CN112624101A - Process for wet treatment of electrolytic aluminum waste cathode material - Google Patents

Process for wet treatment of electrolytic aluminum waste cathode material Download PDF

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Publication number
CN112624101A
CN112624101A CN202011533222.1A CN202011533222A CN112624101A CN 112624101 A CN112624101 A CN 112624101A CN 202011533222 A CN202011533222 A CN 202011533222A CN 112624101 A CN112624101 A CN 112624101A
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China
Prior art keywords
electrolytic aluminum
waste cathode
sample
leaching
crushing
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CN202011533222.1A
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Chinese (zh)
Inventor
张逸飞
张宏忠
钱旭辉
郭方方
杨浩
刘世豪
常德政
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HENAN INSTITUTE OF METALLURGY CO LTD
Henan Academy of Sciences
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HENAN INSTITUTE OF METALLURGY CO LTD
Henan Academy of Sciences
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Priority to CN202011533222.1A priority Critical patent/CN112624101A/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01BNON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00Carbon; Compounds thereof
    • C01B32/20Graphite
    • C01B32/205Preparation
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00Compounds of aluminium
    • C01F7/48Halides, with or without other cations besides aluminium
    • C01F7/50Fluorides
    • C01F7/54Double compounds containing both aluminium and alkali metals or alkaline-earth metals

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Processing Of Solid Wastes (AREA)

Abstract

The invention discloses a process for treating waste cathode materials of electrolytic aluminum by a wet method, which is characterized by comprising the following steps of: step a: coarsely crushing the electrolytic aluminum waste cathode sample; b, fine crushing, namely further crushing the electrolytic aluminum waste cathode sample after coarse crushing in the step a; step c: grinding; step d: alkaline leaching; step e: acid leaching; step f: and mixing the acid and alkali leaching solutions to obtain the cryolite. According to the invention, through research on the waste cathode material of the electrolytic aluminum, the process flow for treating the waste cathode material of the electrolytic aluminum, which has lower treatment temperature, is easier to recycle and has better treatment effect, can provide a new thought and method for treating the carbon block of the waste cathode of the aluminum on the one hand, can improve the recycling rate of the carbon material on the other hand, reduces the treatment cost of aluminum enterprises, and can provide a positive guide effect on solving the problems of pollution discharge and resource utilization in the aluminum industry.

Description

Process for wet treatment of electrolytic aluminum waste cathode material
Technical Field
The invention belongs to the field of harmless treatment of hazardous wastes, and particularly relates to a process for treating electrolytic aluminum waste cathode materials by a wet method.
Background
The amount of the aluminum industry in China is at the first place in the world for years, the related technology of electrolytic aluminum is continuously broken through in social development and technological progress, and the flourishing of the aluminum industry also brings about a great deal of environmental pollution. According to the literature, 30-50 kg of waste cathode materials are produced every 1 ton of electrolytic aluminum, and according to the data, the production amount of the waste cathode materials in 2017 is more than 100 ten thousand tons, and the stacking amount of electrolytic aluminum residues is difficult to estimate for years. In recent years, the illegal dumping of waste cathode carbon blocks in aluminum factories and other problems are always reported, and if the problems existing in the electrolytic aluminum waste cathode carbon blocks cannot be properly treated, the health of people is threatened, and the local soil and water environment are also extremely badly influenced. In addition, with the environmental deterioration and the increasing shortage of mineral resources, how to economically and effectively treat the electrolytic aluminum waste cathode carbon block is a direct and effective means for reducing the pollution discharge cost of an electrolytic aluminum enterprise and promoting the sustainable development of the aluminum industry.
At present, the process of carrying out harmless treatment on waste cathode carbon blocks by a pyrogenic process is commonly applied in industry, but the pyrogenic process has higher requirements on equipment, high-temperature treatment has higher energy consumption and cost, combustion residues need to be buried and treated, the cost is further increased, carbon materials and electrolyte components in the waste cathode carbon blocks of electrolytic aluminum cannot be well recycled, and the method is not the best solution for treating the waste cathode carbon blocks in the future of more and more teaching on environment protection resource utilization. Reagents such as strong acid, strong base and the like are commonly used in wet treatment, so that the corrosion to plant equipment is large, and the safety and the maintenance cost are high; moreover, because the components of the waste cathode carbon block material are complex, the carbon material and the electrolyte can not be well separated through wet treatment; the wet treatment process flow is relatively complex, the actual operation difficulty is high, and the safety is poor, so the wet treatment is mostly in a laboratory or a small test stage and cannot be applied to industrial production on a large scale.
Disclosure of Invention
The technical problem to be solved by the present invention is to provide a wet process for treating waste cathode material of electrolytic aluminum, which is intended to solve the defects of the prior art.
The technical scheme of the invention is as follows: a process for wet processing of electrolytic aluminum waste cathode material is characterized by comprising the following steps:
step a: coarsely crushing the electrolytic aluminum waste cathode sample;
b, fine crushing, namely further crushing the electrolytic aluminum waste cathode sample after coarse crushing in the step a;
step c: b, grinding, namely grinding the finely crushed waste cathode sample of the electrolytic aluminum in the step b into powder;
step d: alkaline leaching, namely selecting an electrolytic aluminum waste cathode sample with the granularity ranging from 100 meshes to 150 meshes, adding a solvent in a mixed solution of water and petroleum ether according to the mass ratio of 20:5, adding 2.4mL of NaOH solution into each 1g of the electrolytic aluminum waste cathode sample, adjusting the liquid-solid ratio to be 20:1, treating the sample for 25-35min by using an ultrasonic cleaner under the condition of keeping the normal temperature, and standing the sample for 2 hours; after leaching, centrifuging the mixed slurry for 7-10min, leaching the precipitate by using absolute ethyl alcohol and petroleum ether, and reserving the cleaned graphitized carbon sample for later use;
step e: d, acid leaching, namely adding a certain amount of 10% HCl solution into the graphitized carbon sample cleaned in the step d, leaching for 2 hours at normal temperature, centrifuging the slurry for 7-10min, washing the precipitate once with absolute ethyl alcohol and petroleum ether respectively, and naturally drying to obtain graphitized carbon;
step f: and mixing the acid and alkali leaching solutions to obtain the cryolite.
In the scheme, the power of the ultrasonic cleaner used in the step d is 300W, and the processing time of the ultrasonic cleaner is 30 min; and d, the centrifugal rotating speed of the mixed slurry in the step d is 10000rpm, and the centrifugal time is 7 min.
In the scheme, the centrifugal rotating speed of the mixed slurry in the step e is 10000rpm, and the centrifugal time is 7 min.
Has the advantages that: according to the invention, through research on the waste cathode material of the electrolytic aluminum, the process flow for treating the waste cathode material of the electrolytic aluminum, which has lower treatment temperature, is easier to recycle and has better treatment effect, can provide a new thought and method for treating the carbon block of the waste cathode of the aluminum on the one hand, can improve the recycling rate of the carbon material on the other hand, reduces the treatment cost of aluminum enterprises, and can provide a positive guide effect on solving the problems of pollution discharge and resource utilization in the aluminum industry.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
The invention is further illustrated by the following examples in conjunction with the accompanying drawings:
as shown in figure 1, the process for wet processing the electrolytic aluminum waste cathode material is characterized by comprising the following steps:
step a: coarsely crushing the electrolytic aluminum waste cathode sample;
b, fine crushing, namely further crushing the electrolytic aluminum waste cathode sample after coarse crushing in the step a;
step c: b, grinding, namely grinding the finely crushed waste cathode sample of the electrolytic aluminum in the step b into powder;
step d: alkaline leaching, namely selecting an electrolytic aluminum waste cathode sample with the granularity ranging from 100 meshes to 150 meshes, adding a solvent in a mixed solution of water and petroleum ether according to the mass ratio of 20:5, adding 2.4mL of NaOH solution into each 1g of the electrolytic aluminum waste cathode sample, adjusting the liquid-solid ratio to be 20:1, treating the sample for 25-35min by using an ultrasonic cleaner under the condition of keeping the normal temperature, and standing the sample for 2 hours; after leaching, centrifuging the mixed slurry for 7-10min, leaching the precipitate by using absolute ethyl alcohol and petroleum ether, and reserving the cleaned graphitized carbon sample for later use; in the scheme, the power of the ultrasonic cleaner used in the step d is 300W, and the processing time of the ultrasonic cleaner is 30 min; and d, the centrifugal rotating speed of the mixed slurry in the step d is 10000rpm, and the centrifugal time is 7 min.
Step e: and d, acid leaching, namely adding a certain amount of 10% HCl solution into the graphitized carbon sample cleaned in the step d, leaching for 2 hours at normal temperature, centrifuging the slurry for 7-10min, washing the precipitate once with absolute ethyl alcohol and petroleum ether respectively, and naturally drying to obtain the graphitized carbon. In the scheme, the centrifugal rotating speed of the mixed slurry in the step e is 10000rpm, and the centrifugal time is 7 min.
Step f: and mixing the acid and alkali leaching solutions to obtain the cryolite.
The above description is only exemplary of the present invention and should not be taken as limiting, and any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (3)

1. A process for wet processing of electrolytic aluminum waste cathode material is characterized by comprising the following steps:
step a: coarsely crushing the electrolytic aluminum waste cathode sample;
b, fine crushing, namely further crushing the electrolytic aluminum waste cathode sample after coarse crushing in the step a;
step c: b, grinding, namely grinding the finely crushed waste cathode sample of the electrolytic aluminum in the step b into powder;
step d: alkaline leaching, namely selecting an electrolytic aluminum waste cathode sample with the granularity ranging from 100 meshes to 150 meshes, adding a solvent in a mixed solution of water and petroleum ether according to the mass ratio of 20:5, adding 2.4mL of NaOH solution into each 1g of the electrolytic aluminum waste cathode sample, adjusting the liquid-solid ratio to be 20:1, treating the sample for 25-35min by using an ultrasonic cleaner under the condition of keeping the normal temperature, and standing the sample for 2 hours; after leaching, centrifuging the mixed slurry for 7-10min, leaching the precipitate by using absolute ethyl alcohol and petroleum ether, and reserving the cleaned graphitized carbon sample for later use;
step e: d, acid leaching, namely adding a certain amount of 10% HCl solution into the graphitized carbon sample cleaned in the step d, leaching for 2 hours at normal temperature, centrifuging the slurry for 7-10min, washing the precipitate once with absolute ethyl alcohol and petroleum ether respectively, and naturally drying to obtain graphitized carbon;
step f: and mixing the acid and alkali leaching solutions to obtain the cryolite.
2. The process for the wet treatment of spent cathode material of electrolytic aluminum according to claim 1, characterized in that: the power of the ultrasonic cleaner used in the step d is 300W, and the processing time of the ultrasonic cleaner is 30 min; and d, the centrifugal rotating speed of the mixed slurry in the step d is 10000rpm, and the centrifugal time is 7 min.
3. The process for the wet treatment of spent cathode material of electrolytic aluminum according to claim 1, characterized in that: and e, the centrifugal rotation speed of the mixed slurry in the step e is 10000rpm, and the centrifugal time is 7 min.
CN202011533222.1A 2020-12-23 2020-12-23 Process for wet treatment of electrolytic aluminum waste cathode material Pending CN112624101A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117263178A (en) * 2023-09-28 2023-12-22 昆明理工大学 Method for preparing high-quality graphite by catalytic graphitization of waste cathode carbon

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US4889695A (en) * 1985-02-20 1989-12-26 Aluminum Company Of America Reclaiming spent potlining
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CN101811695A (en) * 2010-04-02 2010-08-25 北京矿冶研究总院 Method for recovering graphite from electrolytic aluminum waste cathode carbon block
CN102976382A (en) * 2012-05-10 2013-03-20 郑州轻工业学院 Method for regenerating cryolite from electrolytic aluminum waste material
CN107857263A (en) * 2017-11-28 2018-03-30 国家电投集团远达环保催化剂有限公司 A kind of ultrasonic wave alkali leaching and the method for pressurized acid leaching Combined Treatment electrolytic aluminium waste cathode carbon block
CN109719118A (en) * 2019-01-04 2019-05-07 亚太环保股份有限公司 A kind of aluminium cell solid waste recycling treatment system and method
CN111943189A (en) * 2019-05-14 2020-11-17 郑州轻工业学院 Method for purifying graphite from waste cathode carbon block
CN111943190A (en) * 2019-05-14 2020-11-17 郑州轻工业学院 Method for recovering graphite from electrolytic aluminum waste cathode carbon block

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GB8301974D0 (en) * 1983-01-25 1983-02-23 Alcan Int Ltd Aluminium fluoride from scrap
US4889695A (en) * 1985-02-20 1989-12-26 Aluminum Company Of America Reclaiming spent potlining
CN101386017A (en) * 2008-10-17 2009-03-18 东北大学 Method for treating aluminum electrolysis waste cathode carbon block using acid and alkali combination method
CN101811695A (en) * 2010-04-02 2010-08-25 北京矿冶研究总院 Method for recovering graphite from electrolytic aluminum waste cathode carbon block
CN102976382A (en) * 2012-05-10 2013-03-20 郑州轻工业学院 Method for regenerating cryolite from electrolytic aluminum waste material
CN107857263A (en) * 2017-11-28 2018-03-30 国家电投集团远达环保催化剂有限公司 A kind of ultrasonic wave alkali leaching and the method for pressurized acid leaching Combined Treatment electrolytic aluminium waste cathode carbon block
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CN111943190A (en) * 2019-05-14 2020-11-17 郑州轻工业学院 Method for recovering graphite from electrolytic aluminum waste cathode carbon block

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN117263178A (en) * 2023-09-28 2023-12-22 昆明理工大学 Method for preparing high-quality graphite by catalytic graphitization of waste cathode carbon
CN117263178B (en) * 2023-09-28 2024-07-02 昆明理工大学 Method for preparing high-quality graphite by catalytic graphitization of waste cathode carbon

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