CN110540221A - Method for preparing magnesium-aluminum hydrotalcite from waste electrolyte slurry of aluminum-air battery - Google Patents
Method for preparing magnesium-aluminum hydrotalcite from waste electrolyte slurry of aluminum-air battery Download PDFInfo
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- CN110540221A CN110540221A CN201910995557.6A CN201910995557A CN110540221A CN 110540221 A CN110540221 A CN 110540221A CN 201910995557 A CN201910995557 A CN 201910995557A CN 110540221 A CN110540221 A CN 110540221A
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- aluminum
- magnesium
- electrolyte slurry
- waste electrolyte
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/78—Compounds containing aluminium and two or more other elements, with the exception of oxygen and hydrogen
- C01F7/784—Layered double hydroxide, e.g. comprising nitrate, sulfate or carbonate ions as intercalating anions
- C01F7/785—Hydrotalcite
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/82—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
Abstract
The invention provides a method for preparing magnesium-aluminum hydrotalcite from waste electrolyte slurry of an aluminum-air battery, which relates to the technical field of solid waste utilization and comprises the following steps: weighing waste electrolyte slurry and putting the waste electrolyte slurry into a container on the basis of analyzing the solid content of the waste electrolyte slurry and the content of Al and Mg elements of the waste electrolyte slurry, taking the waste electrolyte slurry as a main aluminum source, providing an alkaline condition, taking carbon dioxide as a main carbon source, supplementing a magnesium source to ensure that the molar ratio of the magnesium source to the aluminum source is n (Mg) ((Al) ((3: 1), fully stirring and then putting the mixture into a constant-temperature water tank, introducing carbon dioxide gas into the slurry through a bubbler to continuously stir, and reacting the magnesium source, the aluminum source and the carbon dioxide in the waste slurry to obtain a reaction product; and (4) moving the reaction product to a reaction kettle for reaction, and collecting the carbonate magnesium aluminum hydrotalcite from the reaction product. The method realizes the reutilization of waste resources, has simple preparation process, is environment-friendly and energy-saving, and effectively reduces the production cost of the magnesium-aluminum hydrotalcite.
Description
Technical Field
The invention relates to the technical field of solid waste utilization, in particular to a method for preparing magnesium-aluminum hydrotalcite from waste electrolyte slurry of an aluminum-air battery.
background
The aluminum-air battery consists of three parts, namely a positive electrode, a negative electrode and electrolyte. The negative electrode is usually made of high-purity aluminum or aluminum alloy; the anode is composed of a waterproof breathable film, a catalyst and a conductive material; the electrolyte is composed of a neutral salt solution or an alkali metal hydroxide (KOH or NaOH) solution. When the battery works, the metal aluminum of the negative electrode loses electrons under the action of electrolyte and becomes Al (OH)3 or AlO2-, and meanwhile, a small amount of alloy elements such as: mg also reacts to form Mg (OH) 2; oxygen (air) enters through the waterproof breathable film of the anode and generates electrochemical reaction to generate OH < - > under the action of a catalyst and an electrolyte. Therefore, after the aluminum-air battery works for a period of time, waste electrolyte slurry containing Al (OH)3, AlO2-, Mg (OH)2 and the like is formed in the electrolyte. However, there has been no report on the preparation of hydrotalcite using a waste electrolyte slurry generated from an aluminum-air battery.
hydrotalcite is a layered double hydroxide, is a typical layered novel functional material, belongs to an anionic compound, has a typical chemical formula of [ Mg6Al2(OH)16] CO 3.4H 2O, is a layered compound infinitely extended by magnesium-oxygen octahedrons through a prism, and is combined by layer under the action of hydrogen bonds to form a Layered Double Hydroxide (LDHs) consisting of a positively charged metal hydroxide layer and a negatively charged interlayer anion.
The synthesis of hydrotalcite is carried out by using chemical reagents such as: aluminum hydroxide, magnesium hydroxide or magnesium oxide is produced by reacting with an alkaline substance, and therefore, the production cost is high. The waste electrolyte slurry generated by the aluminum-air battery contains alkaline substances, an aluminum source and a magnesium source, and the magnesium-aluminum hydrotalcite can be prepared by only supplementing a proper amount of the magnesium source in the ingredients.
Disclosure of Invention
technical problem to be solved
aiming at the defects of the prior art, the invention provides a method for preparing magnesium-aluminum hydrotalcite by using waste electrolyte slurry of an aluminum-air battery, which realizes the utilization of waste resources, saves energy and reduces cost.
(II) technical scheme
In order to achieve the purpose, the invention is realized by the following technical scheme:
A method for preparing magnesium-aluminum hydrotalcite from waste electrolyte slurry of an aluminum-air battery is characterized by comprising the following steps:
(1) Weighing waste electrolyte slurry and putting the waste electrolyte slurry into a container on the basis of analyzing the solid content of the waste electrolyte slurry and the content of Al and Mg elements of the waste electrolyte slurry, taking the waste electrolyte slurry as a main aluminum source, providing an alkaline condition, taking carbon dioxide as a main carbon source, supplementing a magnesium source to ensure that the molar ratio of the magnesium source to the aluminum source is n (Mg) ((Al) ((3: 1), fully stirring and then putting the mixture into a constant-temperature water tank, introducing carbon dioxide gas into the slurry through a bubbler to continuously stir, and reacting the magnesium source, the aluminum source and the carbon dioxide in the waste slurry to obtain a reaction product;
(2) And (4) moving the reaction product to a reaction kettle for reaction, and collecting the carbonate magnesium aluminum hydrotalcite from the reaction product.
Further, in the step (1), the heating temperature of the water bath in the constant-temperature water tank is 40-80 ℃, and the reaction time of the reaction is 20-40 min.
Further, the reaction temperature of the reaction kettle in the step (2) is 120-.
Further, the collection method in the step (2) comprises cooling, filtering, washing and drying.
further, during filtration and washing, the pH value is washed to 9-10, and the filtrate is dried for 5h at 80 ℃.
(III) advantageous effects
The invention provides a method for preparing magnesium-aluminum hydrotalcite from waste electrolyte slurry of an aluminum-air battery, which realizes the reutilization of waste resources, has simple preparation process, is environment-friendly and energy-saving and effectively reduces the production cost of the magnesium-aluminum hydrotalcite.
Drawings
FIG. 1 is an X-ray diffraction pattern of the magnesium aluminum hydrotalcite prepared in example 1;
FIG. 2 is an infrared spectrum of the magnesium aluminum hydrotalcite prepared in example 1;
FIG. 3 is an X-ray diffraction pattern of the magnesium aluminum hydrotalcite prepared in example 2;
FIG. 4 is a transmission electron microscope spectrum of the Mg-Al hydrotalcite prepared in example 2;
FIG. 5 is a transmission electron microscope atlas of Mg-Al hydrotalcite prepared in example 2;
FIG. 6 is a transmission electron microscope atlas of Mg-Al hydrotalcite prepared in example 2;
FIG. 7 is a transmission electron microscope atlas of Mg-Al hydrotalcite prepared in example 2;
FIG. 8 is an infrared spectrum of the magnesium aluminum hydrotalcite prepared in example 2;
FIG. 9 is an X-ray diffraction pattern of the magnesium aluminum hydrotalcite prepared in example 3;
FIG. 10 is an infrared spectrum of the magnesium aluminum hydrotalcite prepared in example 3;
FIG. 11 is an X-ray diffraction pattern of the magnesium aluminum hydrotalcite prepared in example 4;
FIG. 12 is an infrared spectrum of the magnesium aluminum hydrotalcite prepared in example 4;
FIG. 13 is an X-ray diffraction pattern of the magnesium aluminum hydrotalcite prepared in example 5;
FIG. 14 is an infrared spectrum of magnesium aluminum hydrotalcite prepared in example 5.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, 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 invention.
example 1:
preparing magnesium-aluminum hydrotalcite by using waste electrolyte slurry of an aluminum-air battery: weighing 15ml of waste slurry in a beaker, adding deionized water to 150ml, heating and stirring in a water bath at 80 ℃ for 5min, then weighing 5g of magnesium oxide in the beaker, heating and stirring in the water bath for 40min, introducing carbon dioxide into the beaker, heating and stirring in the water bath for 40min, finally transferring a reaction product into a reaction kettle, continuously reacting for 6h at 180 ℃, cooling, filtering and washing for several times to obtain the wet hydrotalcite material. Drying at 80 ℃ for 5h to obtain the magnesium-aluminum hydrotalcite.
Example 2:
preparing magnesium-aluminum hydrotalcite by using waste electrolyte slurry of an aluminum-air battery: weighing 15ml of waste slurry in a beaker, adding deionized water to 150ml, heating and stirring for 5min at 80 ℃ in a water bath; then weighing 5g of magnesium oxide in a beaker, heating in a water bath and stirring for 30 min; then introducing carbon dioxide into the beaker, and heating and stirring for 30min in a water bath at the same time; finally, moving the reaction product into a reaction kettle, and continuously reacting for 6 hours at 180 ℃; after cooling, filtering and washing for several times to obtain the hydrotalcite wet material. Drying at 80 ℃ for 5h to obtain the magnesium-aluminum hydrotalcite. The element contents of the magnesium-aluminum hydrotalcite are shown in table 1.
Table 1:
example 3:
Preparing magnesium-aluminum hydrotalcite by using waste electrolyte slurry of an aluminum-air battery: weighing 15ml of waste slurry in a beaker, adding deionized water to 150ml, heating and stirring for 5min at 80 ℃ in a water bath; then weighing 4.23g of magnesium oxide in a beaker, heating in a water bath and stirring for 20 min; then introducing carbon dioxide into the beaker, and heating and stirring for 20min in a water bath at the same time; finally, moving the reaction product into a reaction kettle, and continuously reacting for 6 hours at 180 ℃; after cooling, filtering and washing for several times to obtain the hydrotalcite wet material. Drying at 80 ℃ for 5h to obtain the magnesium-aluminum hydrotalcite.
Example 4:
preparing magnesium-aluminum hydrotalcite by using waste electrolyte slurry of an aluminum-air battery: measuring 15ml of waste slurry in a beaker, adding deionized water to 150ml, heating and stirring for 5min at 60 ℃ in a water bath; then weighing 4.23g of magnesium oxide in a beaker, heating in a water bath and stirring for 30 min; then introducing carbon dioxide into the beaker, and heating and stirring for 30min in a water bath at the same time; finally, moving the reaction product into a reaction kettle, and continuously reacting for 10 hours at 150 ℃; after cooling, filtering and washing for several times to obtain the hydrotalcite wet material. Drying at 80 ℃ for 5h to obtain the magnesium-aluminum hydrotalcite.
example 5:
preparing magnesium-aluminum hydrotalcite by using waste electrolyte slurry of an aluminum-air battery: weighing 15ml of waste slurry in a beaker, adding deionized water to 150ml, heating and stirring for 5min at 40 ℃ in a water bath; then weighing 4.23g of magnesium oxide in a beaker, heating in a water bath and stirring for 30 min; then introducing carbon dioxide into the beaker, and heating and stirring for 30min in a water bath at the same time; finally, moving the reaction product into a reaction kettle, and continuously reacting for 15 hours at 120 ℃; after cooling, filtering and washing for several times to obtain the hydrotalcite wet material. Drying at 80 ℃ for 5h to obtain the magnesium-aluminum hydrotalcite.
In summary, the embodiment of the invention has the following beneficial effects: in the embodiments 1-5 of the invention, the magnalium hydrotalcite is prepared by using the waste electrolyte slurry of the aluminum-air battery, so that the waste resource is recycled, the preparation process is simple, environment-friendly and energy-saving, and the production cost of the magnalium hydrotalcite is reduced.
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (6)
1. a method for preparing magnesium-aluminum hydrotalcite from waste electrolyte slurry of an aluminum-air battery is characterized by comprising the following steps:
(1) Weighing waste electrolyte slurry on the basis of analysis of the solid content and the contents of Al and Mg elements of the waste electrolyte slurry, putting the waste electrolyte slurry into a container, supplementing a magnesium source, enabling the molar ratio of the magnesium source to an aluminum source to be n (Mg): n (Al): 3:1, fully stirring, putting the mixture into a constant-temperature water tank, introducing carbon dioxide gas into the slurry through a bubbler, and continuously stirring, wherein the magnesium source, the aluminum source and the carbon dioxide react in the waste electrolyte slurry to obtain a reaction product;
(2) and (4) moving the reaction product to a reaction kettle for reaction, and collecting the carbonate magnesium aluminum hydrotalcite from the reaction product.
2. the method for preparing magnesium aluminum hydrotalcite from waste electrolyte slurry of aluminum-air battery as claimed in claim 1, wherein the waste electrolyte slurry is used as main aluminum source and alkaline condition is provided, and carbon dioxide is used as main carbon source.
3. The method for preparing magnesium-aluminum hydrotalcite from waste electrolyte slurry of aluminum-air battery as claimed in claim 1, wherein the heating temperature of water bath in the thermostatic water tank in step (1) is 40-80 ℃, and the stirring reaction time is 20-40 min.
4. the method for preparing the magnesium-aluminum hydrotalcite with the waste electrolyte slurry of the aluminum-air battery as claimed in claim 1, wherein the reaction temperature of the reaction kettle in the step (2) is 120-180 ℃ and the time is 6-15 h.
5. The method for preparing the magnesium-aluminum hydrotalcite from the waste electrolyte slurry of the aluminum-air battery as claimed in claim 1, wherein the collection method in the step (2) is cooling, filtering, washing and drying.
6. the method for preparing Mg-Al hydrotalcite from waste electrolyte slurry of Al-air battery as claimed in claim 5, wherein the pH value is 9-10 after filtration and washing, and the filtrate is dried at 80 ℃ for 5 h.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113526532A (en) * | 2021-06-30 | 2021-10-22 | 云南创能斐源金属燃料电池有限公司 | Method for treating waste electrolyte of aluminum-air battery |
CN113620326A (en) * | 2021-08-20 | 2021-11-09 | 云南创能斐源金属燃料电池有限公司 | Method for preparing magnesium-aluminum-zinc hydrotalcite from aluminum-air battery electrolysis waste liquid and application thereof |
CN113697833A (en) * | 2021-08-09 | 2021-11-26 | 云南创能斐源金属燃料电池有限公司 | Method for preparing hydrotalcite and application thereof |
Citations (2)
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CN106663830A (en) * | 2014-04-13 | 2017-05-10 | 奥科宁克有限公司 | Systems and methods for regeneration of aqueous alkaline solution |
CN107416872A (en) * | 2017-09-01 | 2017-12-01 | 上海华峰新材料研发科技有限公司 | The preparation method of magnalium carbonate form hydrotalcite |
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2019
- 2019-10-18 CN CN201910995557.6A patent/CN110540221A/en active Pending
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN106663830A (en) * | 2014-04-13 | 2017-05-10 | 奥科宁克有限公司 | Systems and methods for regeneration of aqueous alkaline solution |
CN107416872A (en) * | 2017-09-01 | 2017-12-01 | 上海华峰新材料研发科技有限公司 | The preparation method of magnalium carbonate form hydrotalcite |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113526532A (en) * | 2021-06-30 | 2021-10-22 | 云南创能斐源金属燃料电池有限公司 | Method for treating waste electrolyte of aluminum-air battery |
CN113697833A (en) * | 2021-08-09 | 2021-11-26 | 云南创能斐源金属燃料电池有限公司 | Method for preparing hydrotalcite and application thereof |
CN113620326A (en) * | 2021-08-20 | 2021-11-09 | 云南创能斐源金属燃料电池有限公司 | Method for preparing magnesium-aluminum-zinc hydrotalcite from aluminum-air battery electrolysis waste liquid and application thereof |
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Application publication date: 20191206 |