CN112611786B - Preparation of graphene-loaded tin dioxide quantum dot for formaldehyde and nitrogen dioxide gas detection, product and application - Google Patents
Preparation of graphene-loaded tin dioxide quantum dot for formaldehyde and nitrogen dioxide gas detection, product and application Download PDFInfo
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- CN112611786B CN112611786B CN202011381411.1A CN202011381411A CN112611786B CN 112611786 B CN112611786 B CN 112611786B CN 202011381411 A CN202011381411 A CN 202011381411A CN 112611786 B CN112611786 B CN 112611786B
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- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
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- G01N27/126—Composition of the body, e.g. the composition of its sensitive layer comprising organic polymers
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Abstract
The invention discloses a preparation method of graphene-loaded tin dioxide quantum dots for formaldehyde and nitrogen dioxide gas detection, and a product and application thereof 2 In the preparation process of the quantum dot modified graphene, tin salt and zinc salt are adopted as precursors, the precursors are mixed with graphene oxide and then subjected to hydrothermal reaction, and then the step of acid washing is adopted to remove Zn in the product, so that the surface and the interior of the metal oxide have more defect states, and the existence of the defect states can improve the adsorption of the material on target gas and preferentially carry out catalytic reaction, thereby improving the sensitivity of the material for gas detection; the metal oxide is compounded with the graphene, so that the conductivity of the graphene can be improved, and the catalytic reaction on the target gas at room temperature is realized, so that NO is realized at room temperature 2 Detection of (3).
Description
Technical Field
The invention relates to the field of gas detection, in particular to a preparation method of a gas sensitive material, and particularly relates to a preparation method of graphene-loaded tin dioxide quantum dots for detecting formaldehyde and nitrogen dioxide gas, and a product and application thereof.
Background
With the increasing environmental pollution, especiallyNO 2 Is the waste gas of automobile exhaust and coal combustion, has great harm to human health when formaldehyde is used as the waste gas of coating and paint, and has NO effect on formaldehyde and NO 2 And the detection of toxic and harmful gases is the primary task of environmental management.
The metal oxide can be used as a gas detection sensitive material because the resistance changes under the gas atmosphere with different concentrations, and has competitive advantages compared with other types of sensors because the metal oxide is cheap. However, the metal oxide has a high working temperature, which is generally above 200 ℃, and the sensitivity and selectivity are not ideal. The reaction temperature can be reduced and the sensitivity can be improved by constructing the nano material and the composite material.
The present invention utilizes SnO 2 Quantum dot modified graphene and SnO comprehensive utilization 2 The gas response and the conductivity of graphene improve the defects of the gas sensitive material in the aspects of high sensitivity and high working temperature, and the material prepared by the method can realize the reaction of NO at room temperature 2 And (3) detecting the gas, namely detecting the formaldehyde gas at the working temperature of about 180 ℃.
Disclosure of Invention
The invention aims to provide a preparation method of graphene-loaded tin dioxide quantum dots for detecting formaldehyde and nitrogen dioxide gas.
Yet another object of the present invention is to: provides a product prepared by the method.
Yet another object of the present invention is to: provides an application of the product.
The purpose of the invention is realized by the following scheme: a preparation method of graphene-loaded tin dioxide quantum dots for formaldehyde and nitrogen dioxide gas detection utilizes SnO 2 In the preparation process of the quantum dot modified graphene, a precursor adopts tin salt and zinc salt, and is mixed with graphene oxide for hydrothermal reaction, and then, the step of acid washing is adopted to remove Zn in the product, so that the surface and the inside of the metal oxide have more defect states, and the existence of the defect states can improve the adsorption of the material to target gas and preferentially catalyze the reaction, and the preparation method comprises the following steps:
the method comprises the following steps: weighing 2 to 5mmol of tin salt and 0.1 to 0.5mmol of zinc salt in 10mL of deionized water, and dissolving in the deionized water;
step two: taking 10mL of deionized water, preparing an aqueous solution of a triblock polymer with the molar concentration of 0.8-1.2M, slowly dropping the solution obtained in the step one into the aqueous solution of the triblock polymer under the stirring state, continuously stirring for 30-50min, adding 1-3mL of hydrochloric acid, and continuously stirring for 30-50min;
step three: adding 5-10mL of graphene oxide with the concentration of 1mg/mL into the solution obtained in the second step, stirring for 1-2h, carrying out hydrothermal reaction at 180-200 ℃, cooling to room temperature, centrifuging, collecting precipitate, and drying at 60-80 ℃ to obtain powder;
step four: putting the powder obtained in the step three into a nitric acid aqueous solution with the concentration of 1-2M, and carrying out hydrothermal reaction at 160-180 ℃ for 12-14h to obtain graphene-loaded SnO 2 And (4) quantum dots.
Wherein, in the step one, the tin salt is SnCl 4 ·5H 2 O，SnCl 2 ·2H 2 O，Sn(Ac) 2 At least one of (a); the zinc salt is Zn (NO) 3 ) 2 ·6H 2 O，Zn(AC) 2 ，ZnCl 2 ，ZnSO 4 At least one of (1).
In the second step, the triblock polymer is at least one of P123 or F127.
The invention also provides a graphene-loaded tin dioxide quantum dot product for detecting formaldehyde and nitrogen dioxide gas, and the graphene-loaded tin dioxide quantum dot product is prepared according to any one of the methods.
The invention also provides application of the graphene-loaded tin dioxide quantum dot in detection of formaldehyde and nitrogen dioxide gas.
The powder prepared by the invention is dispersedly coated on a six-pin ceramic tube gas-sensitive test element for respectively testing NO 2 And response to formaldehyde gas, to NO 2 The optimum corresponding temperature is room temperature for NO concentration of 1ppm 2 The corresponding sensitivity of the gas is 11.9-15.1, the optimal corresponding temperature for formaldehyde gas is 180 ℃, and the response sensitivity for formaldehyde gas with the concentration of 10ppm is 25.8-30.9.
The invention provides a simple and feasible SnO 2 The method for modifying graphene by quantum dots can realize detection of different target gases at different temperatures by the composite material prepared by the method. The method utilizes SnO 2 In the preparation process of the quantum dot modified graphene, tin salt and zinc salt are adopted as precursors, the precursors are mixed with graphene oxide and then are subjected to hydrothermal reaction, and then the step of acid washing is adopted to remove Zn in the product, so that the surface and the interior of the metal oxide have more defect states, and the existence of the defect states can improve the adsorption of the material on the target gas and preferentially carry out catalytic reaction, thereby improving the sensitivity of the material for gas detection; the metal oxide is compounded with the graphene, so that the conductivity of the graphene can be improved, and the catalytic reaction of the graphene on target gas at room temperature is realized, so that NO is realized at room temperature 2 Detection of (3).
Drawings
FIG. 1 shows that the graphene loaded SnO prepared by the invention 2 Quantum dot pair NO 2 And formaldehyde gas working schematic.
Detailed Description
Example 1:
graphene-loaded tin dioxide quantum dot for detecting formaldehyde and nitrogen dioxide gas by using SnO 2 In the preparation process of the quantum dot modified graphene, a precursor adopts tin salt and zinc salt, and is mixed with graphene oxide for hydrothermal reaction, then, the step of acid washing is adopted to remove Zn in the product, so that the surface and the interior of the metal oxide have more defect states, the existence of the defect states can improve the adsorption of the material to target gas and preferentially carry out catalytic reaction, and the preparation method comprises the following steps:
the method comprises the following steps: taking 10mL of deionized water, weighing 5mmol of tin salt SnCl 4 ·5H 2 O and 0.1mmol of Zn (NO) 3 ) 2 ·6H 2 Dissolving O in deionized water;
step two: taking 10mL of deionized water, preparing an aqueous solution of a triblock polymer P123 with the molar concentration of 1.0M, slowly dropping the solution obtained in the step one into the aqueous solution of the triblock polymer P123 under the stirring state, continuously stirring for 50min, adding 2mL of hydrochloric acid, and continuously stirring for 30min;
step three: adding 10mL of graphene oxide with the concentration of 1mg/mL into the solution obtained in the second step, stirring for 2 hours, carrying out hydrothermal reaction at 180 ℃, cooling to room temperature, centrifuging, collecting precipitate, and drying at 80 ℃ to obtain powder;
step four: putting the powder obtained in the step three into a nitric acid aqueous solution with the concentration of 1M, and carrying out hydrothermal reaction for 12h at 180 ℃ to obtain graphene-loaded SnO 2 And (4) quantum dots. Prepared graphene-loaded SnO 2 Quantum dot pair NO 2 And formaldehyde gas as shown in figure 1:
the powder prepared in the embodiment is dispersedly coated on a six-pin ceramic tube gas-sensitive testing element for respectively testing NO 2 And response of formaldehyde gas to NO 2 The optimum corresponding temperature is room temperature for NO concentration of 1ppm 2 The corresponding sensitivity of the gas is 13.5, the optimal corresponding temperature for formaldehyde gas is 180 ℃, and the response sensitivity for formaldehyde gas with the concentration of 10ppm is 25.8.
Example 2:
the graphene-supported tin dioxide quantum dot for detecting formaldehyde and nitrogen dioxide gas is similar to that in example 1 and is prepared by the following steps:
the method comprises the following steps: taking 10mL of deionized water, weighing 2mmol of tin salt SnCl 2 ·2H 2 O and 0.1mmol of Zn (NO) 3 ) 2 ·6H 2 Dissolving O in deionized water;
step two: taking 10mL of deionized water, preparing an aqueous solution of a triblock polymer P123 with the molar concentration of 0.8M, slowly dropping the solution obtained in the step one into the aqueous solution of the triblock polymer P123 under the stirring state, continuously stirring for 50min, adding 1mL of hydrochloric acid, and continuously stirring for 30min;
step three: adding 5mL of graphene oxide with the concentration of 1mg/mL into the solution obtained in the second step, stirring for 2h, carrying out hydrothermal reaction at 180 ℃, cooling to room temperature, centrifuging, collecting precipitate, and drying at 80 ℃ to obtain powder;
step four: putting the powder obtained in the step three into a nitric acid aqueous solution with the concentration of 2M, and carrying out hydrothermal reaction for 12 hours at 180 ℃ to obtain graphene-loaded SnO 2 And (4) quantum dots.
The powder prepared by the embodiment is dispersedly coated on a six-pin ceramic tube gas-sensitive test elementIn the above, test on NO separately 2 And response of formaldehyde gas to NO 2 The optimum corresponding temperature is room temperature for NO concentration of 1ppm 2 The gas response sensitivity is 11.9, the optimal response temperature for formaldehyde gas is 180 ℃, and the response sensitivity for formaldehyde gas with the concentration of 10ppm is 28.4.
Example 3:
similar to example 1, the graphene-supported tin dioxide quantum dot for detecting formaldehyde and nitrogen dioxide gas is prepared by the following steps:
the method comprises the following steps: taking 10mL of deionized water, weighing 3mmol of tin salt Sn (Ac) 2 And 0.3mmol of Zn (AC) 2 Dissolving in deionized water;
step two: taking 10mL of deionized water, preparing an aqueous solution of a triblock polymer P127 with the molar concentration of 1.2M, slowly dropping the solution obtained in the step one into the aqueous solution of the P127 under the stirring state, continuously stirring for 50min, adding 3mL of hydrochloric acid, and continuously stirring for 30min;
step three: adding 5mL of graphene oxide with the concentration of 1mg/mL into the solution obtained in the second step, stirring for 2 hours, carrying out hydrothermal reaction at 200 ℃, cooling to room temperature, centrifuging, collecting precipitate, and drying at 80 ℃ to obtain powder;
step four: putting the powder obtained in the step three into a nitric acid aqueous solution with the concentration of 2M, and carrying out hydrothermal reaction for 12h at 160 ℃ to obtain graphene-loaded SnO 2 And (4) quantum dots.
The powder prepared in the embodiment is dispersedly coated on a six-pin ceramic tube gas-sensitive test element to respectively test NO 2 And response of formaldehyde gas to NO 2 The optimum corresponding temperature is room temperature for NO concentration of 1ppm 2 The corresponding sensitivity of the gas is 15.1, the optimal corresponding temperature for formaldehyde gas is 180 ℃, and the response sensitivity for formaldehyde gas with the concentration of 10ppm is 30.9.
The embodiments described above are described to facilitate an understanding and appreciation of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the embodiments described herein, and those skilled in the art should make improvements and modifications to the present invention based on the disclosure of the present invention within the protection scope of the present invention.
Claims (4)
1. A preparation method of graphene-loaded tin dioxide quantum dots for formaldehyde and nitrogen dioxide gas detection is characterized in that SnO is utilized 2 In the preparation process of the quantum dot modified graphene, a precursor adopts tin salt and zinc salt, and is mixed with graphene oxide for hydrothermal reaction, and then, the step of acid washing is adopted to remove Zn in the product, so that the surface and the inside of the metal oxide have more defect states, and the existence of the defect states can improve the adsorption of the material to target gas and preferentially catalyze the reaction, and the preparation method comprises the following steps:
the method comprises the following steps: weighing 2 to 5mmol of tin salt and 0.1 to 0.5mmol of zinc salt in 10mL of deionized water, and dissolving in the deionized water;
step two: taking 10mL of deionized water, preparing an aqueous solution of a triblock polymer with the molar concentration of 0.8-1.2M, slowly dropping the solution obtained in the step one into the aqueous solution of the triblock polymer under the stirring state, continuously stirring for 30-50min, adding 1-3mL of hydrochloric acid, and continuously stirring for 30-50min;
step three: adding 5-10mL of graphene oxide with the concentration of 1mg/mL into the solution obtained in the second step, stirring for 1-2h, carrying out hydrothermal reaction at 180-200 ℃, cooling to room temperature, centrifuging, collecting precipitate, and drying at 60-80 ℃ to obtain powder;
step four: putting the powder obtained in the step three into a nitric acid aqueous solution with the concentration of 1-2M, and carrying out hydrothermal reaction at 160-180 ℃ for 12-14h to obtain graphene-loaded SnO 2 Quantum dots; wherein the content of the first and second substances,
in the step one, the tin salt is SnCl 4 ·5H 2 O，SnCl 2 ·2H 2 O，Sn(Ac) 2 At least one of; the zinc salt is Zn (NO) 3 ) 2 ·6H 2 O，Zn(AC) 2 ，ZnCl 2 ，ZnSO 4 At least one of (a).
2. The method for preparing the graphene-supported tin dioxide quantum dot for detecting formaldehyde and nitrogen dioxide gas as claimed in claim 1, wherein the method comprises the following steps: in the second step, the triblock polymer is at least one of P123 or F127.
3. A graphene-supported tin dioxide quantum dot for detecting formaldehyde and nitrogen dioxide gases, which is characterized by being prepared according to any one of the methods of claims 1-2.
4. The application of the graphene-supported tin dioxide quantum dot according to claim 3 in detection of formaldehyde and nitrogen dioxide gas.
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