A method for preparing an al / s catalyst

By preparing MQDs through reaction in toluene solvent at 150℃, the problems of oxidation and structural damage of Ti3C2Tx MXene material under high temperature and high pressure were solved, and stable catalyst preparation was achieved, thus improving the performance of aluminum-sulfur batteries.

CN116995240BActive Publication Date: 2026-02-17JILIN NORMAL UNIV
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Patent Information

Application Number
CN202311128678.3
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2023-09-04
Publication Date
2026-02-17
Estimated Expiration
2043-09-04

AI Technical Summary

Technical Problem

In the preparation of Ti3C2Tx MXene materials, the high temperature and high pressure conditions in the existing technology lead to the oxidation and structural damage of MQDs, which affects their catalytic performance.

Method used

MQDs were prepared by reacting them in toluene solvent at 150℃ for 3-6 hours to avoid oxidation and structural damage to the MQDs caused by high temperature and high pressure. The brown liquid was obtained by separation through a filter.

Benefits of technology

Circular MQDs with an average diameter of 5 nm were successfully prepared, exhibiting good dispersibility and stable catalytic activity. They are suitable for aluminum-sulfur batteries, suppressing the sulfur shuttle effect and improving the cycle stability and energy density of the battery.

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Abstract

The application belongs to the technical field of aluminum-sulfur batteries and provides a preparation method of an aluminum-sulfur battery catalyst, wherein the catalyst is MQDs, and the preparation method comprises the following steps: step 1, 0.2g of multilayer Ti3C2T x is loaded into a reaction kettle containing 50ml of toluene, the reaction kettle is transferred to a blast drying oven, the temperature is adjusted to 150 DEG C, and the reaction is carried out; step 2, after the reaction is completed, the reaction kettle is cooled at room temperature, and the dispersion liquid in the reaction kettle is sucked into a syringe; step 3, a filter is installed at the needle head part of the syringe to separate a brown liquid. The method uses a reducing toluene solvent as a reaction solvent to prepare MQDs, and effectively inhibits the oxidation of the MQDs and the destruction of the structure of the MQDs when the reaction is carried out at high temperature and high pressure.
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Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of aluminum-sulfur batteries, and particularly relates to a preparation method of an aluminum-sulfur battery catalyst. BACKGROUND

[0002] An aluminum-sulfur battery is a high-energy-density battery in which an aluminum anode and a sulfur cathode undergo electrochemical reactions through an electrolyte separator. Sulfur is a highly reactive non-metallic element that can release a large amount of electrical energy during electrochemical reactions. Aluminum is a common and inexpensive metal with a high potential and energy density, making it an ideal battery material. The reaction process of an aluminum-sulfur battery involves the transfer of electrons from the aluminum anode to the sulfur cathode, while simultaneously releasing aluminum ions at the aluminum end. The sulfur cathode is reduced to polysulfides under the action of electrons, releasing a large amount of heat and electrical energy in the process. The overall energy density of the battery system is very high, much higher than that of traditional lead-acid batteries and lithium-ion batteries. Aluminum-sulfur batteries have many advantages, such as high energy density, low cost, long life, fast charging, and non-toxic pollution. However, aluminum-sulfur batteries also have many challenges, such as anode corrosion during electrochemical reactions, electrolyte stability, sulfur cathode life, and charge-discharge efficiency. Therefore, the research on aluminum-sulfur batteries is still in its early stages, and further work is needed to realize its commercial application.

[0003] Shuttle effect is one of the reasons for inhibiting the performance of aluminum-sulfur batteries, as polysulfides in the sulfur cathode are prone to dissolution, diffusion, and migration during charging and discharging, leading to the reaction of sulfur in the battery being controlled only by the solid electrolyte separator of the sulfur cathode, rather than relying on electron conduction between solid electrodes. As a result, some polysulfides penetrate the separator and deposit on the aluminum anode, causing problems such as reduced battery capacity, decreased cycle life, increased internal resistance, and reduced safety. To address the sulfur shuttle effect, researchers of aluminum-sulfur batteries have adopted various methods, such as improving the electrolyte, designing new separators, and using additives. One of these methods is to introduce catalysts into the cathode. These catalysts can promote reactions on the electrode surface, prevent the formation of sulfides, and slow down the oxidation reaction rate, thereby inhibiting the occurrence of the shuttle effect. In addition, catalysts can also allow the formation of more stable reaction products and more complete electrode surface structures on the electrode surface, thereby reducing the defect density of the electrode surface, strengthening the mechanical stability and corrosion resistance of the electrode material, and further improving the cycle stability and energy density of the battery.

[0004] MXene materials are a new type of two-dimensional material that is attracting increasing attention and research due to its unique structure and chemical properties. MXene materials are composed of layered carbides of transition metals and have a two-dimensional crystal structure similar to graphene. The chemical formula of MXene is usually represented as M n+1 X n T xwhere M is a transition metal element, X is an element such as carbon (C), nitrogen (N), and silicon (Si), and T represents a functional group. MXene materials have a two-dimensional structure and are generally only a few nanometers thick, making them one of the thinnest materials known. MXene materials have very diverse chemical properties, and since their surfaces are covered with functional groups, the types and amounts of these functional groups can be controlled through chemical synthesis, allowing for optimization of material properties. They also have high electrical conductivity and excellent mechanical properties, making them suitable for use in flexible electronic devices and other fields. MQDs have excellent chemical and thermal stability, making them suitable for use in harsh conditions such as high temperatures and acidic or basic environments. In summary, MQDs have good controllability, optical properties, stability, and biocompatibility, and are expected to play an important role in the fields of biomedicine, photoelectric conversion, and energy storage. MQDs can also be used as oxidation reaction catalysts, catalyzing the oxidation of organic compounds and the oxidation of CO, among other reactions, and have good catalytic activity and stability. MQDs can be used in the electrolysis of water to produce hydrogen, and have high catalytic activity and stability. MXene materials not only can be used as catalysts, but also can be used to prepare other catalysts by taking advantage of their material properties. For example, MXene can be combined with other metals or nitrogen-doped materials to prepare composite catalysts with high catalytic activity.

[0005] In the prior art, Ti3C2T x The preparation of MXene materials often involves high temperatures, high pressures, and strong corrosive substances, which can cause excessive oxidation and structural damage to the obtained MQDs. SUMMARY

[0006] The purpose of the embodiments of the present application is to provide a preparation method of an aluminum-sulfur battery catalyst, which aims to solve the problems raised in the above background.

[0007] The embodiments of the present application are implemented as follows: a preparation method of an aluminum-sulfur battery catalyst, the catalyst being MQDs, the preparation method comprising the following steps:

[0008] Step 1: 0.2 g of multi-layer Ti3C2T x The reaction kettle is transferred to a forced air drying oven, and the temperature is adjusted to 150℃ for reaction.

[0009] Step 2: After the reaction is completed, the reaction kettle is cooled to room temperature, and the dispersion liquid in the reaction kettle is sucked into a syringe.

[0010] Step 3: A filter is installed at the needle part of the syringe to separate and obtain a brown liquid.

[0011] In a further technical solution, the reaction time of step 1 is set to 3h.

[0012] Further technical solutions, the reaction time of step 1 is set to 4h.

[0013] Further technical solutions, the reaction time of step 1 is set to 5h.

[0014] Further technical solutions, the reaction time of step 1 is set to 6h.

[0015] Further technical solutions, in the step 3, the pore size of the filter is 22μm.

[0016] The embodiment of the application provides a preparation method of an aluminum-sulfur battery catalyst, which uses a reducing toluene solvent as a reaction solvent to prepare MQDs, and effectively inhibits oxidation of the MQDs and damage to the structure of the MQDs when the reaction is carried out at high temperature and high pressure. BRIEF DESCRIPTION OF DRAWINGS

[0017] Figure 1 TEM image of the MQDs prepared after 3h of reaction;

[0018] Figure 2 Absorption spectrum of the MQDs prepared after 3h of reaction;

[0019] Figure 3 Absorption spectrum of the MQDs prepared after 4h of reaction;

[0020] Figure 4 Absorption spectrum of the MQDs prepared after 5h of reaction;

[0021] Figure 5 TEM image of the MQDs prepared after 6h of reaction;

[0022] Figure 6 Absorption spectrum of the MQDs prepared after 6h of reaction. DETAILED DESCRIPTION

[0023] In order to make the purpose, technical solutions and advantages of the application more clear, the application is further described in detail below in combination with the drawings and examples. It should be understood that the specific examples described herein are only used to explain the application, and are not used to limit the application.

[0024] The specific implementation of the application is described in detail below in combination with specific examples.

[0025] An embodiment of the application provides a preparation method of an aluminum-sulfur battery catalyst, the catalyst is MQDs, and the preparation method comprises the following steps:

[0026] Step 1, 0.2g multi-layer Ti3C2T xThe reaction kettle containing 50 ml of toluene is transferred to a blast drying oven, the temperature is adjusted to 150°C, and the reaction is carried out, and the reaction time is set to 3 h;

[0027] Step 2: After the reaction is completed, the reaction kettle is cooled at room temperature, and the dispersion liquid in the reaction kettle is sucked into a syringe;

[0028] Step 3: A filter (pore size 22 μm) is installed at the needle part of the syringe to separate and obtain a brown liquid.

[0029] In an embodiment of the present application, the transmission electron microscope (TEM) photo of the prepared MQDs is as shown in Figure 1 The photo shows that the morphology of the MQDs is circular and has good dispersibility, and the average diameter is 5 nm after measurement, proving that the MQDs are successfully prepared. The absorption spectrum is as shown in Figure 2 It is found from the spectrum that strong absorption occurs at 200 nm in the ultraviolet region and extends to the visible region.

[0030] Another embodiment of the present application provides a preparation method of an aluminum-sulfur battery catalyst, wherein the catalyst is MQDs, and the preparation method comprises the following steps:

[0031] Step 1: 0.2 g of multi-layer Ti3C2T x The reaction kettle containing 50 ml of toluene is transferred to a blast drying oven, the temperature is adjusted to 150°C, and the reaction time is set to 4 h;

[0032] Step 2: After the reaction is completed, the reaction kettle is cooled at room temperature, and the dispersion liquid in the reaction kettle is sucked into a syringe;

[0033] Step 3: A filter (pore size 22 μm) is installed at the needle part of the syringe to separate and obtain a brown liquid.

[0034] In an embodiment of the present application, the absorption spectrum is as shown in Figure 3 It is found from the spectrum that strong absorption occurs at 200 nm in the ultraviolet region and extends to the visible region.

[0035] Another embodiment of the present application provides a preparation method of an aluminum-sulfur battery catalyst, wherein the catalyst is MQDs, and the preparation method comprises the following steps:

[0036] Step 1: 0.2 g of multi-layer Ti3C2T x The reaction kettle containing 50 ml of toluene is transferred to a blast drying oven, the temperature is adjusted to 150°C, and the reaction time is set to 5 h;

[0037] Step 2: After the reaction is completed, the reaction kettle is cooled at room temperature, and the dispersion liquid in the reaction kettle is sucked into a syringe;

[0038] Step 3, install a filter (pore size 22 μm) at the needle part of the syringe to separate and obtain a brown liquid.

[0039] In the embodiment of the present application, the transmission electron microscope (TEM) photo of the prepared MQDs is as shown in Figure 4 The strong absorption in the ultraviolet region at 200 nm and extending to the visible region is found from the spectrum.

[0040] Another embodiment of the present application provides a preparation method of an aluminum-sulfur battery catalyst, the catalyst being MQDs, and the preparation method comprising the following steps:

[0041] Step 1, 0.2 g of multi-layer Ti3C2T x is loaded into a reaction kettle containing 50 ml of toluene, the reaction kettle is transferred to a blast drying oven, the temperature is adjusted to 150°C, and the reaction time is set to 6 h;

[0042] Step 2, after the reaction is completed, the reaction kettle is cooled at room temperature, and the dispersion liquid in the reaction kettle is sucked into a syringe;

[0043] Step 3, install a filter (pore size 22 μm) at the needle part of the syringe to separate and obtain a brown liquid.

[0044] In the embodiment of the present application, the transmission electron microscope (TEM) photo of the prepared MQDs is as shown in Figure 5 The photo shows that the morphology of the MQDs is circular and has good dispersibility, and the average diameter is 5 nm after measurement, proving that the MQDs are successfully prepared. The absorption spectrum is as shown in Figure 6 The strong absorption in the ultraviolet region at 200 nm and extending to the visible region is found from the spectrum.

[0045] The above merely describes the preferred embodiments of the present application and is not used to limit the present application, and any modification, equivalent replacement and improvement made within the spirit and principle of the present application shall be included in the protection scope of the present application.

Claims

1. A method of preparing an aluminum-sulfur battery catalyst, characterized by, The catalyst is MQDs, and the preparation method comprises the following steps: Step 1, 0.2 g of multi-layer Ti3C2T x was loaded into a reaction kettle containing 50 ml of toluene, the reaction kettle was transferred to a blast drying oven, the temperature was adjusted to 150°C, and the reaction was carried out; Step 2, after the reaction is completed, the dispersion liquid in the reaction kettle is sucked into a syringe at room temperature; Step 3, a filter is installed at the needle part of the syringe to separate a brown liquid.

2. The method of claim 1, wherein the aluminum-sulfur battery catalyst is prepared by the steps of: The reaction time of step 1 is set to 3h.

3. The method of claim 1, wherein the aluminum-sulfur battery catalyst is prepared by the steps of: The reaction time of step 1 is set to 4h.

4. The method of claim 1, wherein the aluminum-sulfur battery catalyst is prepared by the steps of: The reaction time of step 1 is set to 5h.

5. The method of claim 1, wherein the aluminum-sulfur battery catalyst is prepared by the steps of: The reaction time of step 1 is set to 6h.

6. The method of claim 1, wherein the aluminum-sulfur battery catalyst is prepared by the steps of: In step 3, the pore size of the filter is 22μm.