CN114084935A - Preparation method of iron-carbon micro-electrolysis filler formed by slowing down formation of isolation layer through rare earth carbonization - Google Patents

Preparation method of iron-carbon micro-electrolysis filler formed by slowing down formation of isolation layer through rare earth carbonization Download PDF

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CN114084935A
CN114084935A CN202111343614.6A CN202111343614A CN114084935A CN 114084935 A CN114084935 A CN 114084935A CN 202111343614 A CN202111343614 A CN 202111343614A CN 114084935 A CN114084935 A CN 114084935A
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iron
mixed metal
carbonization
metal powder
rare earth
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CN114084935B (en
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赵红磊
王廷文
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Shandong Northern Sanwei Environmental Protection Technology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/46Treatment of water, waste water, or sewage by electrochemical methods
    • C02F1/461Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
    • C02F1/46104Devices therefor; Their operating or servicing
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/46Treatment of water, waste water, or sewage by electrochemical methods
    • C02F1/461Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
    • C02F1/46104Devices therefor; Their operating or servicing
    • C02F1/46109Electrodes
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/46Treatment of water, waste water, or sewage by electrochemical methods
    • C02F1/461Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
    • C02F1/46104Devices therefor; Their operating or servicing
    • C02F1/46109Electrodes
    • C02F1/46114Electrodes in particulate form or with conductive and/or non conductive particles between them
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/46Treatment of water, waste water, or sewage by electrochemical methods
    • C02F1/461Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
    • C02F1/46104Devices therefor; Their operating or servicing
    • C02F1/46109Electrodes
    • C02F2001/46133Electrodes characterised by the material

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
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  • Electrodes For Compound Or Non-Metal Manufacture (AREA)
  • Electrolytic Production Of Metals (AREA)

Abstract

The application discloses a preparation method of an iron-carbon micro-electrolysis filler formed by a rare earth carbonization retarding isolation layer, which comprises the following steps: mixing and sintering metal powder; grinding the mixed metal blocks; preparing paste; coating and carbonizing; making into pill. This application reasonable in design does benefit to the tiny and even fine and close of electrolytic coating crystalline grain, reduce the formation of big electrolytic coating crystalline grain, and then slow down the formation of isolation layer, extend the life of the little electrolytic filler of iron carbon, the little electrolytic filler of iron carbon after using simultaneously, can decompose under the chloride powder effect of the scandium of easy deliquescence in the air, avoid the condition that hardens that the clearance appears after stacking, adopt the mode of mould pill, can improve the porous solid performance on the little electrolytic filler surface of iron carbon, and the outermost surface of the little electrolytic filler of iron carbon does not contain metallic element, can avoid the condition that bonding hardens between the little electrolytic filler of iron carbon that the metal passivation caused.

Description

Preparation method of iron-carbon micro-electrolysis filler formed by slowing down formation of isolation layer through rare earth carbonization
Technical Field
The application relates to the field of iron-carbon micro-electrolysis fillers, in particular to a preparation method of an iron-carbon micro-electrolysis filler formed by a rare earth carbonization retarding isolation layer.
Background
The iron-carbon micro-electrolysis is a good process for treating wastewater by a galvanic cell formed by a metal corrosion principle method, also called an internal electrolysis method, an iron scrap filtration method and the like, the micro-electrolysis technology is an ideal process for treating high-concentration organic wastewater at present, also called an internal electrolysis method, and the micro-electrolysis technology is used for electrolyzing wastewater by utilizing a 1.2V potential difference generated by a micro-electrolysis material filled in the wastewater under the condition of no power supply so as to achieve the purpose of degrading organic pollutants.
In utilizing indisputable carbon microelectrolysis filler to carry out indisputable carbon microelectrolysis to waste water and handling, the electrolysis forms the big electrolytic coating crystalline grain of crystalline grain between iron and the carbon, causes the isolation layer to form speed relatively very fast, and then indisputable carbon microelectrolysis filler can't reuse, easily bonds together at the electrolysis in-process between the little electrolysis filler of indisputable carbon simultaneously, the condition that hardens appears, and the clearance is come out the little electrolysis filler of indisputable carbon of stacking and also is brought inconvenience for subsequent processing. Therefore, the preparation method of the iron-carbon micro-electrolysis filler for slowing down the formation of the isolation layer by the rare earth carbonization is provided for solving the problems.
Disclosure of Invention
A preparation method of an iron-carbon micro-electrolysis filler formed by a rare earth carbonization retarding isolation layer comprises the following steps:
step 1, metal powder mixing and sintering: taking 50-90g of Fe, 5-20g of C, 1-2g of yttrium, 1-2g of cerium and 1.5-3g of tungsten from each storage spare container, uniformly mixing, filling into a refractory container, and sintering in a sintering furnace according to three temperature stages of 1200-1250 ℃, 1300-1350 ℃ and 1400-1450 ℃ for 16 hours to integrally combine the materials in a solid phase manner;
step 2, grinding the mixed metal block: crushing the cooled mixed metal blocks by a crusher, grinding the crushed mixed metal blocks by a grinder to obtain mixed metal powder at a nanometer level, wherein the total mass of the mixed metal powder is 100-200g, and storing the mixed metal powder for later use;
step 3, paste preparation: mixing graphene powder, ytterbium powder, scandium chloride powder and a thickening agent according to the ratio of 8: 1: 2: 12 or 10: 1: 1: 6, weighing the components according to the proportion, putting the components into a mixing machine bin, and fully mixing the components into a paste mixed solution for later use by a mixing machine;
step 4, slurry coating and carbonization: taking 100g of mixed metal powder in the step 2, putting the mixed metal powder into a mixing machine bin filled with the pasty mixed liquid in the step 3, fully and uniformly mixing until the surface of each fine mixed metal powder particle is fully coated with slurry, drying the mixture in a dryer at the gradual change high temperature of 300 ℃, cooling and taking out the mixture, putting the mixture into a refractory container, putting the refractory container into a high-temperature sintering furnace, carbonizing the surface of the coated slurry of the mixed metal powder, activating by high-temperature steam to open micropores, and taking the mixture out of the furnace for standby after anaerobic cooling;
step 5, pelleting: and (3) adding a proper amount of coupling agent into any one of the 20-90 parts of mixed metal powder in the step (4), wherein the mass of each part of carbonized mixed metal powder is 2-3 g, sending the mixture into a stirrer to be fully stirred and mixed for 15-25 minutes, uniformly adding 0.2-0.5g of natural rubber juice, fully stirring and reacting for 30-45 minutes to obtain paste, then pouring the paste into a pelleting die, sending the paste into a microwave high-temperature furnace at 260-960 ℃ to be dried and sintered for 10-12 hours, cooling the paste to below 30 ℃, and taking the paste out of the furnace to obtain the iron-carbon micro-electrolysis filler formed by the rare earth carbonization retarding partition layer.
Preferably, in the step 1, Ti: 5-10g and taking Ag: 10-20g, cerium: 2g and tungsten: 3g were mixed together to form a cerium tungsten electrode.
Preferably, 10-15g of plant cellulose and 5-10g of coal powder are also taken in the step 3.
Preferably, the step 4 is carried out by loading a refractory container into a high-temperature sintering furnace, controlling the temperature at 700-865 ℃ and carrying out oxygen-free roasting for 7-9 hours.
The invention has the beneficial effects that: the electrolytic conductivity of little electrolysis filler of reinforcing iron carbon, improve electrolysis efficiency, be good for the high-efficient electrolytic treatment of waste water, ytterbium powder through the increase, do benefit to and become tiny and even fine and close with the electrolytic coating crystalline grain, reduce the formation of big electrolytic coating crystalline grain, and then slow down the formation of isolation layer, extend the life of little electrolysis filler of iron carbon, little electrolysis filler of iron carbon after the while uses, can decompose under the chloride powder effect of the scandium of easy deliquescence in the air, avoid the condition that hardens that appears after the clearance is stacked, adopt the mode of mould pelletization, can improve the porous solid performance on little electrolysis filler surface of iron carbon, and the outermost surface of little electrolysis filler of iron carbon does not contain metallic element, can avoid the condition that bonding between the little electrolysis filler of iron carbon that the metal passivation caused hardens.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings needed to be used in the description of the embodiments or the prior art will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present application, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without inventive exercise.
FIG. 1 is a flow chart of the preparation method of the present application.
Detailed Description
In order to make the technical solutions better understood by those skilled in the art, the technical solutions in the embodiments of the present application will be clearly and completely described below with reference to the drawings in the embodiments of the present application, and it is obvious that the described embodiments are only partial embodiments of the present application, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
It should be noted that the terms "first," "second," and the like in the description and claims of this application and in the drawings described above are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It should be understood that the data so used may be interchanged under appropriate circumstances such that embodiments of the application described herein may be used. Furthermore, the terms "comprises," "comprising," and "having," and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed, but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
In this application, the terms "upper", "lower", "left", "right", "front", "rear", "top", "bottom", "inner", "outer", "middle", "vertical", "horizontal", "lateral", "longitudinal", and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings. These terms are used primarily to better describe the present application and its embodiments, and are not used to limit the indicated devices, elements or components to a particular orientation or to be constructed and operated in a particular orientation.
Moreover, some of the above terms may be used to indicate other meanings besides the orientation or positional relationship, for example, the term "on" may also be used to indicate some kind of attachment or connection relationship in some cases. The specific meaning of these terms in this application will be understood by those of ordinary skill in the art as appropriate.
Furthermore, the terms "mounted," "disposed," "provided," "connected," and "sleeved" are to be construed broadly. For example, it may be a fixed connection, a removable connection, or a unitary construction; can be a mechanical connection, or an electrical connection; may be directly connected, or indirectly connected through intervening media, or may be in internal communication between two devices, elements or components. The specific meaning of the above terms in the present application can be understood by those of ordinary skill in the art as appropriate.
It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict. The present application will be described in detail below with reference to the embodiments with reference to the attached drawings.
The first embodiment is as follows:
as shown in fig. 1, a method for preparing an iron-carbon micro-electrolysis filler formed by a rare earth carbonization retarding spacer layer comprises the following steps:
step 1, taking 50-90g of Fe, 5-20g of C, 1-2g of yttrium, 1-2g of cerium and 1.5-3g of tungsten from each storage spare container, uniformly mixing, filling into a refractory container, and sintering in a sintering furnace according to three temperature stages of 1200-1250 ℃, 1300-1350 ℃ and 1400-1450 ℃ for 16 hours to integrally combine the materials in a solid phase manner;
step 2, grinding the mixed metal block: and crushing the cooled mixed metal blocks by a crusher, grinding the crushed mixed metal blocks by a grinder to obtain the mixed metal powder at the nanometer level, wherein the total mass is 100-200g, and storing for later use.
Further, in the step 1, Ti: 5-10g and taking Ag: 10-20g, cerium: 2g and tungsten: 3g were mixed together to form a cerium tungsten electrode.
The preparation method of the iron-carbon micro-electrolysis filler formed by the rare earth carbonization retarding partition layer enhances the electrolytic conductivity of the iron-carbon micro-electrolysis filler, improves the electrolysis efficiency and is beneficial to efficient electrolysis treatment of wastewater.
Example two:
as shown in fig. 1, a method for preparing an iron-carbon micro-electrolysis filler formed by a rare earth carbonization retarding spacer layer comprises the following steps:
step 3, paste preparation: mixing graphene powder, ytterbium powder, scandium chloride powder and a thickening agent according to the ratio of 8: 1: 2: 12 or 10: 1: 1: 6, weighing the components according to the proportion, putting the components into a mixing machine bin, and fully mixing the components into a paste mixed solution for later use by a mixing machine;
step 4, slurry coating and carbonization: and (3) putting 100g of mixed metal powder obtained in the step (2) into a mixing machine bin filled with the pasty mixed liquid in the step (3) for fully and uniformly mixing until the surface of each fine mixed metal powder particle is fully coated with slurry, putting the mixture into a drying machine for drying at the gradual change high temperature of 300 ℃, cooling and taking out, putting the mixture into a refractory container, putting the refractory container into a high-temperature sintering furnace, carbonizing the surface of the coated slurry of the mixed metal powder, activating by high-temperature steam to open micropores, and taking the mixture out of the furnace for standby after anaerobic cooling.
Further, 10-15g of plant cellulose and 5-10g of coal powder are also taken in the step 3.
Further, the step 4 is to load a refractory container into a high-temperature sintering furnace, control the temperature at 700-865 ℃ and bake for 7-9 hours without oxygen.
Above-mentioned tombarthite carbonization slows down iron carbon micro-electrolysis filler preparation method that barrier layer formed, through the ytterbium powder that increases, does benefit to the tiny and even compactness of electrolytic coating crystalline grain, reduces the formation of big electrolytic coating crystalline grain, and then slows down the formation of barrier layer, extends the life of iron carbon micro-electrolysis filler, and the iron carbon micro-electrolysis filler after using simultaneously can decompose under the chloride powder effect of the scandium of easy deliquescence in the air, avoids the condition that the hardening appears after the clearance is stacked.
Example three:
as shown in fig. 1, a method for preparing an iron-carbon micro-electrolysis filler formed by a rare earth carbonization retarding spacer layer comprises the following steps:
step 5, pelleting: and (3) adding a proper amount of coupling agent into any one of the 20-90 parts of mixed metal powder in the step (4), wherein the mass of each part of carbonized mixed metal powder is 2-3 g, sending the mixture into a stirrer to be fully stirred and mixed for 15-25 minutes, uniformly adding 0.2-0.5g of natural rubber juice, fully stirring and reacting for 30-45 minutes to obtain paste, then pouring the paste into a pelleting die, sending the paste into a microwave high-temperature furnace at 260-960 ℃ to be dried and sintered for 10-12 hours, cooling the paste to below 30 ℃, and taking the paste out of the furnace to obtain the iron-carbon micro-electrolysis filler formed by the rare earth carbonization retarding partition layer.
According to the preparation method of the iron-carbon micro-electrolysis filler formed by slowing down the formation of the isolation layer through the rare earth carbonization, the mode of making pills through a mold is adopted, the porous solid performance of the surface of the iron-carbon micro-electrolysis filler can be improved, the outermost surface of the iron-carbon micro-electrolysis filler does not contain metal elements, and the condition that the iron-carbon micro-electrolysis filler is bonded and hardened due to metal passivation can be avoided.
The above description is only a preferred embodiment of the present application and is not intended to limit the present application, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, improvement and the like made within the spirit and principle of the present application shall be included in the protection scope of the present application.

Claims (4)

1. A preparation method of iron-carbon micro-electrolysis filler formed by rare earth carbonization retarding isolation layer is characterized by comprising the following steps: the method comprises the following steps:
step 1, metal powder mixing and sintering: taking 50-90g of Fe, 5-20g of C, 1-2g of yttrium, 1-2g of cerium and 1.5-3g of tungsten from each storage spare container, uniformly mixing, filling into a refractory container, and sintering in a sintering furnace according to three temperature stages of 1200-1250 ℃, 1300-1350 ℃ and 1400-1450 ℃ for 16 hours to integrally combine the materials in a solid phase manner;
step 2, grinding the mixed metal block: crushing the cooled mixed metal blocks by a crusher, grinding the crushed mixed metal blocks by a grinder to obtain mixed metal powder at a nanometer level, wherein the total mass of the mixed metal powder is 100-200g, and storing the mixed metal powder for later use;
step 3, paste preparation: mixing graphene powder, ytterbium powder, scandium chloride powder and a thickening agent according to the ratio of 8: 1: 2: 12 or 10: 1: 1: 6, weighing the components according to the proportion, putting the components into a mixing machine bin, and fully mixing the components into a paste mixed solution for later use by a mixing machine;
step 4, slurry coating and carbonization: taking 100g of mixed metal powder in the step 2, putting the mixed metal powder into a mixing machine bin filled with the pasty mixed liquid in the step 3, fully and uniformly mixing until the surface of each fine mixed metal powder particle is fully coated with slurry, drying the mixture in a dryer at the gradual change high temperature of 300 ℃, cooling and taking out the mixture, putting the mixture into a refractory container, putting the refractory container into a high-temperature sintering furnace, carbonizing the surface of the coated slurry of the mixed metal powder, activating by high-temperature steam to open micropores, and taking the mixture out of the furnace for standby after anaerobic cooling;
step 5, pelleting: and (3) adding a proper amount of coupling agent into any one of the 20-90 parts of mixed metal powder in the step (4), wherein the mass of each part of carbonized mixed metal powder is 2-3 g, sending the mixture into a stirrer to be fully stirred and mixed for 15-25 minutes, uniformly adding 0.2-0.5g of natural rubber juice, fully stirring and reacting for 30-45 minutes to obtain paste, then pouring the paste into a pelleting die, sending the paste into a microwave high-temperature furnace at 260-960 ℃ to be dried and sintered for 10-12 hours, cooling the paste to below 30 ℃, and taking the paste out of the furnace to obtain the iron-carbon micro-electrolysis filler formed by the rare earth carbonization retarding partition layer.
2. The method for preparing the iron-carbon micro-electrolysis filler formed by the rare earth carbonization retarding spacer layer according to claim 1 is characterized in that: taking Ti in the step 1: 5-10g and taking Ag: 10-20g, cerium: 2g and tungsten: 3g were mixed together to form a cerium tungsten electrode.
3. The method for preparing the iron-carbon micro-electrolysis filler formed by the rare earth carbonization retarding spacer layer according to claim 1 is characterized in that: in the step 3, 10-15g of plant cellulose and 5-10g of coal powder are also taken.
4. The method for preparing the iron-carbon micro-electrolysis filler formed by the rare earth carbonization retarding spacer layer according to claim 1 is characterized in that: in the step 4, a refractory container is loaded into a high-temperature sintering furnace, the temperature is controlled at 700-865 ℃, and the sintering is carried out for 7-9 hours in an oxygen-free manner.
CN202111343614.6A 2021-11-13 2021-11-13 Preparation method of iron-carbon micro-electrolysis filler for slowing down formation of isolation layer by rare earth carbonization Active CN114084935B (en)

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Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101704565A (en) * 2009-11-16 2010-05-12 同济大学 Preparation method of iron-carbon micro-electrolytic filler
CN109607704A (en) * 2019-01-31 2019-04-12 内蒙古科技大学 Using rare-earth tailing as multiple catalyzing iron carbon microelectrode filler of raw material and the preparation method and application thereof
CN111777133A (en) * 2020-07-02 2020-10-16 山东北方三潍环保科技有限公司 Preparation method of novel non-hardening coupling iron-carbon micro-electrolysis filler
CN112225297A (en) * 2020-10-20 2021-01-15 山东万泓环保科技有限公司 Anti-hardening iron-carbon micro-electrolysis filler and preparation method thereof

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101704565A (en) * 2009-11-16 2010-05-12 同济大学 Preparation method of iron-carbon micro-electrolytic filler
CN109607704A (en) * 2019-01-31 2019-04-12 内蒙古科技大学 Using rare-earth tailing as multiple catalyzing iron carbon microelectrode filler of raw material and the preparation method and application thereof
CN111777133A (en) * 2020-07-02 2020-10-16 山东北方三潍环保科技有限公司 Preparation method of novel non-hardening coupling iron-carbon micro-electrolysis filler
CN112225297A (en) * 2020-10-20 2021-01-15 山东万泓环保科技有限公司 Anti-hardening iron-carbon micro-electrolysis filler and preparation method thereof

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Title
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