Method for synthesizing NANO zinc sulfide / bamboo charcoal photocatalytic material

By using a mixed solvent of methanol and water and a surfactant of nano zinc sulfide/bamboo charcoal photocatalytic materials to process bamboo charcoal particles to form nano zinc sulfide/bamboo charcoal composite materials, the problems of poor stability and high cost in the existing technology are solved, and efficient and environmentally friendly photocatalytic performance improvement is achieved.

WO2025179617A1PCT designated stage Publication Date: 2025-09-04ANHUI SCI & TECH UNIV
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Patent Information

Application Number
PCT/CN2024/080239
Authority / Receiving Office
WO · WO
Patent Type
Applications
Current Assignee / Owner
Priority Date
2024-03-01
Filing Date
2024-03-06
Publication Date
2025-09-04

AI Technical Summary

Technical Problem

In the existing nano zinc sulfide/bamboo charcoal photocatalytic material synthesis methods, nano zinc sulfide cannot be fully dissolved, resulting in poor stability, insufficient dispersion of bamboo charcoal, low photocatalytic activity and reaction rate, and use expensive and toxic solvents, which are costly and have a great impact on the environment.

Method used

Use a mixed solvent of methanol and water to dissolve the zinc sulfide powder, and add surfactant to promote dispersion. Use ethanol and water to treat bamboo charcoal particles, and form nano zinc sulfide/bamboo charcoal composites through heat treatment, avoid the use of expensive and toxic solvents, and control the parameters of each step such as temperature, time and gas protection.

Benefits of technology

The stability and photocatalytic properties of nano zinc sulfide/bamboo charcoal photocatalytic materials are improved, the synthesis cost is reduced, the impact on the environment is reduced, and the specific surface area and reaction rate of the material are enhanced.

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Abstract

Disclosed in the present invention is a method for synthesizing a nano zinc sulfide / bamboo charcoal photocatalytic material. The method comprises the synthesis of a precursor solution, a treatment of bamboo charcoal, the mixing of the bamboo charcoal and the precursor solution, a heat treatment, and washing and drying. An appropriate dissolving environment is provided by mixing methanol and water as a mixed solvent, such that a zinc sulfide powder can be fully dispersed and dissolved, which is beneficial to the subsequent synthesis process. The mixed solvent of methanol and water can endow the surface of the bamboo charcoal with certain hydrophilicity, thereby interacting with zinc sulfide in the solution, facilitating the compounding of the nano zinc sulfide and the bamboo charcoal, and improving the photocatalytic performance. In addition, methanol and water are both common and environmentally friendly solvents, are non-toxic and harmless, have little influence on the environment, and complex synthesis conditions or expensive reagents do not need to be used during the synthesis process, thereby reducing the synthesis cost of the nano zinc sulfide / bamboo charcoal photocatalytic material.
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Description

A method for synthesizing nano zinc sulfide / bamboo charcoal photocatalytic material Technical Field

[0001] The invention relates to the synthesis of a nano zinc sulfide / bamboo charcoal photocatalytic material, in particular to a method for synthesizing the nano zinc sulfide / bamboo charcoal photocatalytic material. Background Art

[0002] Nano-zinc sulfide / bamboo charcoal photocatalytic materials have a wide range of applications in the field of photocatalysis. They have high photocatalytic activity and stability and can be used in environmental cleaning technologies such as photocatalytic decomposition of organic pollutants and photocatalytic water decomposition to produce hydrogen. The synthesis of nano-zinc sulfide / bamboo charcoal photocatalytic materials usually adopts solvent thermal method or hydrothermal method. First, nano-zinc sulfide and bamboo charcoal are synthesized separately to obtain nano-zinc sulfide solution and bamboo charcoal solution. Then, the two solutions are mixed and heat-treated under high temperature and high pressure conditions to make the nano-zinc sulfide and bamboo charcoal uniformly dispersed and form a composite material.

[0003] However, the current methods for synthesizing nano-zinc sulfide / bamboo charcoal photocatalytic materials have the following disadvantages: in the existing methods for synthesizing nano-zinc sulfide / bamboo charcoal photocatalytic materials, nano-zinc sulfide cannot be fully dissolved in the solvent, resulting in an uneven precursor solution, which leads to poor stability of the final synthesized nano-zinc sulfide / bamboo charcoal photocatalytic material; in the existing methods for synthesizing nano-zinc sulfide / bamboo charcoal photocatalytic materials, bamboo charcoal is not dispersed, resulting in insufficient contact between nano-zinc sulfide and bamboo charcoal, which in turn leads to low photocatalytic activity and reaction rate of the synthesized nano-zinc sulfide / bamboo charcoal photocatalytic material; the solvents used in the existing methods for synthesizing nano-zinc sulfide / bamboo charcoal photocatalytic materials are expensive, resulting in a high cost for synthesizing nano-zinc sulfide / bamboo charcoal photocatalytic materials using the synthesis method; in addition, the solvents used are toxic to a certain extent and have a significant impact on the environment. Summary of the Invention

[0004] The purpose of the present invention is to solve the problems in the existing method for synthesizing nano zinc sulfide / bamboo charcoal photocatalytic materials, that nano zinc sulfide cannot be fully dissolved in the solvent, making the precursor solution uneven, resulting in poor stability of the finally synthesized nano zinc sulfide / bamboo charcoal photocatalytic material; in the existing method for synthesizing nano zinc sulfide / bamboo charcoal photocatalytic materials, bamboo charcoal is not dispersed, resulting in insufficient contact between nano zinc sulfide and bamboo charcoal, which in turn leads to low photocatalytic activity and reaction rate of the synthesized nano zinc sulfide / bamboo charcoal photocatalytic material; the solvent used in the existing method for synthesizing nano zinc sulfide / bamboo charcoal photocatalytic material is expensive, resulting in high cost of synthesizing nano zinc sulfide / bamboo charcoal photocatalytic material by the synthesis method; in addition, the solvent used has certain toxicity and has a great impact on the environment, and thus a method for synthesizing nano zinc sulfide / bamboo charcoal photocatalytic material is proposed.

[0005] The purpose of the present invention can be achieved by the following technical solution: a method for synthesizing a nano zinc sulfide / bamboo charcoal photocatalytic material, the method comprising the following steps:

[0006] Step 1: Synthesis of precursor solution: Methanol and water are mixed to obtain a mixed solvent, zinc sulfide powder is added to the mixed solvent, and a surfactant is added for stirring to dissolve the zinc sulfide powder in the mixed solvent to synthesize a precursor solution. The mixed solvent of methanol and water provides an appropriate dissolution environment so that the zinc sulfide powder can be fully dispersed and dissolved, which is beneficial to the subsequent synthesis process. The addition of the surfactant can reduce the surface energy during the dissolution process, promote the dispersion and dissolution of the zinc sulfide powder, and be beneficial to the formation of a uniform precursor solution and improve the stability and photocatalytic performance of the nano zinc sulfide / bamboo charcoal photocatalytic material. The mixed solvent of methanol and water can make the bamboo charcoal surface have a certain hydrophilicity, thereby interacting with the zinc sulfide in the solution, which is beneficial to the composite of nano zinc sulfide and bamboo charcoal and improving the photocatalytic performance. In addition, methanol and water are common and environmentally friendly solvents, non-toxic and harmless, with little impact on the environment. No complex synthesis conditions or expensive reagents are required during the synthesis process, thereby reducing the synthesis cost of the nano zinc sulfide / bamboo charcoal photocatalytic material.

[0007] Step 2: Bamboo charcoal treatment: soak the bamboo charcoal particles in a mixed solvent of ethanol and water, heat and stir, and disperse the bamboo charcoal particles in the mixed solvent, which can achieve effective dispersion of the bamboo charcoal particles, thereby obtaining uniformly dispersed bamboo charcoal particles. After treatment, the bamboo charcoal particles can be better dispersed, making the interface between nano-zinc sulfide and bamboo charcoal more sufficient, which can increase the specific surface area of ​​the nano-zinc sulfide / bamboo charcoal photocatalytic material and improve the photocatalytic activity and reaction rate of the material. In addition, after the bamboo charcoal particles are treated, some oxygen-containing functional groups will appear on the surface. These functional groups can interact with the sulfur functional groups on the surface of the nano-zinc sulfide particles, thereby enhancing the binding force between the nano-zinc sulfide particles and the bamboo charcoal particles, which helps to improve the stability and photocatalytic activity of the nano-zinc sulfide / bamboo charcoal photocatalytic material.

[0008] Step 3: Mixing bamboo charcoal with precursor solution: Mix the treated bamboo charcoal with the precursor solution and stir evenly;

[0009] Step 4: Heat treatment: heat treating the mixture to form a nano zinc sulfide / bamboo charcoal composite material;

[0010] Step 5: washing and drying: the composite material after heat treatment is naturally cooled to room temperature, filtered, washed to neutrality, and dried to obtain the nano zinc sulfide / bamboo charcoal photocatalytic material.

[0011] A further technical improvement of the present invention is that in step 1, the mass ratio of the mixture of methanol and water is controlled at 1:1-10, and the mass ratio of the zinc sulfide powder to the mixed solvent is controlled at 1.5-2.8:20-200.

[0012] The present invention further improves the technology by selecting sodium lauryl sulfate as the surfactant in step 1. Sodium lauryl sulfate has good dispersibility and stability, can effectively help zinc sulfide powder to be evenly dispersed in the mixed solvent and prevent powder aggregation. Sodium lauryl sulfate has good surface activity, can reduce surface energy, improve the dispersibility and stability of the nanomaterial, and facilitate subsequent material synthesis and performance control. The mass ratio of sodium lauryl sulfate to zinc sulfide is controlled at 2-5:1.

[0013] A further technical improvement of the present invention is that in step 2, the mass ratio of ethanol to water is controlled within 1:1-5, and the mass ratio of the mixed solution of ethanol and water to bamboo charcoal is controlled within 20-30:1.

[0014] A further technical improvement of the present invention is that the heating temperature in step 2 is controlled at 65-85° C., and the stirring time is controlled at 1-2.5 h.

[0015] A further technical improvement of the present invention is that: in step 3, the mixture is stirred 3-5 times, with each stirring time controlled at 0.2-0.5 h, and ultrasonic treatment is applied during the stirring process to improve the mixing and dispersion effects.

[0016] A further technical improvement of the present invention is that the specific steps of the heat treatment in step 4 are: transferring the mixture to a flask for heating, and flushing inert gas into the flask. By flushing inert gas, the oxidation reaction can be prevented from occurring, thereby avoiding damage or change in the quality of the material and improving the purity of the synthesized nano-zinc sulfide / bamboo charcoal photocatalytic material.

[0017] Further technical improvements of the present invention are: the heat treatment heating temperature is controlled at 400-600°C. Too low a temperature may cause incomplete combination of zinc sulfide and bamboo charcoal, thereby affecting the photocatalytic performance. Too high a temperature may cause sintering and pyrolysis of bamboo charcoal. The heating time is controlled at 2-6 hours, and nitrogen is selected as the inert gas.

[0018] A further technical improvement of the present invention is that the drying temperature in step 5 is controlled at 145-175° C. and the drying time is controlled at 12-16 hours.

[0019] Compared with the prior art, the present invention has the following beneficial effects:

[0020] In the present invention, methanol and water are mixed as a mixed solvent. The mixed solvent of methanol and water provides a suitable dissolving environment, so that zinc sulfide powder can be fully dispersed and dissolved, which is beneficial to the subsequent synthesis process. The mixed solvent of methanol and water can make the surface of bamboo charcoal have a certain hydrophilicity, thereby interacting with zinc sulfide in the solution, which is beneficial to the composite of nano zinc sulfide and bamboo charcoal and improves the photocatalytic performance. In addition, methanol and water are both common and environmentally friendly solvents, are non-toxic and harmless, and have little impact on the environment. Complex synthesis conditions or expensive reagents do not need to be used in the synthesis process, thereby reducing the synthesis cost of the nano zinc sulfide / bamboo charcoal photocatalytic material.

[0021] In the present invention, a surfactant is added when dissolving zinc sulfide powder. The addition of the surfactant can reduce the surface energy during the dissolution process, promote the dispersion and dissolution of the zinc sulfide powder, facilitate the formation of a uniform precursor solution, and improve the stability and photocatalytic performance of the nano zinc sulfide / bamboo charcoal photocatalytic material.

[0022] In the present invention, bamboo charcoal particles are treated with a mixed solvent of ethanol and water so that the bamboo charcoal particles are dispersed in the mixed solvent, thereby achieving effective dispersion of the bamboo charcoal particles and obtaining uniformly dispersed bamboo charcoal particles. The bamboo charcoal particles can be better dispersed after treatment, so that the interface between nano-zinc sulfide and bamboo charcoal is more complete, thereby increasing the specific surface area of ​​the nano-zinc sulfide / bamboo charcoal photocatalytic material and improving the photocatalytic activity and reaction rate of the material. In addition, after the bamboo charcoal particles are treated, some oxygen-containing functional groups appear on the surface, and these functional groups can interact with the sulfur functional groups on the surface of the nano-zinc sulfide particles, thereby enhancing the binding force between the nano-zinc sulfide particles and the bamboo charcoal particles, which helps to improve the stability and photocatalytic activity of the nano-zinc sulfide / bamboo charcoal photocatalytic material. DETAILED DESCRIPTION

[0023] The technical solutions of the present invention will be clearly and completely described below in conjunction with the embodiments. Obviously, the embodiments described are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the present invention. Example 1

[0024] A method for synthesizing a nano zinc sulfide / bamboo charcoal photocatalytic material, comprising the following steps:

[0025] Step 1: Synthesis of precursor solution: Methanol and water are mixed in a mass ratio of 1:5 to obtain a mixed solvent, 0.003g of zinc sulfide powder is weighed, and the zinc sulfide powder is added to the mixed solvent. The mass ratio of zinc sulfide powder to the mixed solvent is 2:25, and sodium lauryl sulfate is added for stirring. The mass ratio of sodium lauryl sulfate to zinc sulfide powder is controlled at 2.5:1, so that the zinc sulfide powder is dissolved in the mixed solvent to synthesize a precursor solution. The mixed solvent of methanol and water provides an appropriate dissolution environment so that the zinc sulfide powder can be fully dispersed and dissolved, which is beneficial to the subsequent synthesis process. The addition of surfactants can reduce The low surface energy during the dissolution process promotes the dispersion and dissolution of zinc sulfide powder, is conducive to the formation of a uniform precursor solution, and improves the stability and photocatalytic performance of the nano-zinc sulfide / bamboo charcoal photocatalytic material. The mixed solvent of methanol and water can make the bamboo charcoal surface have a certain hydrophilicity, thereby interacting with the zinc sulfide in the solution, which is conducive to the composite of nano-zinc sulfide and bamboo charcoal and improves the photocatalytic performance. In addition, methanol and water are common and environmentally friendly solvents, non-toxic and harmless, with little impact on the environment. No complex synthesis conditions or expensive reagents are required during the synthesis process, thereby reducing the synthesis cost of the nano-zinc sulfide / bamboo charcoal photocatalytic material.

[0026] Step 2: Bamboo charcoal treatment: soak the bamboo charcoal particles in a mixed solvent of ethanol and water, wherein the mass ratio of ethanol to water in the mixed solvent is 1:3, and the mass ratio of the mixed solution of ethanol and water to the bamboo charcoal is 24:1. Heat and stir, the heating temperature is 70°C, and the stirring time is controlled at 2h, so that the bamboo charcoal particles are dispersed in the mixed solvent, which can achieve effective dispersion of the bamboo charcoal particles, thereby obtaining uniformly dispersed bamboo charcoal particles. After treatment, the bamboo charcoal particles can be better dispersed, making the interface between nano-zinc sulfide and bamboo charcoal more sufficient, which can increase the specific surface area of ​​the nano-zinc sulfide / bamboo charcoal photocatalytic material and improve the photocatalytic activity and reaction rate of the material. In addition, after the bamboo charcoal particles are treated, some oxygen-containing functional groups will appear on the surface. These functional groups can interact with the sulfur functional groups on the surface of the nano-zinc sulfide particles, thereby enhancing the binding force between the nano-zinc sulfide particles and the bamboo charcoal particles, which helps to improve the stability and photocatalytic activity of the nano-zinc sulfide / bamboo charcoal photocatalytic material.

[0027] Step 3: Mixing bamboo charcoal with precursor solution: Mix the treated bamboo charcoal with the precursor solution, stir evenly, and stir for 3 times, with each stirring time controlled at 0.4 h. Apply ultrasonic treatment during the stirring process;

[0028] Step 4: Heat treatment: The mixture synthesized in step 3 is transferred to a flask and heated at a temperature of 480° C. for 4 hours, and nitrogen is flushed into the flask to form a nano-zinc sulfide / bamboo charcoal composite material;

[0029] Step 5: washing and drying: the composite material after heat treatment is naturally cooled to room temperature, filtered, washed to neutrality, and dried at a drying temperature of 150° C. for 15 hours to obtain the nano zinc sulfide / bamboo charcoal photocatalytic material. Example 2

[0030] A method for synthesizing a nano zinc sulfide / bamboo charcoal photocatalytic material, comprising the following steps:

[0031] Step 1: Synthesis of precursor solution: Methanol and water are mixed in a mass ratio of 1:8 to obtain a mixed solvent, 0.004g of zinc sulfide powder is weighed, and the zinc sulfide powder is added to the mixed solvent. The mass ratio of zinc sulfide powder to the mixed solvent is 2.5:80, and sodium lauryl sulfate is added for stirring. The mass ratio of sodium lauryl sulfate to zinc sulfide powder is controlled at 2:1, so that the zinc sulfide powder is dissolved in the mixed solvent to synthesize a precursor solution. The mixed solvent of methanol and water provides an appropriate dissolution environment so that the zinc sulfide powder can be fully dispersed and dissolved, which is beneficial to the subsequent synthesis process. The addition of surfactants can reduce The low surface energy during the dissolution process promotes the dispersion and dissolution of zinc sulfide powder, is conducive to the formation of a uniform precursor solution, and improves the stability and photocatalytic performance of the nano-zinc sulfide / bamboo charcoal photocatalytic material. The mixed solvent of methanol and water can make the bamboo charcoal surface have a certain hydrophilicity, thereby interacting with the zinc sulfide in the solution, which is conducive to the composite of nano-zinc sulfide and bamboo charcoal and improves the photocatalytic performance. In addition, methanol and water are common and environmentally friendly solvents, non-toxic and harmless, with little impact on the environment. No complex synthesis conditions or expensive reagents are required during the synthesis process, thereby reducing the synthesis cost of the nano-zinc sulfide / bamboo charcoal photocatalytic material.

[0032] Step 2: Bamboo charcoal treatment: soak the bamboo charcoal particles in a mixed solvent of ethanol and water, wherein the mass ratio of ethanol to water in the mixed solvent is 1:4, and the mass ratio of the mixed solution of ethanol and water to bamboo charcoal is 25:1. Heat and stir, the heating temperature is 80°C, and the stirring time is controlled at 2.4h, so that the bamboo charcoal particles are dispersed in the mixed solvent, which can achieve effective dispersion of the bamboo charcoal particles, thereby obtaining uniformly dispersed bamboo charcoal particles. After treatment, the bamboo charcoal particles can be better dispersed, making the interface between nano-zinc sulfide and bamboo charcoal more sufficient, thereby increasing the specific surface area of ​​the nano-zinc sulfide / bamboo charcoal photocatalytic material and improving the photocatalytic activity and reaction rate of the material. In addition, after the bamboo charcoal particles are treated, some oxygen-containing functional groups will appear on the surface, which can interact with the sulfur functional groups on the surface of the nano-zinc sulfide particles, thereby enhancing the binding force between the nano-zinc sulfide particles and the bamboo charcoal particles, which helps to improve the stability and photocatalytic activity of the nano-zinc sulfide / bamboo charcoal photocatalytic material.

[0033] Step 3: Mixing bamboo charcoal with precursor solution: Mix the treated bamboo charcoal with the precursor solution, stir evenly, and stir for 4 times, with each stirring time controlled at 0.3 h. Apply ultrasonic treatment during the stirring process;

[0034] Step 4: Heat treatment: The mixture synthesized in step 3 was transferred to a flask and heated at a temperature of 550° C. for 5 h, and nitrogen was flushed into the flask to form a nano-zinc sulfide / bamboo charcoal composite material;

[0035] Step 5: washing and drying: the composite material after heat treatment is naturally cooled to room temperature, filtered, washed to neutrality, and dried at a drying temperature of 165° C. for 14 h to obtain the nano zinc sulfide / bamboo charcoal photocatalytic material.

[0036] The preferred embodiments of the present invention disclosed above are intended only to help illustrate the present invention. These preferred embodiments do not exhaustively describe all details, nor do they limit the present invention to specific embodiments. Obviously, many modifications and variations are possible based on the contents of this specification. These embodiments are selected and described in detail in this specification to better explain the principles and practical applications of the present invention, thereby enabling those skilled in the art to better understand and utilize the present invention. The present invention is limited only by the claims and their full scope and equivalents.

Claims

1. A method for synthesizing nano zinc sulfide / bamboo charcoal photocatalytic material, characterized by: The synthesis method comprises the following steps: Step 1: Precursor solution synthesis: Methanol and water are mixed to obtain a mixed solvent, zinc sulfide powder is added to the mixed solvent, and a surfactant is added and stirred to dissolve the zinc sulfide powder in the mixed solvent to synthesize a precursor solution; Step 2: Bamboo charcoal treatment: soak the bamboo charcoal particles in a mixed solvent of ethanol and water, heat and stir to disperse the bamboo charcoal particles in the mixed solvent; Step 3: Mixing bamboo charcoal with precursor solution: Mix the treated bamboo charcoal with the precursor solution and stir evenly; Step 4: Heat treatment: heat treating the mixture to form a nano zinc sulfide / bamboo charcoal composite material; Step 5: washing and drying: the composite material after heat treatment is naturally cooled to room temperature, filtered, washed to neutrality, and dried to obtain the nano zinc sulfide / bamboo charcoal photocatalytic material.

2. The method for synthesizing a nano zinc sulfide / bamboo charcoal photocatalytic material according to claim 1, wherein: In step 1, the mass ratio of methanol to water is controlled at 1:1-10, and the mass ratio of zinc sulfide powder to mixed solvent is controlled at 1.5-2.8:20-200.

3. The method for synthesizing a nano zinc sulfide / bamboo charcoal photocatalytic material according to claim 1, wherein: In step 1, the surfactant is sodium lauryl sulfate, and the mass ratio of sodium lauryl sulfate to zinc sulfide is controlled at 2-5:

1.

4. The method for synthesizing a nano zinc sulfide / bamboo charcoal photocatalytic material according to claim 1, wherein: In step 2, the mass ratio of ethanol to water is controlled at 1:1-5, and the mass ratio of the mixed solution of ethanol and water to bamboo charcoal is controlled at 20-30:

1.

5. The method for synthesizing a nano zinc sulfide / bamboo charcoal photocatalytic material according to claim 1, wherein: In step 2, the heating temperature is controlled at 65-85° C., and the stirring time is controlled at 1-2.5 h.

6. The method for synthesizing a nano zinc sulfide / bamboo charcoal photocatalytic material according to claim 1, wherein: In step 3, the mixture is stirred for 3-5 times, with each stirring time controlled at 0.2-0.5 h. Ultrasonic treatment is applied during the stirring process to improve the mixing and dispersion effects.

7. The method for synthesizing a nano zinc sulfide / bamboo charcoal photocatalytic material according to claim 1, wherein: The specific steps of the heat treatment in step 4 are: transferring the mixture into a flask and heating it, and flushing the flask with inert gas.

8. The method for synthesizing the nano zinc sulfide / bamboo charcoal photocatalytic material according to claim 7, characterized in that: The heat treatment heating temperature is controlled at 400-600°C, the heating time is controlled at 2-6h, and nitrogen is selected as the inert gas.

9. The method for synthesizing the nano zinc sulfide / bamboo charcoal photocatalytic material according to claim 1, characterized in that: In step 5, the drying temperature is controlled at 145-175°C, and the drying time is controlled at 12-16 hours.

Citation Information

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