CN113173602A - Preparation method of n-nonanal volatile gas sensitive material - Google Patents
Preparation method of n-nonanal volatile gas sensitive material Download PDFInfo
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- CN113173602A CN113173602A CN202110399336.XA CN202110399336A CN113173602A CN 113173602 A CN113173602 A CN 113173602A CN 202110399336 A CN202110399336 A CN 202110399336A CN 113173602 A CN113173602 A CN 113173602A
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- C01G41/00—Compounds of tungsten
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- 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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- C—CHEMISTRY; METALLURGY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C—CHEMISTRY; METALLURGY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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Abstract
The invention discloses a preparation method of n-nonanal volatile gas sensitive material in the technical field of gas sensitive material, which comprises the following steps of (1) mixing WCl6Dissolving in methanol, and weighing RuCl3Adding RuCl3Adding the mixture into the mixed solvent while stirring; (2) transferring the mixed solution into a high-pressure reaction kettle, sealing for reaction, naturally cooling, centrifuging, washing and drying to obtain a precursor; (3) carrying out heat treatment on the precursor in an inert atmosphere to obtain the gas sensitive material; when the gas sensitive material prepared by the invention is used for detecting n-nonanal volatile gas, the detection precision can be improved.
Description
Technical Field
The invention belongs to the technical field of gas sensitive materials, and particularly relates to a preparation method of a n-nonanal volatile gas sensitive material.
Background
Rice is one of staple food of human beings, contains abundant nutrient substances, is a main heat source of human bodies, is closely related to the life of people, and the quality of the rice is directly related to the national civilization. Rice is aged and mildewed during storage, which is controlled by adjusting its own moisture content and cannot be eliminated all the time, thus affecting the practicality of rice, and aging of rice needs to be detected. As the storage time is prolonged, the content of aldehyde volatile substances such as n-nonanal and the like generated by rice aging is increased. Therefore, the detection of the concentration of the n-nonanal is of great significance for the recognition of the rice storage quality.
The change of the concentration of the n-nonanal can represent the deterioration degree to a certain extent, people often judge whether the rice is aged according to the smell of the n-nonanal, but the sensory evaluation method has the defects of strong subjectivity and low accuracy and has potential health hazard to operators. Based on the aspects of physicochemical and microbial detection, the prior art discloses a method for detecting the content of fatty aldehyde in vegetable-derived edible oil and application thereof, which is published as CN 111562329A and published as 2020.08.21, and the method adopts ultra-high performance liquid chromatography-tandem quadrupole mass spectrometry to detect the content of n-nonanal.
Disclosure of Invention
The invention aims to overcome the defects in the prior art, provides the preparation method of the n-nonanal volatile gas sensitive material, solves the technical problem of low detection sensitivity in the prior art, and can obviously improve the detection sensitivity by using the method.
The purpose of the invention is realized as follows: a method for preparing a n-nonanal volatile gas sensitive material, which comprises the following steps,
(1) mixing WCl6Dissolving in methanol, and weighing RuCl3Adding RuCl3Adding the mixture into the mixed solvent while stirring;
(2) transferring the mixed solution into a high-pressure reaction kettle, sealing for reaction, naturally cooling, centrifuging, washing and drying to obtain a precursor;
(3) and carrying out heat treatment on the precursor in an inert atmosphere to obtain the gas sensitive material.
In the step (1), WCl6And RuCl3The mass ratio of (A) to (B) is 60-90: 1.
As a further improvement of the invention, in the step (2), the sealing reaction temperature is 160 ℃ and the sealing reaction time is 24 hours.
As a further improvement of the invention, in the step (3), the temperature of the heat treatment is 300-400 ℃ and the time is 2 h.
As a further improvement of the invention, in the step (1), WCl6And a methanol solvent at a molar ratio of 1: 1.
as a further improvement of the invention, the weight percentage of the Ru element in the gas sensitive material is 1%.
As a further improvement of the invention, the inert atmosphere is nitrogen or argon.
As a further improvement of the invention, in the step (2), during drying, the mixture is dried in a freeze dryer for 24-36 h.
As a further improvement of the invention, in the step (3), the temperature rise rate during the heat treatment is 2 ℃/min.
In order to further improve the upper specific surface area of the prepared gas sensitive material, the microstructure of the gas sensitive material is sea urchin-shaped, and the average diameter is 600-800 nm.
The specific surface area of the gas sensitive material prepared by the method is obviously improved, and the detection sensitivity of the gas sensitive material to the n-nonanal serving as a rice aging marker is improved.
Drawings
FIG. 1 shows pure WO3-xAnd 1wt% Ru-doped WO3-xTransmission electron microscope image of gas sensitive material, in which (a) is pure WO3-xTEM image, (b) 1wt% Ru-doped WO3-xTransmission electron microscopy images.
FIG. 2 shows pure WO3-xAnd 1wt% Ru-doped WO3-xGraph of specific surface area, in which (a) is pure WO3-xSpecific surface area curve, (b) 1wt% Ru-doped WO3-xCurve of specific surface area.
FIG. 3 shows pure WO3-xAnd 1wt% Ru-doped WO3-xResponse/recovery profile of gas sensor to 1ppm n-nonanal.
Detailed Description
The invention is further described below with reference to the accompanying drawings.
A preparation method of n-nonanal volatile gas sensitive material comprises the following steps:
(1) mixing WCl6Dissolving in methanol, and weighing RuCl3Adding RuCl3Adding the mixture into the mixed solvent while stirring;
(2) transferring the mixed solution into a high-pressure reaction kettle, sealing for reaction, naturally cooling, centrifuging, washing and drying to obtain a precursor;
(3) carrying out heat treatment on the precursor in an inert atmosphere to obtain the gas sensitive material;
(4) and adding deionized water into the obtained gas sensitive material, grinding to form paste, uniformly coating the paste on the outer surface of a gas sensor substrate, completely covering a gold electrode, and naturally drying at room temperature to form a gas sensitive coating to obtain the gas sensitive element.
In step (1), WCl6And a methanol solvent at a molar ratio of 1: 1, WCl6And RuCl3The mass ratio of (A) to (B) is 60-90: 1; in the step (2), the sealing reaction temperature is 160 ℃, and the time is 24 hours; drying in a freeze dryer for 24-36 hr;
in the step (3), during the heat treatment, the temperature is raised to 400 ℃ at the temperature raising rate of 2 ℃/min for 2 h, and the inert atmosphere is nitrogen or argon.
In the step (4), the prepared gas sensitive material contains 1% of Ru element by weight, the microstructure of the gas sensitive material is sea urchin-shaped, and the average diameter is 600-800 nm.
Example 1
(1) Weighing 0.375 g WCl6Dissolved in 80 ml of methanol solvent, 5 mg of RuCl was weighed3Adding the mixture into the mixed solvent while stirring;
(2) transferring the mixed solution into a high-pressure reaction kettle, carrying out hydrothermal reaction at 160 ℃ for 24 hours, and carrying out centrifugal drying to obtain a precursor;
(3) placing the precursor in an inert atmosphere, and carrying out heat treatment at 300 ℃ for 2 h to obtain a gas sensitive material;
wherein the prepared gas sensitive material component comprises WO3-xAnd Ru, WO3-xAnd Ru 99% and 1% by mass, respectively, WO in this example3-xIs W18O49。
The prepared gas sensitive material is detected by a transmission electron microscope, and the microstructure of the gas sensitive material is obviously shown to be sea urchin-shaped as shown in figure 1 and pure WO3-xHas an average diameter of 700-800 nm and is doped with 1wt% of Ru3-xThe average diameter of the crystal grains is 600-700 nm, and the size of the crystal grains is obviously reduced; the prepared gas-sensitive material was subjected to a specific surface area test, as shown in FIG. 2, pure WO3-xHas a specific surface of 17 m2/g, 1wt% Ru doped WO3-xThe specific surface area is 104 m2/g, and the specific surface area is obviously improved; in synthetic air (79% N)2+21%O2) The prepared sensor is subjected to n-nonanal volatile gas test under the environment, as shown in figure 3, 1wt% of Ru is doped with WO when 1ppm of n-nonanal gas is introduced3-xThe sensitivity of the compound reaches 40.2 which is far higher than that of pure WO3-xSensitivity of (12.4), analysis of 1ppm n-nonanal gas response curve, 1wt% Ru doped WO as shown in FIG. 33-xThe response/recovery time of (1) is respectively 8 s and 102 s, which is faster than that of pure WO3-xResponse/recovery time of (12 s/149 s).
Example 2
This example is different from example 1 in that Ag was used in place of RuCl in step (1)3The component of the prepared gas-sensitive material comprises WO3-xAnd Ag, the mass percent of which is 99 percent and 1 percent respectively; pure WO3-xHas a specific surface of 17 m2/g, 1wt% Ag doped WO3-xHas a specific surface of 50 m 2/g; when 1ppm of n-nonanal gas is introduced, 1wt% of Ag is doped with WO3-xThe sensitivity of the product reaches 15.6 which is higher than that of pure WO3-xSensitivity of (12.4); 1wt% Ag doped WO3-xThe response/recovery time of (1) is 10 s and 122 s respectively, which is faster than that of pure WO3-xResponse/recovery time of (12 s/149 s).
Example 3
This example differs from example 1 in that Pt was used in place of RuCl in step (1)3The component of the prepared gas-sensitive material comprises WO3-xAnd Pt, the mass percent of which is 99% and 1% respectively; when the gas sensitive material is detected, pure WO is adopted3-xHas a specific surface of 17 m2/g, 1wt% Pt doped WO3-xHas a specific surface of 47 m 2/g; 1wt% Pt was doped with WO when 1ppm n-nonanal gas was introduced3-xThe sensitivity of the product reaches 19.4 which is higher than that of pure WO3-xSensitivity of (12.4); 1wt% Pt doped WO3-xThe response/recovery time of (1) is 9 s and 116 s respectively, which is faster than that of pure WO3-xResponse/recovery time of (12 s/149 s).
Example 4
This example differs from example 1 in that Au was used in place of RuCl in step (1)3The component of the prepared gas-sensitive material comprises WO3-xAnd Au, the mass percent of which is respectively 99% and 1%; when the gas sensitive material is detected, pure WO is adopted3-xHas a specific surface of 17 m2/g, 1wt% of Au doped WO3-xHas a specific surface of 64 m 2/g; when 1ppm of n-nonanal gas is introduced, 1wt% of Au is doped with WO3-xThe sensitivity of the product reaches 28.6, which is higher than that of pure WO3-xSensitivity of (12.4); 1wt% Au-doped WO3-xThe response/recovery time of (1) is 8 s and 136 s respectively, which is faster than that of pure WO3-xResponse/recovery time of (12 s/149 s).
Example 5
This example differs from example 1 in that Pd is used in place of RuCl in step (1)3The component of the prepared gas-sensitive material comprises WO3-xAnd Pd, the mass percent of which is 99% and 1% respectively; detecting the gas sensitive material to obtain pure WO3-xHas a specific surface of 17 m2/g, 1wt% Pd doped WO3-xHas a specific surface of 44 m 2/g. (ii) a 1wt% Pd doped WO when 1ppm n-nonanal gas was introduced3-xThe sensitivity of the product reaches 16.3 which is higher than that of pure WO3-xSensitivity of (12.4); 1wt% Pd doped WO3-xResponse/recovery times of 11 s and 132 s, respectively, faster than pureWO3-xResponse/recovery time of (12 s/149 s).
As can be seen from the above examples, the specific surface area of the gas sensitive material prepared by the method is remarkably improved, and the detection sensitivity of the gas sensitive material on the n-nonanal serving as a rice aging marker is improved.
Example 6
This example differs from example 1 in that RuCl3The mass of (2) was 6.25 g.
Example 7
This example differs from example 1 in that RuCl3The mass of (3) was 4.17 g.
The present invention is not limited to the above-mentioned embodiments, and based on the technical solutions disclosed in the present invention, those skilled in the art can make some substitutions and modifications to some technical features without creative efforts according to the disclosed technical contents, and these substitutions and modifications are all within the protection scope of the present invention.
Claims (10)
1. A method for preparing a n-nonanal volatile gas sensitive material, which comprises the following steps,
(1) mixing WCl6Dissolving in methanol, and weighing RuCl3Adding RuCl3Adding the mixture into the mixed solvent while stirring;
(2) transferring the mixed solution into a high-pressure reaction kettle, sealing for reaction, naturally cooling, centrifuging, washing and drying to obtain a precursor;
(3) and carrying out heat treatment on the precursor in an inert atmosphere to obtain the gas sensitive material.
2. The method for preparing n-nonanal volatile gas sensitive material in the step (1), wherein WCl is used in the step (1)6And RuCl3The mass ratio of (A) to (B) is 60-90: 1.
3. The method for preparing n-nonanal volatile gas sensitive material according to claim 1, wherein in the step (2), the sealing reaction is carried out at 160 ℃ for 24 hours.
4. The method as claimed in claim 1, wherein the heat treatment temperature in step (3) is 300-400 ℃ and the time is 2 h.
5. The method for preparing n-nonanal volatile gas sensitive material in the step (1), wherein WCl is used in the step (1)6And a methanol solvent at a molar ratio of 1: 1.
6. the method for preparing the n-nonanal volatile gas sensitive material according to claim 1, wherein the weight percentage of the Ru element in the gas sensitive material is 1%.
7. The method for preparing n-nonanal volatile gas sensitive material according to claim 1, wherein the inert atmosphere is nitrogen or argon.
8. The method for preparing n-nonanal volatile gas sensitive material in the step (2), wherein the drying is carried out in a freeze dryer for 24-36 h.
9. The method for preparing n-nonanal volatile gas sensitive material according to claim 4, wherein in the step (3), the temperature rise rate during the heat treatment is 2 ℃/min.
10. The method for preparing n-nonanal volatile gas sensitive material according to any one of claims 1 to 8, wherein the microstructure of the gas sensitive material is sea urchin-shaped, and the average diameter is 600-800 nm.
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| CN114455629A (en) * | 2022-01-27 | 2022-05-10 | 扬州大学 | Preparation method of ternary composite material for gas sensing and product thereof |
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