste water to make the organic macromolecules generate chain-breaking degradation, so that the chromaticity of organic matters, especially printing and dyeing waste water, is eliminated, the biochemical degree of the waste water is improved, and a large amount of H is consumed by cathode reaction+A large amount of OH is generated-This also increases the pH of the wastewater.
The iron-carbon micro-electrolysis filler is prepared by a plurality of methods, generally, an iron-based material and a carbon-based material are formed by a binder, and the simple mixing mode causes the iron-carbon to be uneven and large in particle, the formed primary battery is few, and the degradation efficiency is low. The iron-carbon binding material of the nano-iron particles is prepared by the Caoshao and the like in Jiangsu university through a liquid-phase chemical deposition method, but the nano-iron has complex preparation process and higher cost and cannot be applied in a large scale. From the current commercial application, the common problem with microelectrolytic fillers is that: the galvanic cell made of solid particulate iron-carbon raw material is also a macro cell or a relative micro cell in the strict sense, and the number of the micro cells is obviously influenced by the particle size (generally 3-5cm spheres) and the number of the material particles, so that the number of the micro cells in a unit volume is limited, and the sewage treatment capacity is limited.
This patent is to the ubiquitous problem such as inefficiency, with high costs of present conventional little electrolysis filler processing waste water technique, provides a novel preparation method of indisputable carbon little electrolysis filler to increase in the unit volume microbattery quantity and with waste water area of contact, improve sewage treatment capacity.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method of an iron-carbon micro-electrolysis ball, which utilizes conventional raw materials to be melted by high temperature to form a solid solution, so as to achieve the purposes of uniformly mixing and forming countless micro-batteries, thereby achieving the purpose of improving the efficiency of degrading organic wastewater.
The specific scheme of the invention is as follows:
a preparation method of an iron-carbon micro-electrolysis ball comprises the following steps:
(1) mixing raw materials, fluxing agent and pore-forming agent in proportion;
(2) ball-milling the mixed raw materials to a certain particle size;
(3) heating and melting at a certain temperature under the protection of nitrogen;
(4) spray granulation and molding;
(5) soaking in tap water for a proper time.
In the step (1), the raw materials are iron powder and activated carbon, the fluxing agent is sodium hexafluoroaluminate, the pore-forming agent is sodium chloride, and the mass ratio of sodium hexafluoroaluminate is as follows: NaCl: iron powder: 15-20 parts of activated carbon: 10-15: 10: 1;
the particle size of the raw materials after ball milling in the step (2) is less than 0.2 mm.
Heating to the melting temperature of 1000-;
the spray granulation method in the step (4) is such that the melt flows out from the hole diameter of 5mm, the side spray breaks the fluid and cools it, and then the cold water is cooled down rapidly.
The time for soaking in tap water in the step (5) is 1-5 days.
The iron-carbon micro-electrolysis ball is used for degrading high-concentration organic wastewater, particularly high-concentration organic wastewater containing benzene rings.
The invention has the beneficial effects that:
(1) the iron and carbon can be uniformly mixed by utilizing high-temperature melting energy, so that the number of formed micro batteries is greatly increased, and the degradation of organic matters in wastewater is facilitated;
(2) the granulation method provided by the invention utilizes the rapid cooling shrinkage of the lower surface of the free falling body of the molten mass to form small particle ellipsoids.
(3) The sodium chloride is used as a pore-forming agent, and after the sodium chloride is soaked for a period of time, the sodium chloride is dissolved in water, and the electrolytic ball is porous. The longer the service time is, the more the holes are, the better the wastewater degradation effect is.
(4) The preparation method has low requirement on equipment precision, simple process, mass production, low cost, low requirement on raw materials, no use of environmental harmful substances, no production of environmental harmful substances and environmental friendliness.
Detailed Description
The invention will be further illustrated with reference to specific examples, to which the present invention is not at all restricted.
A preparation method of an iron-carbon micro-electrolysis ball comprises the following steps:
mixing raw materials, fluxing agent and pore-forming agent in proportion;
ball-milling the mixed raw materials to a certain particle size;
heating and melting at a certain temperature under the protection of nitrogen;
spray granulation and molding;
soaking in tap water for a proper time.
In the step (1), the raw materials are iron powder and activated carbon, the fluxing agent is sodium hexafluoroaluminate, the pore-forming agent is sodium chloride, and the mass ratio of sodium hexafluoroaluminate is as follows: NaCl: iron powder: 15-20 parts of activated carbon: 10-15: 10: 1;
the particle size of the raw materials after ball milling in the step (2) is less than 0.2 mm.
In the step (3), the heating and melting temperature is 1000-;
the spray granulation method in the step (4) is such that the melt flows out from the hole diameter of 5mm, the side spray breaks the fluid and cools it, and then the cold water is cooled down rapidly.
The time for soaking in tap water in the step (5) is 1-5 days.
Example 1
Weighing 300g of sodium hexafluoroaluminate, 200g of sodium chloride, 200g of iron powder and 20g of activated carbon, mixing, putting into a ball mill, ball-milling for 5 hours, taking out, transferring into a corundum crucible, putting into a tubular furnace, heating to 1100 ℃, preserving heat for 2 hours, taking out, immediately pouring into a forming container with the aperture of 5mm, spraying water mist from the side while the melt flows out of holes, naturally falling into cold water to form small granular iron-carbon balls, continuously soaking the iron-carbon balls in the cold water for 1 day, filtering and drying to obtain 542g of finished iron-carbon micro-electrolysis balls.
And (3) comparing degradation effects: 1 kg of iron-carbon micro-electrolysis balls purchased in the market and 1 kg of the iron-carbon micro-electrolysis balls prepared in the example are filled into a hard glass tube with the diameter of 5cm, the initial COD concentration of industrial wastewater with the pH value of 3.5 is 1826mg/L, a lower pipe opening flows out at the flow rate of 5ml/min, and the COD is 1108mg/L after the hard glass tube is filled with the iron-carbon micro-electrolysis balls purchased in the market, and the effective degradation rate of the COD is 39.3%; after the iron-carbon micro-electrolysis ball hard tube filled in the example is measured, the COD is 233mg/L, and the effective degradation rate of the COD is 87.2%.
Example 2
Weighing 400g of sodium hexafluoroaluminate, 300g of sodium chloride, 200g of iron powder and 20g of activated carbon, mixing, putting into a ball mill, ball-milling for 5 hours, taking out, transferring into a corundum crucible, putting into a tubular furnace, heating to 1000 ℃, preserving heat for 5 hours, taking out, immediately pouring into a forming container with the aperture of 5mm, spraying water mist from the side while the melt flows out of a hole, naturally falling into cold water to form small granular iron-carbon balls, continuously soaking the iron-carbon balls in the cold water for 5 days, filtering and drying to obtain 602g of finished iron-carbon micro-electrolysis balls.
And (3) comparing degradation effects: 1 kg of iron-carbon micro-electrolysis balls purchased in the market and 1 kg of the iron-carbon micro-electrolysis balls prepared in the example are filled into a hard glass tube with the diameter of 5cm, the initial COD concentration of industrial wastewater with the pH value of 3.5 is 1826mg/L, a lower pipe opening flows out at the flow rate of 5ml/min, and the COD is 1058mg/L after the hard glass tube is filled with the iron-carbon micro-electrolysis balls purchased in the market, and the effective degradation rate of the COD is 42.1%; after the iron-carbon micro-electrolysis ball hard tube filled in the example is measured, the COD is 218mg/L, and the effective degradation rate of the COD is 88.1%.
Example 3
Weighing 350g of sodium hexafluoroaluminate, 250g of sodium chloride, 200g of iron powder and 20g of activated carbon, mixing, putting into a ball mill, ball-milling for 5 hours, taking out, transferring into a corundum crucible, putting into a tubular furnace, heating to 1050 ℃, preserving heat for 3 hours, taking out, immediately pouring into a forming container with the aperture of 5mm, spraying water mist from the side while the melt flows out of holes, naturally falling into cold water to form small granular iron-carbon balls, continuously soaking the iron-carbon balls in the cold water for 3 days, filtering and drying to obtain 552g of finished iron-carbon micro-electrolysis balls.
And (3) comparing degradation effects: 1 kg of iron-carbon micro-electrolysis balls purchased in the market and 1 kg of the iron-carbon micro-electrolysis balls prepared in the example are filled into a hard glass tube with the diameter of 5cm, the initial COD concentration of industrial wastewater is 1826mg/L when the pH value is 3.5, the COD flows out from a lower pipe opening at the flow rate of 5ml/min, the COD is 1132mg/L after the hard glass tube is filled with the iron-carbon micro-electrolysis balls purchased in the market, and the effective degradation rate of the COD is 38.0%; the COD of the iron-carbon micro-electrolysis ball hard tube filled by the example is measured to be 225mg/L, and the effective degradation rate of the COD is 87.7%.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any modification, equivalent replacement, and improvement made by those skilled in the art within the technical scope of the present invention should be included in the scope of the present invention.
Claims (7)
1. A preparation method of an iron-carbon micro-electrolysis ball is characterized by comprising the following steps: the method comprises the following steps:
(1) mixing raw materials, fluxing agent and pore-forming agent in proportion;
(2) ball-milling the mixed raw materials to a certain particle size;
(3) heating and melting at a certain temperature under the protection of nitrogen;
(4) spray granulation and molding;
(5) and soaking in tap water for a proper time to form holes.
2. The method for preparing the iron-carbon micro-electrolysis ball according to claim 1, wherein the method comprises the following steps: the raw materials in the step (1) are iron powder and activated carbon, the fluxing agent is sodium hexafluoroaluminate, and the pore-forming agent is sodium chloride.
3. The method for preparing the iron-carbon micro-electrolysis ball according to claim 1, wherein the method comprises the following steps: in the step (2), the required particle size of the ball mill is below 0.2 mm.
4. The method for preparing the iron-carbon micro-electrolysis ball according to claim 1, wherein the method comprises the following steps: the heating and melting temperature in the step (3) is 1000-1100 ℃, and the heat preservation time is 2-5 hours.
5. The method for preparing the iron-carbon micro-electrolysis ball according to claim 1, wherein the method comprises the following steps: in the spray granulation molding method in the step (4), the molten mass flows out from the hole with the diameter of 5mm, the side surface is sprayed to break the fluid and rapidly cool the fluid, and the cooling water continues to cool the fluid.
6. The method for preparing the iron-carbon micro-electrolysis ball according to claim 1, wherein the method comprises the following steps: and (5) soaking the mixture in tap water for 1 to 5 days.
7. The iron-carbon micro-electrolysis ball according to any one of claims 1 to 6 is used for degrading high-concentration organic wastewater.
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| CN202010169770.4A CN111362368A (en) | 2020-03-12 | 2020-03-12 | Preparation method of iron-carbon micro-electrolysis ball |
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| CN202010169770.4A CN111362368A (en) | 2020-03-12 | 2020-03-12 | Preparation method of iron-carbon micro-electrolysis ball |
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Citations (4)
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| JP2008069385A (en) * | 2006-09-12 | 2008-03-27 | Ntn Corp | Method for producing sintered metal member |
| CN101608271A (en) * | 2009-07-20 | 2009-12-23 | 河北工业大学 | A kind of preparation method of through-hole foam copper |
| CN106222469A (en) * | 2016-09-14 | 2016-12-14 | 郑州峰泰纳米材料有限公司 | The preparation method of enhancement mode foam aluminium alloy |
| CN206814454U (en) * | 2017-02-21 | 2017-12-29 | 陕西兴华环保科技有限公司 | A kind of aeration reinforcing micro-electrolysis reaction device for sewage disposal |
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2020
- 2020-03-12 CN CN202010169770.4A patent/CN111362368A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008069385A (en) * | 2006-09-12 | 2008-03-27 | Ntn Corp | Method for producing sintered metal member |
| CN101608271A (en) * | 2009-07-20 | 2009-12-23 | 河北工业大学 | A kind of preparation method of through-hole foam copper |
| CN106222469A (en) * | 2016-09-14 | 2016-12-14 | 郑州峰泰纳米材料有限公司 | The preparation method of enhancement mode foam aluminium alloy |
| CN206814454U (en) * | 2017-02-21 | 2017-12-29 | 陕西兴华环保科技有限公司 | A kind of aeration reinforcing micro-electrolysis reaction device for sewage disposal |
Non-Patent Citations (2)
| Title |
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| 冯文钦主编: "《神奇的矿晶宝石》", 30 September 2015, 地质出版社, pages: 97 * |
| 刘广文编著: "《喷雾干燥实用技术大全》", 31 October 2001, 中国轻工业出版社, pages: 491 * |
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