阅读说明：本技术 一种以铝-空气电池废电解液浆料制备纳米镁铝尖晶石的方法 (Method for preparing nano magnesia-alumina spinel from waste electrolyte slurry of aluminum-air battery ) 是由 武杏荣 杨星 潘甜甜 申星梅 曹发斌 王平 李辽沙 于 2019-10-18 设计创作，主要内容包括：本发明公开了一种以铝-空气电池产生的废电解液浆料制备纳米镁铝尖晶石的方法的方法,包括以下步骤：(1)用蒸馏水反复清洗,过滤废浆料,使清洗后的水pH＝8.3～8.5,分离,干燥,得固体物质；(2)取步骤(1)得到的固体物质放入氧化镁坩埚中,通过一步煅烧法进行煅烧,冷却至室温,得到纳米镁铝尖晶石。本发明方法制备过程简单、环保、节能,制备得到的纳米镁铝尖晶石的粒径分布均匀,实现了对铝-空气电池废电解液的资源再利用。(The invention discloses a method for preparing nano magnesia-alumina spinel by using waste electrolyte slurry generated by an aluminum-air battery, which comprises the following steps: (1) repeatedly washing with distilled water, filtering the waste slurry to ensure that the pH value of the washed water is 8.3-8.5, separating and drying to obtain a solid substance; (2) and (2) putting the solid substance obtained in the step (1) into a magnesium oxide crucible, calcining by a one-step calcining method, and cooling to room temperature to obtain the nano magnesia-alumina spinel. The method has the advantages of simple preparation process, environmental protection and energy conservation, and the prepared nano magnesia-alumina spinel has uniform particle size distribution, thereby realizing the resource reutilization of the waste electrolyte of the aluminum-air battery.)

1. A method for preparing nano magnesia-alumina spinel by using waste electrolyte slurry of an aluminum-air battery comprises the following steps:

(1) repeatedly washing the waste electrolyte slurry with distilled water, separating, filtering, and drying to obtain solid substance;

(2) and (2) putting the solid matter obtained in the step (1) into a magnesium oxide crucible, calcining by a one-step calcining method, and cooling to room temperature to obtain the nano magnesia-alumina spinel.

2. The method for preparing nano magnesium aluminate spinel from waste electrolyte slurry of aluminum-air battery as claimed in claim 1, wherein the pH of the water after washing in step (1) is 8.3-8.5.

3. The method for preparing nano magnesium aluminate spinel from waste electrolyte slurry of aluminum-air battery as claimed in claim 1, wherein the drying temperature in step (1) is 90-110 ℃ for 60-180 minutes.

4. The method for preparing nano magnesium aluminate spinel from waste electrolyte slurry of aluminum-air battery as claimed in claim 1, wherein the drying temperature in step (1) is 100 ℃ and the drying time is 120 minutes.

5. The method for preparing nano magnesium aluminate spinel from aluminum-air battery waste electrolyte slurry as claimed in claim 1, wherein the one-step calcination method comprises heating to 900-1200 ℃ and then keeping the temperature for 100-140 minutes.

6. The method for preparing nano magnesium aluminate spinel from waste electrolyte slurry of aluminum-air battery as claimed in claim 1, wherein the one-step calcination process comprises heating to 1100 ℃ and holding for 120 minutes.

Technical Field

The invention relates to the technical field of resource regeneration, in particular to a method for preparing nano magnesia-alumina spinel from waste electrolyte slurry of an aluminum-air battery.

Background

The alkaline aluminum-air battery takes metallic aluminum as an anode, air as a cathode, and the electrolyte adopts KOH or NaOH solution and the like; however, metallic aluminum produces a corrosive action in an alkaline electrolyte, and also accompanies the following hydrogen evolution reaction at the time of discharge: 2Al +6H₂O+2OH^-→2Al(OH)^4-+3H₂×) and therefore a significant portion of the aluminum reacts with the alkaline electrolyte to generate hydrogen gas, reducing the utilization of the aluminum anode while consuming electrolyte to affect the life of the cell. In order to increase the discharge performance of the aluminum-air battery, the aluminum anode is made of alloy materials, wherein an alloy element Mg is one of the most main elements influencing the electrochemical performance of the aluminum anode, when the Mg content is low, the electrochemical performance and the corrosion performance of the aluminum anode can be greatly improved, Al-0.5Mg series alloys such as Al-0.5Mg-Sn and the like are formed, and when the aluminum-air battery works, precipitates containing Al and Mg can be generated in electrolyte.

The invention patent (201510830134.0) mentions that the discharge product of an aluminum-air battery is washed to be neutral as an aluminum source, and the nano alumina with high purity and uniform particle size is prepared by adding sulfuric acid, then adding ammonium sulfate, dissolving, evaporating, calcining, adding organic dispersant (polyethylene glycol, sodium dodecyl sulfate, polyoxyethylene ether and the like) and the like, thereby realizing waste utilization. The invention patent (201510833729.1) relates to the production of nano-aluminum hydroxide by the discharge process of aluminum-air battery, and the aluminum hydroxide prepared by the method has uniform and fine particle size and high purity. And the aluminum-air battery can also output electric energy outwards in the preparation process, so that the method greatly reduces the operation cost of the aluminum-air battery and realizes waste utilization. Preparation of monodisperse nano alpha-Al from discharge product of aluminum-air battery₂O₃The optimum temperature and the amount of acid required for leaching of the discharge products, the influence of the titration rate of the reactants on the precursor and the calcination were investigated in "(" chemical industry and engineering ", 2017, 34(4): 39-43")Influence of conditions on the dispersibility of the nano-alumina. When m (concentrated sulfuric acid) is 5:2, the discharge product can be completely dissolved when the leaching temperature is 100 ℃, a pure ammonium aluminum carbonate precursor can be obtained when the titration speed of aluminum sulfate is less than 16mL/min, the precursor is heated at a low temperature of 300 ℃ and then calcined at a high temperature of 1200 ℃, and monodisperse alpha-Al with the particle size of about 50nm can be obtained₂O₃The experimental process is simple and the reproducibility is good. The above patents and documents both use the discharge product of aluminum-air battery to prepare nano aluminum oxide and nano aluminum hydroxide, and there is no report on the preparation of nano magnesium aluminate spinel from the waste electrolyte slurry generated by aluminum-air battery.

Disclosure of Invention

The invention aims to make up the defects of the prior art and provides a method for preparing nano magnesia-alumina spinel from waste electrolyte slurry of an aluminum-air battery.

In order to achieve the purpose, the invention is realized by the following scheme:

the invention provides a method for preparing nano magnesia-alumina spinel from waste electrolyte slurry of an aluminum-air battery, which comprises the following steps:

(1) repeatedly cleaning the waste electrolyte slurry with distilled water to enable the pH of the cleaned water to be 8.3-8.5, separating, filtering and drying to obtain a solid substance;

(2) and (2) putting the solid matter obtained in the step (1) into a magnesium oxide crucible, calcining by a one-step calcining method, and cooling to room temperature to obtain the nano magnesia-alumina spinel.

Preferably, in the step (1), the pH of the water after washing is 8.3 to 8.5.

Preferably, the drying temperature in the step (1) is 90-110 ℃, and the drying time is 60-180 minutes.

Preferably, the drying temperature in step (1) is 100 ℃ and the time is 120 minutes.

Preferably, the one-step calcining method is heating to 900-1200 ℃ and then preserving heat for 100-140 minutes.

Preferably, the one-step calcination process is carried out by heating to 1100 ℃ and then holding for 120 minutes.

The invention has the beneficial effects that:

the method is simple, environment-friendly and energy-saving in preparation process, and the prepared nano magnesia-alumina spinel has uniform particle size distribution, so that the resource reutilization of the waste electrolyte of the aluminum-air battery is realized.

Drawings

FIG. 1 is an X-ray diffraction pattern of nano magnesium aluminate spinel prepared in example 1;

FIG. 2 is an X-ray diffraction pattern of nano magnesium aluminate spinel prepared in example 2;

FIG. 3 is an X-ray diffraction pattern of nano magnesium aluminate spinel prepared in example 3;

FIG. 4 is an X-ray diffraction pattern of nano-magnesia-alumina spinel prepared in example 4;

FIG. 5 is a transmission electron microscope spectrum of nano-magnesia-alumina spinel prepared in example 2;

FIG. 6 is a transmission electron micrograph at 10nm of nano-magnesia alumina spinel prepared by the method of example 2;

FIG. 7 is a transmission electron micrograph at 10nm of nano-magnesia alumina spinel prepared by the method of example 2;

FIG. 8 is a transmission electron microscope spectrum at 100nm of the nano-magnesia-alumina spinel prepared in example 2.

Detailed Description

The technical solutions of the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the 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.