CN119040657B - A system and method for efficiently separating and extracting lithium from electrolytic aluminum solid waste - Google Patents
A system and method for efficiently separating and extracting lithium from electrolytic aluminum solid waste Download PDFInfo
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- CN119040657B CN119040657B CN202411175140.2A CN202411175140A CN119040657B CN 119040657 B CN119040657 B CN 119040657B CN 202411175140 A CN202411175140 A CN 202411175140A CN 119040657 B CN119040657 B CN 119040657B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B26/00—Obtaining alkali, alkaline earth metals or magnesium
- C22B26/10—Obtaining alkali metals
- C22B26/12—Obtaining lithium
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- C—CHEMISTRY; METALLURGY
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/20—Graphite
- C01B32/21—After-treatment
- C01B32/215—Purification; Recovery or purification of graphite formed in iron making, e.g. kish graphite
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/001—Dry processes
- C22B7/003—Dry processes only remelting, e.g. of chips, borings, turnings; apparatus used therefor
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Abstract
本发明提供一种从电解铝固废中分离提锂的系统及方法，该方法先将废阴极炭块破碎，然后以高温电炉加热将电解质从废阴极炭块中分离，最后将电解质注入到熔盐电化学反应炉中持续加热，以去除电解质中杂质、进一步富集Li元素。该方法不仅可以将废阴极炭块中的电解质与炭质组分高效分离，还能从分离出的电解质中富集含锂物质，解决了电解铝工业生产中产生的大量危险废弃物废阴极炭块无法无害化资源化处置的问题，实现了电解铝固废的高效资源化再利用。
The present invention provides a system and method for separating and extracting lithium from electrolytic aluminum solid waste. The method first crushes the waste cathode carbon blocks, then separates the electrolyte from the waste cathode carbon blocks by heating in a high-temperature electric furnace, and finally injects the electrolyte into a molten salt electrochemical reactor for continuous heating to remove impurities in the electrolyte and further enrich the Li element. This method can not only efficiently separate the electrolyte from the carbonaceous components in the waste cathode carbon blocks, but also enrich lithium-containing substances from the separated electrolyte, solving the problem that a large amount of hazardous waste waste cathode carbon blocks generated in the electrolytic aluminum industry cannot be harmlessly disposed of, and realizes efficient resource recycling of electrolytic aluminum solid waste.
Description
Technical Field
The invention relates to the field of environmental protection solid waste treatment, in particular to a system and a method for efficiently separating and extracting lithium from electrolytic aluminum solid waste.
Background
The waste cathode carbon blocks are solid waste which is overhauled and replaced by the problems of deformation, cracking and the like after being used for 4-6 years because the cathode carbon blocks at the bottom and the side parts of the electrolytic tank are inevitably corroded by high-temperature melt (950-970 ℃) for a long time in the production process of electrolytic aluminum. The waste cathode carbon block is classified as nonferrous metal smelting waste (HW 48) by the national hazardous waste directory (2021 edition) because of adsorbing a large amount of soluble fluoride, a small amount of cyanide and other harmful substances, and the code is 321-023-48.
The production of waste cathode carbon blocks is about 10-15 kg per 1t of raw aluminum in China, and the production of electrolytic aluminum in China is 4159 ten thousand tons by taking 2023 as an example, so that the annual production of the waste cathode carbon blocks is 41.59 ten thousand tons to 62.38 ten thousand tons. The waste cathode carbon block mainly comprises carbonaceous components (about 60% -70%) and electrolyte (about 30% -40%), wherein the two components have higher recovery value, particularly the electrolyte, and along with development and application of lithium-containing medium-low grade bauxite in recent years, the concentration of Li element can reach 1.0% -2.7% (calculated by Li +) in the electrolyte of an aluminum electrolysis cell using the alumina raw material, so that the lithium carbonate production enterprises are gradually concerned. Therefore, the high-efficiency recycling of the electrolytic aluminum waste cathode carbon block, and particularly the separation and extraction of lithium elements from the electrolytic aluminum waste cathode carbon block, have important significance.
Disclosure of Invention
In order to solve the problems, the invention provides a method for efficiently separating and extracting lithium from electrolytic aluminum solid waste, which comprises the following steps:
and 1, delivering the electrolytic aluminum waste cathode carbon blocks into a crusher for crushing.
And 2, loading the crushed waste cathode carbon blocks into a high-temperature melting furnace, and loading a covering material on the upper layer of the high-temperature melting furnace to prevent high-temperature oxidation.
And 3, carrying out power transmission heating on the high-temperature melting furnace, discharging gas generated in the heating process through negative pressure of an exhaust port, and discharging the gas after innocent treatment.
And 4, after the heating is finished, the carbon components in the waste cathode carbon blocks are reserved in a high-temperature melting furnace, electrolyte close to a cathode of the high-temperature melting furnace flows into a cathode end of a molten salt electrolysis furnace from a No.1 discharge port, electrolyte close to an anode of the high-temperature melting furnace flows into an anode end of the molten salt electrolysis furnace from a No. 2 discharge port, after the electrolyte is added, the molten salt electrolysis furnace is sealed, power is continuously supplied for heating for a period of time, li elements are fully enriched at the cathode end of the molten salt electrolysis furnace, and finally lithium-rich electrolyte is obtained at the cathode end of the molten salt electrolysis furnace, and lithium-poor electrolyte is obtained at the anode end of the molten salt electrolysis furnace.
In some embodiments, the crusher in step 1 is one or more of a jaw crusher, a box crusher, a hammer crusher, a roller ball mill.
In some embodiments, step 1 entails crushing the spent cathode carbon blocks into 3-10 cm pieces.
In some embodiments, the coating in step 2 is one or more of alumina, anthracite, graphite powder.
In some embodiments, in step 3, the high-temperature melting furnace is heated by applying a voltage according to a preset temperature schedule, where the temperature schedule is as follows:
The first section is at room temperature to 1000 ℃ for 0 to 15 hours;
the second section is 1000-2200 ℃ for 15-25 hours;
the third section is 2000-2200 ℃ for 25-40 h;
and in the fourth stage, the temperature is 2200 ℃ to room temperature, the time is 40 to 60 hours, and the temperature is naturally cooled until the mechanical operation slag removal can be performed.
And 4, after heating, the carbonaceous components in the waste cathode carbon blocks are remained in a high-temperature melting furnace, and can be taken out through slag skimming. The carbon component is mainly graphite, the purity is 90% -98%, and the carbon component can be used as resources for recycling after being crushed into graphite blocks or graphite powder. In some embodiments, after the carbonaceous component is crushed into particles of 0-10 mm, the particles are returned to the step 2 to be recycled as a covering material.
In some embodiments, in step 4, the molten salt electrolysis furnace is preheated to a temperature of >400 ℃ before the electrolyte discharged from the high temperature tapping furnace flows into the molten salt electrolysis furnace.
In some embodiments, in step 4, the heating temperature is 1200-1400 ℃ and the time is 5-10 hours.
After separation and discharge, the Li content in the lithium-rich electrolyte is more than 4 percent, and the Li content in the lithium-poor electrolyte is less than 0.3 percent.
In another aspect, the invention also provides a system for separating and extracting lithium from solid waste of electrolytic aluminum, which can be used for executing the method as described above, comprising the following parts:
The crusher is used for crushing the electrolytic aluminum waste cathode carbon blocks;
The high-temperature melting furnace is used for accommodating broken waste cathode carbon blocks, the upper layer of the waste cathode carbon blocks is filled with covering materials to prevent high-temperature oxidation, then the waste cathode carbon blocks are heated by power transmission, gas generated in the heating process is discharged from an exhaust port under negative pressure and is exhausted after innocent treatment;
the molten salt electrolysis furnace is continuously powered and heated to fully enrich Li element at the cathode end of the molten salt electrolysis furnace, and finally, a lithium-rich electrolyte is obtained at the cathode end of the molten salt electrolysis furnace, and a lithium-poor electrolyte with higher purity is obtained at the anode end of the molten salt electrolysis furnace.
In some embodiments, the furnace body material of the molten salt electrolysis furnace is graphite.
In some embodiments, the lining material of the high-temperature melting furnace is one or more of silicon carbide bricks, magnesia carbon bricks, high-alumina hollow bricks and silicon nitride bricks, and is built by adopting a multi-layer continuous masonry mode.
In some embodiments, at the bottom of the high temperature melting furnace, two inverted conical structures are respectively arranged at the cathode and the anode, and the positions of the two inverted conical structures correspond to the No. 1 discharge port and the No. 2 discharge port respectively, so that the electrolyte in a molten state is collected and discharged through the discharge ports quickly.
The method provided by the invention can not only efficiently separate the electrolyte and the carbonaceous component in the waste cathode carbon block, but also enrich the lithium-containing substance from the separated electrolyte, solves the problem that a large amount of dangerous waste cathode carbon block generated in the industrial production of electrolytic aluminum cannot be subjected to harmless recycling treatment, and realizes the efficient recycling of the solid waste of electrolytic aluminum.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the description of the embodiments below are briefly introduced, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and that other drawings can be obtained according to these drawings without inventive effort for a person skilled in the art.
Fig. 1 shows a flow chart of a method for efficiently separating and extracting lithium from electrolytic aluminum solid waste.
Detailed Description
The following describes the scheme provided in the present specification with reference to the drawings.
In order to make the objects, technical solutions and advantages of the embodiments of the present application more apparent, the technical solutions of the embodiments of the present application will be described below with reference to the accompanying drawings.
In describing embodiments of the present application, words such as "exemplary," "such as" or "for example" are used to mean serving as examples, illustrations or explanations. Any embodiment or design described herein as "exemplary," "such as" or "for example" is not necessarily to be construed as preferred or advantageous over other embodiments or designs. Rather, the use of words such as "exemplary," "such as" or "for example," etc., is intended to present related concepts in a concrete fashion.
In the description of the embodiment of the present application, the term "and/or" is merely an association relationship describing the association object, and indicates that three relationships may exist, for example, a and/or B, and may indicate that a exists alone, B exists alone, and both a and B exist. In addition, unless otherwise indicated, the term "plurality" means two or more.
Furthermore, the terms "first," "second," and the like, are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating an indicated technical feature. Thus, a feature defining "a first" or "a second" may explicitly or implicitly include one or more such feature. The terms "comprising," "including," "having," and variations thereof mean "including but not limited to," unless expressly specified otherwise.
The invention provides a method for efficiently separating and extracting lithium from solid waste of electrolytic aluminum, which comprises the steps of crushing waste cathode carbon blocks, heating the waste cathode carbon blocks by a high-temperature electric furnace to separate electrolyte from the waste cathode carbon blocks, and finally injecting the electrolyte into a molten salt electrochemical reaction furnace to achieve the purposes of removing impurities in the electrolyte and further enriching Li elements. The method provided by the invention is further explained below with reference to the accompanying drawings, wherein the process flow chart of the method is shown in fig. 1, and the specific steps are as follows:
and 1, delivering the electrolytic aluminum waste cathode carbon blocks into a crusher for crushing.
In some embodiments, the crusher is one or more of a jaw crusher, a box crusher, a hammer crusher, a roller ball mill.
In some embodiments, step 1 entails crushing the spent cathode carbon blocks into 3-10 cm pieces.
The step is to crush the waste cathode carbon block to facilitate subsequent assembly, filling and heating, and separating electrolyte.
And 2, loading the crushed waste cathode carbon blocks into a high-temperature melting furnace, and loading a covering material on the upper layer of the high-temperature melting furnace to prevent high-temperature oxidation.
In some embodiments, the coating in step 2 is one or more of alumina, anthracite, graphite powder.
Step 3, power is transmitted to the high-temperature melting furnace for heating, and gas generated in the heating process is discharged through negative pressure of an exhaust port and is discharged after innocent treatment;
In some embodiments, in step 3, the high-temperature melting furnace is heated by applying a voltage according to a preset temperature schedule, where the temperature schedule is as follows:
The first section is at room temperature to 1000 ℃ for 0 to 15 hours;
a second stage, at 1000-2200 ℃ for 15-25 hours,
The third section is 2000-2200 ℃ for 25-40 h;
and in the fourth stage, the temperature is 2200 ℃ to room temperature, the time is 40 to 60 hours, and the temperature is naturally cooled until the mechanical operation slag removal can be performed.
The step is power transmission heating, and is to realize the effect of efficiently separating the electrolyte and the carbonaceous component in the waste cathode carbon block. After the heating is finished, the electrolyte in a molten state sinks into the lower layer of the high-temperature melting furnace, flows out into the molten salt electrolysis furnace in the step 4, and the carbonaceous component is reserved in the high-temperature melting furnace.
And 4, after the heating is finished, the carbon components in the waste cathode carbon blocks are reserved in a high-temperature melting furnace, electrolyte close to a cathode of the high-temperature melting furnace flows into a cathode end of a molten salt electrolysis furnace from a No.1 discharge port, electrolyte close to an anode of the high-temperature melting furnace flows into an anode end of the molten salt electrolysis furnace from a No. 2 discharge port, after the electrolyte is added, the molten salt electrolysis furnace is sealed, power is continuously supplied for heating for a period of time, li elements are fully enriched at the cathode end of the molten salt electrolysis furnace, and finally lithium-rich electrolyte is obtained at the cathode end of the molten salt electrolysis furnace, and lithium-poor electrolyte is obtained at the anode end of the molten salt electrolysis furnace.
And 4, after heating, the carbonaceous components in the waste cathode carbon blocks are remained in a high-temperature melting furnace, and can be taken out through slag skimming. The carbon component is mainly graphite, the purity is 90% -98%, and the carbon component can be used as resources for recycling after being crushed into graphite blocks or graphite powder. In some embodiments, after the carbonaceous component in step 4 is crushed into particles of 0-10 mm, the particles are returned to step 2 to be recycled as a covering material.
In some embodiments, in step 4, the molten salt electrolysis furnace is preheated to a temperature of >400 ℃ before the electrolyte discharged from the high temperature tapping furnace flows into the molten salt electrolysis furnace.
In some embodiments, in step 4, the heating temperature is 1200-1400 ℃ and the time is 5-10 hours.
After separation and discharge, the Li content in the lithium-rich electrolyte is more than 4 percent, and the Li content in the lithium-poor electrolyte is less than 0.3 percent.
The method for treating the solid waste of the electrolytic aluminum provided by the invention is specifically described by combining the following examples:
Example 1
1000Kg of waste cathode carbon blocks of electrolytic aluminum to be treated are taken and added into a box-type crusher, crushed to 3-10 cm and then sent into a high-temperature melting furnace, and a covering material is filled in the upper layer to prevent high-temperature oxidation. And (3) carrying out power transmission heating on the high-temperature melting furnace according to a preset temperature system, discharging gas generated in the heating process through negative pressure of an exhaust port, and exhausting after innocent treatment. The temperature system is as follows:
The first section is at room temperature to 1000 ℃ for 13 hours;
the second section is 1000-2200 ℃ for 20h;
The third section is 2000-2200 ℃ for 30 hours;
and fourthly, naturally cooling to 2200 ℃ to room temperature until mechanically operated slag removal is achieved.
After heating, the carbonaceous component in the waste cathode carbon block is remained in a high-temperature melting furnace, and is taken out through slag skimming, so as to obtain 654kg of carbonaceous component for standby, and the main component is graphite. Electrolyte close to a cathode of the high-temperature melting furnace flows into a cathode end of the molten salt electrolysis furnace from a No. 1 discharge port, electrolyte close to an anode of the high-temperature melting furnace flows into an anode end of the molten salt electrolysis furnace from a No. 2 discharge port, after the electrolyte is added, the molten salt electrolysis furnace is sealed and continuously powered on for heating, the heating temperature is 1300 ℃, the time is 6 hours, and finally 148kg of lithium-rich electrolyte is obtained at the cathode end of the molten salt electrolysis furnace, and 153kg of lithium-poor electrolyte is obtained at the anode end of the molten salt electrolysis furnace. The gas and dust discharged by the negative pressure was about 45kg. The Li content (calculated as Li +) in the lithium-rich electrolyte was 5.4% and the Li content (calculated as Li +) in the lithium-poor electrolyte was 0.2% as measured.
In summary, compared with the prior art, the method for efficiently separating and extracting lithium from the electrolytic aluminum solid waste has the following beneficial effects:
1) The invention adopts an electric heating mode to recycle and treat the electrolytic aluminum solid waste, thereby effectively reducing the environmental pollution and improving the operation safety coefficient;
2) The high-temperature melting furnace adopted by the invention can resist high temperature and corrosion, realize high-efficiency separation of electrolyte and carbonaceous components in the waste cathode carbon blocks, and the adopted molten salt electrolysis furnace can enrich Li element by utilizing the characteristic of molten salt electrolysis, thereby realizing the purpose of recycling the waste cathode carbon blocks.
3) The solid waste of electrolytic aluminum is treated by adopting a fire method, the process flow is shortened, the electrolyte and the carbonaceous component are separated by high-temperature melting, the electrolyte can be further recycled, the Li element in the electrolyte is enriched, and the energy can be greatly saved in industrial production.
In another aspect, the invention also provides a system for separating and extracting lithium from solid waste of electrolytic aluminum, which can be used for executing the method as described above, comprising the following parts:
The crusher is used for crushing the electrolytic aluminum waste cathode carbon blocks;
The high-temperature melting furnace is used for accommodating broken waste cathode carbon blocks, the upper layer of the waste cathode carbon blocks is filled with covering materials to prevent high-temperature oxidation, then the waste cathode carbon blocks are heated by power transmission, gas generated in the heating process is discharged from an exhaust port under negative pressure and is exhausted after innocent treatment;
in some embodiments, the lining material of the high-temperature melting furnace is one or more of silicon carbide bricks, magnesia carbon bricks, high-alumina hollow bricks and silicon nitride bricks, and is built by adopting a multi-layer continuous masonry mode.
In some embodiments, at the bottom of the high temperature melting furnace, two inverted conical structures are respectively arranged at the cathode and the anode, and the positions of the two inverted conical structures correspond to the No. 1 discharge port and the No. 2 discharge port respectively, so that the electrolyte in a molten state is collected and discharged through the discharge ports quickly.
The lithium-rich electrolyte is finally obtained at the cathode end of the molten salt electrolysis furnace, and the lithium-poor electrolyte with higher purity is obtained at the anode end of the molten salt electrolysis furnace. In some embodiments, the furnace body material of the molten salt electrolysis furnace is graphite.
It is noted that the above components can be assembled into a production line to realize the automatic treatment of the waste cathode carbon blocks of the electrolytic aluminum. In addition, the functions of the components can be referred to the related embodiments in the description of the method, which is not described in detail.
The foregoing embodiments have been provided for the purpose of illustrating the general principles of the present invention in further detail, and are not to be construed as limiting the scope of the invention, but are merely intended to cover any modifications, equivalents, improvements, etc. based on the teachings of the invention.
Claims (7)
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| CN107285354A (en) * | 2017-07-28 | 2017-10-24 | 唐红艳 | Aluminum carbonaceous dangerous waste watery fusion permeates continuous separation method and products obtained therefrom |
| CN107541753A (en) * | 2017-08-10 | 2018-01-05 | 中国铝业股份有限公司 | A kind of removing method of the Hull cell containing lithium in lithium electrolyte |
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| CN212247234U (en) * | 2020-03-17 | 2020-12-29 | 国家电投集团宁夏能源铝业科技工程有限公司 | Processing system of electrolytic aluminum carbon slag |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107285354A (en) * | 2017-07-28 | 2017-10-24 | 唐红艳 | Aluminum carbonaceous dangerous waste watery fusion permeates continuous separation method and products obtained therefrom |
| CN107541753A (en) * | 2017-08-10 | 2018-01-05 | 中国铝业股份有限公司 | A kind of removing method of the Hull cell containing lithium in lithium electrolyte |
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