CN114084935B - Preparation method of iron-carbon micro-electrolysis filler for slowing down formation of isolation layer by rare earth carbonization - Google Patents

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

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CN114084935B
CN114084935B CN202111343614.6A CN202111343614A CN114084935B CN 114084935 B CN114084935 B CN 114084935B CN 202111343614 A CN202111343614 A CN 202111343614A CN 114084935 B CN114084935 B CN 114084935B
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mixed metal
carbon micro
metal powder
electrolysis filler
iron
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CN114084935A (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)
  • Organic Chemistry (AREA)
  • 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 for reducing formation of an isolation layer by rare earth carbonization, which comprises the following steps: mixing and sintering metal powder; grinding the mixed metal block; preparing paste; hanging slurry and carbonizing; making into pill. This application reasonable in design does benefit to the formation with electrolytic coating grain tiny and even dense, reduces big electrolytic coating grain, and then slows down the formation of isolation layer, extends the life of indisputable carbon micro-electrolysis filler, and the indisputable carbon micro-electrolysis filler after the use simultaneously can decompose under the chloride powder effect of the scandium of deliquescing in the air, avoids the condition of the hardening that appears after the clearance stacks, adopts the mode of mould pelleting, can improve the porous firm performance on indisputable carbon micro-electrolysis filler surface, and indisputable carbon micro-electrolysis filler does not have metal element, can avoid the condition of bonding the hardening between the indisputable carbon micro-electrolysis filler that the metal passivation caused.

Description

Preparation method of iron-carbon micro-electrolysis filler for slowing down formation of isolation layer by 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 for slowing down the formation of an isolation layer by rare earth carbonization.
Background
The iron-carbon micro-electrolysis is a good process for treating the waste water by utilizing a metal corrosion principle method to form a primary cell, is also called an internal electrolysis method, an iron filings filtering method and the like, and is an ideal process for treating high-concentration organic waste water at present, namely an internal electrolysis method.
In the iron-carbon micro-electrolysis treatment of wastewater by utilizing the iron-carbon micro-electrolysis filler, electrolytic plating grains with large grains are formed between iron and carbon by electrolysis, so that the forming speed of an isolation layer is relatively high, the iron-carbon micro-electrolysis filler cannot be reused, meanwhile, the iron-carbon micro-electrolysis filler is easy to adhere together in the electrolysis process, the hardening condition occurs, and the stacked iron-carbon micro-electrolysis filler is cleaned to bring inconvenience to subsequent treatment. Therefore, a preparation method of the iron-carbon micro-electrolysis filler for reducing the formation of the isolation layer by rare earth carbonization is provided for solving the problems.
Disclosure of Invention
A preparation method of an iron-carbon micro-electrolysis filler for slowing down the formation of an isolation layer by rare earth carbonization comprises the following steps:
step 1, metal powder mixed 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 standby container, uniformly mixing, loading into a refractory container, and sintering in a sintering furnace for 16 hours according to three temperature stages of 1200-1250 ℃, 1300-1350 ℃ and 1400-1450 ℃ to integrate the materials into a solid phase;
step 2, grinding the mixed metal block: crushing the cooled mixed metal blocks by a crusher, grinding the crushed mixed metal blocks into nano-scale mixed metal powder by a grinder, and storing the mixed metal powder for later use, wherein the total mass of the mixed metal powder is 100-200 g;
step 3, paste preparation: graphene powder, ytterbium powder, scandium chloride powder and thickener according to the following ratio of 8:1:2:12 or 10:1:1:6, weighing the materials in proportion, filling the materials into a mixer bin, and fully mixing the materials into paste mixed liquid through a mixer for later use;
step 4, hanging slurry for carbonization: taking 100g of the mixed metal powder in the step 2, putting the mixed metal powder into a mixer 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, putting the mixed metal powder into a dryer, carrying out gradual high-temperature drying at 150-300 ℃, cooling, taking out, putting the mixed metal powder into a refractory container, putting the refractory container into a high-temperature sintering furnace, carbonizing the surface coated with slurry of the mixed metal powder, activating the micropores by high-temperature steam, and carrying out anaerobic cooling and discharging for later use;
step 5, pelleting: and (3) adding a proper amount of coupling agent into any one of 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 mixed metal powder into a stirrer, fully stirring and mixing for 15-25 minutes, uniformly adding 0.2-0.5g of natural rubber juice, fully stirring and reacting for 30-45 minutes, standing in a pasty state, pouring the pasty state into a pelleting mould, sending the pasty state into a microwave high-temperature furnace at 260-960 ℃, drying and sintering for 10-12 hours, cooling to below 30 ℃, and discharging to obtain the iron-carbon micro-electrolysis filler formed by the rare earth carbonization slow-down isolation layer.
Preferably, in the step 1, ti is further taken as follows: 5-10g and taking Ag:10-20g, cerium: 2g and tungsten: 3g are mixed together to form a cerium tungsten electrode.
Preferably, in the step 3, 10-15g of plant cellulose and 5-10g of coal powder are also taken.
Preferably, the refractory container is filled in the step 4, the temperature of the high-temperature sintering furnace is controlled to be 700-865 ℃, and the high-temperature sintering furnace is roasted for 7-9 hours in an oxygen-free mode.
The beneficial effects of the invention are as follows: the method has the advantages that the electrolytic conductivity of the iron-carbon micro-electrolysis filler is enhanced, the electrolytic efficiency is improved, the efficient electrolytic treatment of wastewater is benefited, the grain of an electrolytic coating is miniaturized, uniform and compact through the added ytterbium powder, the formation of the grain of the large electrolytic coating is reduced, the formation of an isolating layer is further slowed down, the service life of the iron-carbon micro-electrolysis filler is prolonged, meanwhile, the iron-carbon micro-electrolysis filler after use can be decomposed under the action of chloride powder of scandium which is easy to deliquest in the air, the hardening condition after cleaning and stacking is avoided, the porous solid performance of the surface of the iron-carbon micro-electrolysis filler can be improved by adopting a mode of preparing pellets by a die, the outermost surface of the iron-carbon micro-electrolysis filler does not contain metal elements, and the bonding hardening condition between the iron-carbon micro-electrolysis fillers caused by metal passivation can be avoided.
Drawings
In order to more clearly illustrate the embodiments of the present application or the technical solutions in the prior art, the drawings that are required in the embodiments or the description of the prior art will be briefly described below, it being obvious that the drawings in the following description are only some embodiments of the present application, and that other drawings may be obtained according to these drawings without inventive faculty for a person skilled in the art.
FIG. 1 is a flow chart of the preparation method of the present application.
Detailed Description
In order to make the present application solution better understood by those skilled in the art, the following description will be made in detail and with reference to the accompanying drawings in the embodiments of the present application, it is apparent that the described embodiments are only some embodiments of the present application, not all embodiments. All other embodiments, which can be made by one of ordinary skill in the art based on the embodiments herein without making any inventive effort, shall fall within the scope of the present application.
It should be noted that the terms "first," "second," and the like in the description and claims of the present application and the above figures are used for distinguishing between similar objects and not necessarily for describing a particular sequential or chronological order. It is to be understood that the data so used may be interchanged where appropriate in order to describe the embodiments of the present application described herein. 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 the present application, the terms "upper", "lower", "left", "right", "front", "rear", "top", "bottom", "inner", "outer", "middle", "vertical", "horizontal", "lateral", "longitudinal" and the like indicate an azimuth or a positional relationship based on that shown in the drawings. These terms are used primarily to better describe the present application and its embodiments and are not intended to limit the indicated device, element or component to a particular orientation or to be constructed and operated in a particular orientation.
Also, some of the terms described above may be used to indicate other meanings in addition to orientation or positional relationships, for example, the term "upper" may also be used to indicate some sort of attachment or connection 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," "configured," "provided," "connected," "coupled," and "sleeved" are to be construed broadly. For example, it may be a fixed connection, a removable connection, or a unitary construction; may 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 terms in this application will be understood by those of ordinary skill in the art as the case may be.
It should be noted that, in the case of no conflict, the embodiments and features in the embodiments may be combined with each other. The present application will be described in detail below with reference to the accompanying drawings in conjunction with embodiments.
Embodiment one:
as shown in fig. 1, the preparation method of the iron-carbon micro-electrolysis filler for forming the rare earth carbonization slowing isolation 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 standby container, uniformly mixing, loading into a refractory container, and sintering in a sintering furnace for 16 hours according to three temperature stages of 1200-1250 ℃, 1300-1350 ℃ and 1400-1450 ℃ to integrate the materials into a solid phase;
step 2, grinding the mixed metal block: crushing the cooled mixed metal blocks by a crusher, grinding the crushed mixed metal blocks into nano-scale mixed metal powder by a grinder, and storing the nano-scale mixed metal powder for standby.
Further, in the step 1, ti:5-10g and taking Ag:10-20g, cerium: 2g and tungsten: 3g are mixed together to form a cerium tungsten electrode.
According to the preparation method of the iron-carbon micro-electrolysis filler formed by the rare earth carbonization retarding isolation layer, the electrolysis conductivity of the iron-carbon micro-electrolysis filler is enhanced, the electrolysis efficiency is improved, and the method is beneficial to high-efficiency electrolysis treatment of wastewater.
Embodiment two:
as shown in fig. 1, the preparation method of the iron-carbon micro-electrolysis filler for forming the rare earth carbonization slowing isolation layer comprises the following steps:
step 3, paste preparation: graphene powder, ytterbium powder, scandium chloride powder and thickener according to the following ratio of 8:1:2:12 or 10:1:1:6, weighing the materials in proportion, filling the materials into a mixer bin, and fully mixing the materials into paste mixed liquid through a mixer for later use;
step 4, hanging slurry for carbonization: and (3) putting 100g of the mixed metal powder in the step (2) into a mixer 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, putting the mixed metal powder into a dryer, carrying out gradual high-temperature drying at 150-300 ℃, cooling, taking out, putting into a refractory container, putting into a high-temperature sintering furnace, carbonizing the surface coated with slurry of the mixed metal powder, activating by high-temperature steam, opening micropores, and carrying out anaerobic cooling and discharging for standby.
Further, in the step 3, 10-15g of plant cellulose and 5-10g of coal powder are also taken.
Further, the refractory container is filled in the step 4, the temperature of the high-temperature sintering furnace is controlled to be 700-865 ℃, and the furnace is roasted for 7-9 hours in an oxygen-free mode.
According to the preparation method of the iron-carbon micro-electrolysis filler formed by the rare earth carbonization retarding isolation layer, the added ytterbium powder is beneficial to miniaturizing, homogenizing and compacting electrolytic plating layer crystal grains, reducing the formation of large electrolytic plating layer crystal grains, further retarding the formation of the isolation layer, prolonging the service life of the iron-carbon micro-electrolysis filler, and meanwhile, the iron-carbon micro-electrolysis filler after being used can be decomposed under the action of the chloride powder of scandium which is easy to deliquesce in the air, so that the hardening condition after cleaning and stacking is avoided.
Embodiment III:
as shown in fig. 1, the preparation method of the iron-carbon micro-electrolysis filler for forming the rare earth carbonization slowing isolation layer comprises the following steps:
step 5, pelleting: and (3) adding a proper amount of coupling agent into any one of 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 mixed metal powder into a stirrer, fully stirring and mixing for 15-25 minutes, uniformly adding 0.2-0.5g of natural rubber juice, fully stirring and reacting for 30-45 minutes, standing in a pasty state, pouring the pasty state into a pelleting mould, sending the pasty state into a microwave high-temperature furnace at 260-960 ℃, drying and sintering for 10-12 hours, cooling to below 30 ℃, and discharging to obtain the iron-carbon micro-electrolysis filler formed by the rare earth carbonization slow-down isolation layer.
According to the preparation method of the iron-carbon micro-electrolysis filler formed by the rare earth carbonization retarding isolation layer, the porous solid performance of the surface of the iron-carbon micro-electrolysis filler can be improved by adopting a mould pelleting mode, the outermost surface of the iron-carbon micro-electrolysis filler does not contain metal elements, and the situation of bonding hardening between the iron-carbon micro-electrolysis fillers caused by metal passivation can be avoided.
The foregoing description is only of the preferred embodiments of the present application and is not intended to limit the same, but rather, various modifications and variations may be made by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principles of the present application should be included in the protection scope of the present application.

Claims (4)

1. A preparation method of an iron-carbon micro-electrolysis filler for slowing down the formation of an isolation layer by rare earth carbonization is characterized by comprising the following steps: the method comprises the following steps:
step 1, metal powder mixed 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 standby container, uniformly mixing, loading into a refractory container, and sintering in a sintering furnace for 16 hours according to three temperature stages of 1200-1250 ℃, 1300-1350 ℃ and 1400-1450 ℃ to integrate the materials into a solid phase;
step 2, grinding the mixed metal block: crushing the cooled mixed metal blocks by a crusher, grinding the crushed mixed metal blocks into nano-scale mixed metal powder by a grinder, and storing the mixed metal powder for later use, wherein the total mass of the mixed metal powder is 100-200 g;
step 3, paste preparation: graphene powder, ytterbium powder, scandium chloride powder and thickener according to the following ratio of 8:1:2:12 or 10:1:1:6, weighing the materials in proportion, filling the materials into a mixer bin, and fully mixing the materials into paste mixed liquid through a mixer for later use;
step 4, hanging slurry for carbonization: taking 100g of the mixed metal powder in the step 2, putting the mixed metal powder into a mixer 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, putting the mixed metal powder into a dryer, carrying out gradual high-temperature drying at 150-300 ℃, cooling, taking out, putting the mixed metal powder into a refractory container, putting the refractory container into a high-temperature sintering furnace, carbonizing the surface coated with slurry of the mixed metal powder, activating the micropores by high-temperature steam, and carrying out anaerobic cooling and discharging for later use;
step 5, pelleting: and (3) adding a proper amount of coupling agent into any one of 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 mixed metal powder into a stirrer, fully stirring and mixing for 15-25 minutes, uniformly adding 0.2-0.5g of natural rubber juice, fully stirring and reacting for 30-45 minutes, standing in a pasty state, pouring the pasty state into a pelleting mould, sending the pasty state into a microwave high-temperature furnace at 260-960 ℃, drying and sintering for 10-12 hours, cooling to below 30 ℃, and discharging to obtain the iron-carbon micro-electrolysis filler formed by the rare earth carbonization slow-down isolation layer.
2. The method for preparing the iron-carbon micro-electrolysis filler for forming the rare earth carbonization slowing down isolation layer according to claim 1, which is characterized in that: in the step 1, ti is also taken: 5-10g and taking Ag:10-20g, cerium: 2g and tungsten: 3g are mixed together to form a cerium tungsten electrode.
3. The method for preparing the iron-carbon micro-electrolysis filler for forming the rare earth carbonization slowing down isolation layer according to claim 1, which 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 for forming the rare earth carbonization slowing down isolation layer according to claim 1, which is characterized in that: and (3) loading a refractory container into the step (4), loading the refractory container into a high-temperature sintering furnace, controlling the temperature to be 700-865 ℃, and roasting the refractory container 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

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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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