CN111289581B - Sensing material for formaldehyde detection and preparation method and application thereof - Google Patents
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Abstract
The invention discloses a formaldehyde detection sensing material and a preparation method and application thereof, wherein the preparation method comprises the following steps: dissolving a zinc source and/or a tin source in an organic solvent to prepare a metal source solution; adding graphene oxide into a metal source solution, adjusting the pH of the solution to be alkaline, and stirring for reaction to obtain a first mixed solution; adding 5-amino-1-naphthalene-sulfonic acid and a reducing agent into the first mixed solution, and heating for reaction to obtain a second mixed solution; and then carrying out impurity removal treatment on the second mixed solution. The raw materials adopted by the preparation method are simple and easy to obtain, the cost is low, the prepared material can be used for rapid detection of formaldehyde, the detection sensitivity is high, and the response speed is high.
Description
Technical Field
The invention relates to the technical field of gas-sensitive materials, in particular to a sensing material for formaldehyde detection, a preparation method and application thereof.
Background
With the progress and development of society, the living standard of people in China is increasingly improved, and living conditions are also greatly improved. At the same time, however, the problem of environmental pollution is becoming increasingly severe, with atmospheric pollution being particularly a concern. The indoor air pollution of China cities is most serious and common in decoration, the indoor decoration becomes an indispensable procedure before residents in each city migrate into new houses, and formaldehyde is the primary decoration chemical indoor air pollutant in China. The novel furniture is manufactured, the wall surface and the ground are decorated and paved by using an adhesive, and the most main pollutant in the adhesive is formaldehyde; in addition, certain chemical fiber carpets, paint coatings also contain a certain amount of formaldehyde. Formaldehyde can cause harm to human health, has strong stimulation to human mucous membrane and skin,continuous headache, weakness, insomnia and the like can occur during inhalation, and long-term exposure can cause dermatitis, abnormal lung function, abnormal liver function, abnormal immune function, affected central nervous system, and can damage genetic materials in cells, thereby causing serious irritation and edema of respiratory tract, increase of respiratory tract resistance, reduction of respiratory frequency, eye irritation, headache and the like. The formaldehyde concentration in each cubic meter of air reaches 0.06-0.07mg/m 3 When children experience mild asthma; when the indoor air reaches 0.1mg/m 3 When the health care food is used, peculiar smell and uncomfortable feeling are generated; up to 0.5mg/m 3 When the eye is stimulated, lacrimation is caused; up to 0.6mg/m 3 Can cause discomfort or pain in the throat. At higher concentrations, nausea, vomiting, cough, chest distress, asthma and even pulmonary edema can be caused; when reaching 30mg/m 3 At this time, the person would immediately die. The international cancer research institutes confirmed that formaldehyde had been "carcinogenic" as an "suspected carcinogen" from the previous "suspected carcinogen," 31 st 2005, a report of carcinogens issued by the U.S. public health agency, which lists formaldehyde as a class of carcinogens. The formaldehyde release is a continuous and slow process, can be continuously released from the finishing material to pollute the indoor air in a long time after finishing, and the release amount changes along with the change of seasons and air temperature, so that the indoor air quality is influenced for a long time. Therefore, the prepared gas sensor has high sensitivity to formaldehyde gas, is convenient to carry and has high detection speed, and becomes a hot spot for scientists to study.
The existing formaldehyde detection methods are numerous, and spectrophotometry, chromatography, electrochemical analysis, instrument monitoring and the like are common. The foreign instruments for detecting formaldehyde indoors are mainly distributed in developed countries such as europe and america and japan. For example, us INTERSCAN developed an apparatus for real-time formaldehyde detection of model INTERSCAN 4160 with a resolution of 0.01ppm and a detection range of 0 to 20ppm; XP-308B formaldehyde detector developed by Nippon COSMOS company, the resolution is 0.01ppm, and the detection range is 0.01-3 ppm; the resolution of PPM-HTV formaldehyde detector developed by the United kingdom PPM company is 0.01PPM, and the detection range is 0.01-10 PPM. The formaldehyde detection instruments developed by the companies are in the leading position in terms of resolution, detection range and the like, but the price of the detectors is very high, and the universal use target cannot be achieved. Meanwhile, the development of domestic formaldehyde detectors is still in an initial stage and is mainly divided into a spectrophotometer, a colorimeter, an electrochemical analyzer and the like, wherein the development of a semiconductor metal oxide formaldehyde gas sensor in the electrochemical analyzer is mainly adopted, and since the sixty twenties, the metal oxide semiconductor gas sensor is favored by scientists because of small volume and high sensitivity.
However, the traditional formaldehyde gas sensor has the problems of poor recovery, high detection limit, high working temperature, complex manufacturing process, high energy consumption and the like, and the practical purposes of convenience, rapidness and flexibility in use cannot be achieved far away, so that how to realize high-sensitivity detection of formaldehyde at room temperature is searched to become important content in the field of semiconductor formaldehyde gas sensors.
Disclosure of Invention
The present invention aims to solve at least one of the technical problems existing in the prior art. Therefore, the invention provides the sensing material for formaldehyde detection, and the preparation method and application thereof, and the sensing material can be used for rapid formaldehyde detection, and has the advantages of high sensitivity, high response speed and low cost.
The technical scheme adopted by the invention is as follows:
in a first aspect of the present invention, there is provided a method for preparing a formaldehyde detection sensor material, comprising the steps of:
s1, dissolving a metal source in an organic solvent to prepare a metal source solution; the metal source is a zinc source and/or a tin source;
s2, adding graphene oxide into the metal source solution, adjusting the pH value of the solution to be alkaline, and stirring for reaction to obtain a first mixed solution containing metal oxide and graphene oxide through supermolecule assembly and compounding;
s3, adding small organic molecules and a reducing agent into the first mixed solution, and heating for reaction to obtain a second mixed solution containing small organic molecule modified reduced graphene oxide and metal oxide; the small organic molecule is selected from 5-amino-1-naphthalene-sulfonic acid;
s4, carrying out impurity removal treatment on the second mixed solution.
According to some embodiments of the invention, in step S1, the metal source is selected from zinc acetate (Zn (CH 3 COO) 2 ) And/or tin acetate (Sn (CH) 3 COO) 2 )。
According to some embodiments of the invention, in step S2, the mass ratio of the added amount of graphene oxide to the metal source is (1 to 1.2): 1. in order to facilitate the fully dispersed mixing of graphene oxide after being added into the metal source dispersion liquid, graphene oxide can be prepared into graphene oxide dispersion liquid with a certain concentration and then added into the metal source solution.
According to some embodiments of the invention, in step S3, a mass ratio of the added amount of the small organic molecule to the graphene oxide is 1: (1.5-2); the mass ratio of the reducing agent to the graphene oxide is (2-5): 1, a step of; preferably, the mass ratio of the reducing agent to the graphene oxide is 3:1. the heating temperature for the heating reaction is generally 80.+ -. 10 ℃.
According to some embodiments of the invention, the reducing agent is selected from at least one of hydrazine hydrate, ascorbic acid. Preferably, the reducing agent is hydrazine hydrate.
According to some embodiments of the invention, in step S1, the organic solvent is selected from organic alcohols; methanol, ethanol, etc. can be specifically used. In addition, after the metal source is mixed with the organic solvent, the metal source can be fully dispersed and dissolved by stirring, vibration, physical ultrasound and other methods, so as to obtain a uniform dispersion system.
According to some embodiments of the invention, in step S4, the impurity removal treatment comprises washing and centrifugation.
In a second aspect of the present invention, there is provided a formaldehyde detection sensor material produced by any one of the methods for producing formaldehyde detection sensor materials provided in the first aspect of the present invention.
In a third aspect of the present invention, there is provided an application of any of the formaldehyde detection sensing materials provided in the second aspect of the present invention in detecting formaldehyde gas.
According to a fourth aspect of the present invention, there is provided a formaldehyde detection sensor comprising a gas-sensitive electrode, wherein a gas-sensitive coating is provided on the surface of the gas-sensitive electrode, and the material of the gas-sensitive coating comprises any of the formaldehyde detection sensing materials provided in the second aspect of the present invention.
The embodiment of the invention has the beneficial effects that:
the embodiment of the invention provides a preparation method of a sensing material for formaldehyde detection, wherein graphene oxide and metal oxide are compounded through the effect of supermolecules, then organic micromolecules are added to reduce the barrier of the composite material so as to improve the gas response performance of the material to formaldehyde, and then the graphene oxide is reduced by a chemical reduction method to prepare a reduced graphene oxide and metal oxide composite material modified by the organic micromolecules; the adopted raw materials are simple and easy to obtain, and the cost is low; graphene oxide is used as a base material, so that the method is environment-friendly, the condition is mild in the synthesis process, and the energy is saved; in addition, the organic micromolecules and the reduced graphene oxide are compounded through non-covalent bonds in the reaction process, so that the two-dimensional plane structure of the graphene is not damaged, and the intrinsic electrical and thermodynamic properties of the graphene can be maintained; the sensing material prepared by the preparation method can quickly respond and recover formaldehyde gas at room temperature, and has high reaction sensitivity, low detection limit and high response speed.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the following description will simply explain the drawings that are required to be used in the description of the embodiments.
FIG. 1a is a schematic structural diagram of the supramolecular assembly ZnO-GO of example 1;
FIG. 1b is a schematic diagram of the structure of 5-amino-1-naphthalene-sulfonic acid, a small organic molecule, in example 1;
FIG. 1c is a schematic diagram of the structure of the composite product ZnO-ANS-rGO prepared in example 1;
FIG. 2 is an SEM topography of the sensing material prepared in example 1;
FIG. 3 is a graph showing the results of the rapid response and recovery test of the sensing materials prepared in examples 1-2 and comparative examples 1-2 to formaldehyde;
FIG. 4 is a graph showing the results of the test of the cycling stability of the sensing material prepared in example 1 for formaldehyde detection;
FIG. 5 is a graph showing the results of the test of the response of the sensor material prepared in example 1 to formaldehyde at different concentrations.
Detailed Description
The conception and the technical effects produced by the present invention will be clearly and completely described in conjunction with the embodiments below to fully understand the objects, features and effects of the present invention. It is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments, and that other embodiments obtained by those skilled in the art without inventive effort are within the scope of the present invention based on the embodiments of the present invention.
Example 1
According to the sensing material for formaldehyde detection, graphene oxide is used as a matrix material, zinc oxide nano particles are assembled on the graphene oxide by utilizing supermolecule interaction to improve the responsiveness and selectivity of the material to formaldehyde gas, and then 5-amino-1-naphthalene-sulfonic acid small molecules are doped in a graphene composite material, and the specific synthesis steps are as follows:
s1, 35mg of zinc acetate (Zn (CH) 3 COO) 2 ) Dissolving in 50mL of methanol, and obtaining a uniform dispersion system by a physical stirring mode;
s2, adding 5mL of Graphene Oxide (GO) dispersion liquid (water is used as a solvent) with the concentration of 1mg/mL into the dispersion system prepared in the step S1, regulating the pH of the solution to be alkaline, and stirring for reaction to form a first mixed solution of a supermolecule assembly (ZnO-GO) containing metal oxide and graphene oxide through supermolecule assembly and compounding; the structural schematic diagram of the supramolecular assembly ZnO-GO is shown in FIG. 1 a;
s3, adding 90mg of 5-amino-1-naphthalene-sulfonic Acid (ANS) micromolecules and hydrazine hydrate solution (with the concentration of 98 percent) which is 3 times of the mass of the graphene oxide into the first mixed solution prepared in the step S2, and placing the mixture into a heating device for heating reaction at the temperature of 80+/-10 ℃ to finally obtain the reduced graphene oxide modified by the 5-amino-1-naphthalene-sulfonic acid and a metal oxide composite product (ZnO-ANS-rGO) to formA second mixed solution; wherein the structural formula of the 5-amino-1-naphthalene-sulfonic Acid (ANS) is
The structural schematic diagram is shown in fig. 1 b; the structural schematic diagram of the composite product ZnO-ANS-rGO is shown in FIG. 1 c;
s4, washing the second mixed solution prepared in the step S3 in a centrifugal way to remove unreacted hydrazine hydrate and other impurities in the solution, and thus obtaining the ZnO-ANS-rGO composite sensing material.
And carrying out SEM (electron microscope) test on the prepared sensing material, wherein a morphology chart of the obtained SEM is shown as a figure 2, and (a) and (b) in the figure 2 both represent distribution patterns of ZnO nano particles on the surface of an rGO sheet layer.
Example 2
The preparation method of the sensing material for formaldehyde detection comprises the following steps:
s1, 35mg of tin acetate (Sn (CH) 3 COO) 2 ) Dissolving in 50mL of methanol, and obtaining a uniform dispersion system by a physical stirring mode;
s2, adding 10mL of Graphene Oxide (GO) dispersion liquid with the concentration of 1mg/mL into the dispersion system prepared in the step S1, regulating the pH value of the solution to be alkaline, and stirring for reaction to form a supermolecule assembly (SnO) containing metal oxide and graphene oxide through supermolecule assembly and recombination 2 -GO);
s3, adding 90mg of 5-amino-1-naphthalene-sulfonic Acid (ANS) micromolecule and hydrazine hydrate solution (with the concentration of 98 percent) which is 2 times of the mass of the graphene oxide into the first mixed solution prepared in the step S2, and placing the mixture into a heating device for heating reaction at the temperature of 80+/-10 ℃ to finally obtain the reduced graphene oxide modified by the 5-amino-1-naphthalene-sulfonic acid and metal oxide composite product (SnO 2 -ANS-rGO) to form a second mixed liquor;
s4, washing the second mixed solution prepared in the step S3 in a centrifugal way to remove unreacted hydrazine hydrate and other impurities in the solution, thereby preparing SnO 2 -an ANS-rGO composite sensing material.
Comparative example 1
A method of preparing a sensing material comprising the steps of:
s1, 35mg of tin acetate (Zn (CH) 3 COO) 2 ) Dissolving in 50mL of methanol, and obtaining a uniform dispersion system by a physical stirring mode;
s2, adding 8mL of Graphene Oxide (GO) dispersion liquid with the concentration of 1mg/mL into the dispersion system prepared in the step S1, regulating the pH value of the solution to be alkaline, and stirring for reaction to form a first mixed liquid containing a metal oxide and a supermolecule assembly (ZnO-GO) of the graphene oxide through supermolecule assembly and compounding;
s3, adding 30mg of 4-hydroxyquinoline (4 HQ) micromolecules and hydrazine hydrate solution which is 3 times of the graphene oxide in mass into the first mixed solution prepared in the step S2, and placing the mixed solution into a heating device for heating reaction at the temperature of 80+/-10 ℃ to finally obtain a reduced graphene oxide modified by the 4-hydroxyquinoline and metal oxide composite product (ZnO-4 HQ-rGO) to form a second mixed solution; wherein the structural formula of the 4-hydroxyquinoline (4 HQ) is as follows
S4, washing the second mixed solution prepared in the step S3 in a centrifugal way to remove unreacted hydrazine hydrate and other impurities in the solution, and thus obtaining the ZnO-4HQ-rGO composite sensing material.
Comparative example 2
A method of preparing a sensing material comprising the steps of:
s1, 35mg of zinc acetate (Zn (CH) 3 COO) 2 ) Dissolving in 50mL of methanol, and obtaining a uniform dispersion system by a physical stirring mode;
s2, adding 6mL of Graphene Oxide (GO) dispersion liquid with the concentration of 1mg/mL into the dispersion system prepared in the step S1, regulating the pH value of the solution to be alkaline, and stirring for reaction to form a first mixed liquid containing a metal oxide and a supramolecular assembly (ZnO-GO) of the graphene oxide through supramolecular assembly and compounding;
s3, adding hydrazine hydrate solution which is 3 times of the graphene oxide in mass into the first mixed solution prepared in the step S2, and placing the solution into a heating device for heating reaction at the temperature of 80+/-10 ℃ to finally obtain a reduced graphene oxide and metal oxide composite product (ZnO-rGO) to form a second mixed solution;
s4, washing the second mixed solution prepared in the step S3 in a centrifugal way to remove unreacted hydrazine hydrate and other impurities in the solution, and thus obtaining the ZnO-rGO composite sensing material.
The sensing material prepared by the method can be applied to formaldehyde gas detection, and particularly can be used for preparing a formaldehyde detection sensor so as to be used for formaldehyde gas detection. The preparation of the formaldehyde detection sensor by using the sensing material comprises the following operation steps:
1) Dispersing a sensing material in deionized water to obtain sensing material dispersion liquid;
2) Coating the sensing material dispersion liquid prepared in the step 1) on the surface of a test electrode in a liquid manner, removing the water of the sensing material dispersion liquid coated on the test electrode in a liquid manner, and forming a gas-sensitive coating on the surface of the test electrode to prepare the gas-sensitive electrode;
3) And (3) connecting the gas-sensitive electrode prepared in the step (2) to a gas-sensitive testing device to prepare the formaldehyde detection sensor. That is, the sensor comprises a gas-sensitive electrode, the surface of the gas-sensitive electrode is provided with a gas-sensitive coating, and the material of the gas-sensitive coating is the sensing material.
The formaldehyde gas to be detected is detected by adopting the formaldehyde detection sensor; the detection method specifically comprises the following steps: a. and placing the gas-sensitive electrode in a closed test cavity in an air atmosphere, testing the initial resistance of the gas-sensitive electrode, injecting formaldehyde gas with a certain concentration into the test cavity after the initial resistance is stabilized, recording the resistance change of the formaldehyde gas, and opening the test cavity after the response is finished, so that the air atmosphere is restored in the test cavity, and recording the resistance change of the gas-sensitive electrode.
The formaldehyde detection sensors prepared by the sensing materials in the embodiment 1-2 and the comparative example 1-2 are used for respectively carrying out gas-sensitive phase response and recovery test on formaldehyde gas with the concentration of 50ppm so as to examine the response and recovery performance of each sensing material on formaldehyde gas, and the obtained results are shown in the figure 3; FIG. 3 (a) shows the response and recovery test results of the sensing material prepared in example 1 to formaldehyde gas; (b) The response and recovery test results of the sensing material prepared in example 2 to formaldehyde gas; (c) The response and recovery test results of the sensing material prepared in comparative example 1 to formaldehyde gas are shown; (d) The sensing material prepared in comparative example 2 was tested for its response to formaldehyde gas and recovery. As can be seen from fig. 3, the sensing materials modified and doped with small organic molecules 5-amino-1-naphthalene-sulfonic acid in example 1 and example 2 have higher response values to formaldehyde; comparative example 1 the response of the modified 4-hydroxyquinoline doped sensor material to formaldehyde gas was not evident.
In addition, the sensor prepared by using the sensor material of example 1 was used to detect formaldehyde gas at a concentration of 50ppm, and the results of the cycle stability test were shown in FIG. 4. As can be seen from the results shown in FIG. 4, the sensing material prepared in example 1 has good stability in formaldehyde gas detection cycle.
The sensor prepared by the sensor material of example 1 was used for testing formaldehyde gases with different concentrations (5 ppm, 120ppm, 30ppm, 50ppm, 100ppm and 150 ppm) to examine the response performance of the sensor material to formaldehyde gases with different concentrations. The results are shown in FIG. 5; FIG. 5 (a) is data of response of the sensing material to formaldehyde gas at different concentrations; (b) The relationship between the formaldehyde concentration and the response data of the sensing material to formaldehyde is shown. As can be seen from fig. 5, the sensing material of example 1 has a low detection limit and has a linear relationship with formaldehyde response and concentration.
The embodiments of the present invention have been described in detail with reference to the accompanying drawings, but the present invention is not limited to the above embodiments, and various changes can be made within the knowledge of one of ordinary skill in the art without departing from the spirit of the present invention.
Claims (8)
1. The preparation method of the sensing material for formaldehyde detection is characterized by comprising the following steps of:
s1, dissolving a metal source in an organic solvent to prepare a metal source solution; the metal source is a zinc source and/or a tin source;
s2, graphene oxide is added into the metal source solution, the pH value of the solution is regulated to be alkaline, and the solution is stirred for reaction to obtain a first mixed solution;
s3, adding small organic molecules and a reducing agent into the first mixed solution, and heating for reaction to obtain a second mixed solution; the organic small molecule is selected from 5-amino-1-naphthalene-sulfonic acid, and the mass ratio of the reducing agent to the graphene oxide is (2-5): 1, a step of;
s4, carrying out impurity removal treatment on the second mixed solution.
2. The method for producing a formaldehyde detection sensor material according to claim 1, wherein in step S1, the metal source is selected from zinc acetate and/or tin acetate.
3. The method for producing a formaldehyde detection sensor material according to claim 1, wherein the reducing agent is at least one selected from the group consisting of hydrazine hydrate and ascorbic acid.
4. The method for producing a formaldehyde sensor according to claim 1, wherein in step S1, the organic solvent is selected from alcohol solvents.
5. The method for producing a formaldehyde detection sensor material according to any one of claims 1 to 4, wherein in step S4, the impurity removal treatment includes washing and centrifugation.
6. A formaldehyde detection sensor material, which is produced by the method for producing a formaldehyde detection sensor material according to any one of claims 1 to 5.
7. The use of the sensing material for formaldehyde detection according to claim 6 for detecting formaldehyde gas.
8. The formaldehyde detection sensor is characterized by comprising a gas-sensitive electrode, wherein a gas-sensitive coating is arranged on the surface of the gas-sensitive electrode;
the material of the gas-sensitive coating layer comprises the formaldehyde detection sensing material according to claim 6.
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| CN113120950B (en) * | 2021-03-04 | 2023-05-12 | 华南师范大学 | Gas-sensitive material, preparation method thereof, gas-sensitive electrode and gas-sensitive detection equipment |
| CN113443646B (en) * | 2021-06-30 | 2022-09-13 | 华南师范大学 | Composite material and preparation method and application thereof |
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