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 PDF

Info

Publication number
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
Authority
CN
China
Prior art keywords
aluminum
magnesium
electrolyte slurry
waste electrolyte
source
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201910995557.6A
Other languages
Chinese (zh)
Inventor
武杏荣
潘甜甜
申星梅
曹发斌
王平
李辽沙
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Anhui University of Technology AHUT
Original Assignee
Anhui University of Technology AHUT
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Anhui University of Technology AHUT filed Critical Anhui University of Technology AHUT
Priority to CN201910995557.6A priority Critical patent/CN110540221A/en
Publication of CN110540221A publication Critical patent/CN110540221A/en
Pending legal-status Critical Current

Links

Classifications

    • 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
    • C01F7/78Compounds containing aluminium and two or more other elements, with the exception of oxygen and hydrogen
    • C01F7/784Layered double hydroxide, e.g. comprising nitrate, sulfate or carbonate ions as intercalating anions
    • C01F7/785Hydrotalcite
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/70Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72Crystal-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
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00Crystal-structural characteristics
    • C01P2002/80Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C01P2002/82Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by IR- or Raman-data
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00Particle morphology
    • C01P2004/01Particle morphology depicted by an image
    • C01P2004/04Particle 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

method for preparing magnesium-aluminum hydrotalcite from waste electrolyte slurry of aluminum-air battery
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.
CN201910995557.6A 2019-10-18 2019-10-18 Method for preparing magnesium-aluminum hydrotalcite from waste electrolyte slurry of aluminum-air battery Pending CN110540221A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201910995557.6A CN110540221A (en) 2019-10-18 2019-10-18 Method for preparing magnesium-aluminum hydrotalcite from waste electrolyte slurry of aluminum-air battery

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201910995557.6A CN110540221A (en) 2019-10-18 2019-10-18 Method for preparing magnesium-aluminum hydrotalcite from waste electrolyte slurry of aluminum-air battery

Publications (1)

Publication Number Publication Date
CN110540221A true CN110540221A (en) 2019-12-06

Family

ID=68716017

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201910995557.6A Pending CN110540221A (en) 2019-10-18 2019-10-18 Method for preparing magnesium-aluminum hydrotalcite from waste electrolyte slurry of aluminum-air battery

Country Status (1)

Country Link
CN (1) CN110540221A (en)

Cited By (3)

* Cited by examiner, † Cited by third party
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)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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)

* Cited by examiner, † Cited by third party
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

Similar Documents

Publication Publication Date Title
CN110540221A (en) Method for preparing magnesium-aluminum hydrotalcite from waste electrolyte slurry of aluminum-air battery
CN109775678B (en) Method for preparing battery-grade iron phosphate and industrial-grade lithium phosphate from waste lithium iron phosphate batteries
CN108288693A (en) A kind of anode material of lithium-ion battery zinc-tin bimetallic sulfide and the preparation method and application thereof
CN115477293B (en) Preparation method of anhydrous ferric phosphate with low impurity and high specific surface area
CN111041215B (en) Method for recovering waste lead acid battery
CN109824095B (en) Zinc-doped nickel-manganese hydrotalcite material and preparation method and application thereof
CN113968578A (en) Method for synthesizing iron phosphate by using ferrous sulfate as titanium dioxide byproduct
CN113620326A (en) Method for preparing magnesium-aluminum-zinc hydrotalcite from aluminum-air battery electrolysis waste liquid and application thereof
CN112938922A (en) Method for preparing battery-grade iron phosphate from titanium dioxide byproduct ferrous sulfate
CN113277550B (en) Lead-containing solid waste treatment method, and preparation method and application of lead dioxide powder
CN103663563B (en) Preparation method of potassium ferrate
CN108821394B (en) Preparation method of iron (II) molybdate/graphene oxide catalytic electrode
CN110311114B (en) Method for preparing ternary precursor of lithium battery through circular electrolysis
CN114956027A (en) Porous iron phosphate and preparation method thereof
TWI696309B (en) Method for preparing and purifying lithium carbonate from waste lithium battery
CN112864384A (en) Preparation method and application of positive electrode material lithium iron phosphate
CN112624168A (en) Waste liquid treatment method of aluminum-air battery
CN113511637A (en) Preparation method of bimetallic compound/carbon composite material
CN106349069A (en) Preparation method of methyl p hydroxybenzoate
CN112456545A (en) Method for preparing sodium stannate trihydrate by using tin stripping waste liquid
JP2023522285A (en) Method for producing lithium hydroxide
CN110330423A (en) The method that pressurization prepares stannous octoate
CN114105208B (en) Low-sulfur manganous-manganic oxide and preparation method thereof
CN109734050B (en) Aluminum hydrolysis hydrogen production method based on polymer composite modification
CN114832835B (en) Z-type heterojunction NiS/Co 3 S 4 ZnCdS nano material and preparation method and application thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20191206