CN108918600B - High-selectivity composite gas-sensitive material for detecting acetic acid gas in air - Google Patents
High-selectivity composite gas-sensitive material for detecting acetic acid gas in air Download PDFInfo
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Abstract
The invention discloses a high-selectivity composite gas-sensitive material for detecting acetic acid gas in air, and belongs to the technical field of gas-sensitive materials. The composite gas-sensitive material consists of C3N4-ZnO wherein C3N4The mass of (A) is 5 of the total mass of the material-20%. The indirectly heated gas-sensitive sensor made of the composite material as the sensitive material has the sensitivity of 0.1ppm acetic acid of 1.2-1.4 at the working temperature of 300 ℃, the sensitivity of the element to 1000ppm acetic acid reaches 290-350, and the sensitivity to the same 1000ppm acetone, formaldehyde, ethanol, acetaldehyde and ammonia gas is below 31, which shows that C is C3N4The sensitivity of zinc oxide to acetic acid gas is improved, the gas sensitivity selectivity of zinc oxide to acetic acid gas is improved, the concentration of acetic acid in air can be rapidly detected, and the interference of acetone, formaldehyde, ethanol, acetaldehyde, ammonia gas and other gases is eliminated.
Description
Technical Field
The invention belongs to the field of gas-sensitive materials, and particularly relates to a composite gas-sensitive material for detecting acetic acid gas in air.
Background
Acetic acid is a volatile colorless liquid with strong pungent odor, has strong corrosivity, can cause skin and mucosa blister, red swelling symptom, and causes rhinitis, bronchitis when the concentration is high, and acute chemical pneumonia can occur in serious cases. At present, the application of acetic acid in chemical enterprises is wider, and more enterprises relate to monitoring the concentration of acetic acid in environmental evaluation and acceptance monitoring. The sanitary standard in America, Japan and the like is 25mg/m3(about 9.3ppm), the limit of acetic acid in air of a working place is not established in China. The existing methods for measuring the concentration of acetic acid in air mainly adopt gas chromatography, ion chromatography and the like, and the methods need expensive instruments and equipment, and take a long time for sampling analysis.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a high-selectivity composite gas-sensitive material for detecting acetic acid gas in air, so that the composite material can eliminate the interference of acetone, formaldehyde, ethanol, acetaldehyde, ammonia gas and the like, and can quickly detect the concentration of the acetic acid gas in the air.
The invention is realized by the following technical scheme.
The invention provides a high-selectivity composite gas sensitive material for detecting acetic acid gas in air, which comprises ZnO and C3N4Wherein: c3N4The mass of (A) is 5-20% of the total mass of the material.
C above3N4The preparation method and the process are as follows: 2 g of melamine were placed in a crucible, raised to 520 ℃ in a muffle furnace at a rate of 5 ℃/min and kept at a constant temperature of 520 ℃ for 5 hours. After naturally cooling to room temperature, the product is washed with deionized water and absolute ethyl alcohol for three times respectively, dried for 24 hours at 60 ℃ and ground into powder for later use.
C above3N4The preparation process of the ZnO composite material comprises the following steps: respectively weighing a certain amount of C3N4Sonication in 20ml of deionized water for 1 hour to give C3N4Suspending the suspension, weighing a certain amount of Zn (NO)3)2·6H2O, adding to C while stirring3N4And fully stirring the suspension for 30 minutes, then slowly dropwise adding 1mol/L NaOH solution into the suspension to adjust the pH of the mixed solution to 10.0, then adding deionized water until the volume of the mixture is 70ml, transferring the reaction solution into a 100ml hydrothermal reaction kettle to react for 12 hours at 180 ℃, washing the obtained precipitate with absolute ethyl alcohol for three times, and drying the product for 24 hours at 80 ℃.
The material of the invention can be used as a sensitive material of an acetic acid gas sensitive element, and the method for manufacturing the indirectly heated gas sensitive element by utilizing the material comprises the following steps: mixing and grinding 0.1 g of the material and 0.5 g of terpineol to prepare slurry, and coating the slurry on the surface of an alumina ceramic tube by using a small brush; the dimensions of the alumina ceramic tube are: the length is 6 mm, the inner diameter is 1.6 mm, the outer diameter is 2 mm, gold prizes are used as electrodes at two ends of the alumina tube, gold wires are welded on the electrodes as leads, and the distance between the electrodes is 1 mm; placing a nickel-chromium alloy wire as a heating wire in the alumina tube, and controlling the temperature of the sensitive material on the surface of the alumina tube by controlling the current flowing through the heating wire and the voltage at two ends of the heating wire; and (3) drying the alumina tube coated with the sensitive material slurry under an infrared lamp to obtain the indirectly heated gas sensitive element. The sensitivity of the element to a gas is the ratio of the resistance of the element in air to the resistance of the element in the gas being measured at the operating temperature.
Compared with the prior art, the invention has the following technical effects:
when the working temperature is 300 ℃, the sensitivity of the element to 1000ppm acetic acid reaches 290-350, and the sensitivity to acetone, formaldehyde, ethanol, acetaldehyde and ammonia gas with the same concentration is below 31, which shows that C is the temperature of the gas sensitive sensor3N4Not only improves the sensitivity of zinc oxide to acetic acid gas, but also improves the gas sensitivity selectivity of zinc oxide to acetic acid gas; the sensitivity to 0.1ppm acetic acid gas reaches 1.2-1.4, and the response and recovery time to 0.1ppm acetic acid gas do not exceed 20 s. The material has short response recovery time to acetic acid gas, and can realize the rapid detection of the concentration of acetic acid in the air.
Detailed Description
The present invention will be described in detail with reference to specific examples, but the present invention is not limited to the examples.
Example 1
0.04 g of C is weighed out separately3N4Sonication in 20ml of deionized water for 1 hour to give C3N4The suspension, in turn weighed 2.97g of Zn (NO)3)2·6H2O, adding to C while stirring3N4And fully stirring the suspension for 30 minutes, then slowly dropwise adding 1mol/L NaOH solution into the suspension to adjust the pH of the mixed solution to 10.0, then adding deionized water until the volume of the mixture is 70ml, transferring the reaction solution into a 100ml hydrothermal reaction kettle to react for 12 hours at 180 ℃, washing the obtained precipitate with absolute ethyl alcohol for three times, and drying the product for 24 hours at 80 ℃. To obtain a catalyst containing 5 wt% of C3N4-a ZnO composite.
The material is made into an indirectly heated element, and the highest sensitivity of the indirectly heated element to 0.1, 1, 10, 100 and 1000ppm acetic acid gas at the working temperature of 300 ℃ is respectively 1.2, 2.0, 7.2, 25.8, 81.5 and 290.0; the sensitivity to 1000ppm acetone, formaldehyde, ethanol, acetaldehyde and ammonia gas is below 20.1; the response time and recovery time for 0.1ppm acetic acid did not exceed 20 seconds.
Example 2
0.08 g of C was weighed out separately3N4Sonication in 20ml of deionized water for 1 hour to give C3N4The suspension, in turn weighed 2.97g of Zn (NO)3)2·6H2O, adding to C while stirring3N4And fully stirring the suspension for 30 minutes, then slowly dropwise adding 1mol/L NaOH solution into the suspension to adjust the pH of the mixed solution to 10.0, then adding deionized water until the volume of the mixture is 70ml, transferring the reaction solution into a 100ml hydrothermal reaction kettle to react for 12 hours at 180 ℃, washing the obtained precipitate with absolute ethyl alcohol for three times, and drying the product for 24 hours at 80 ℃. To obtain a catalyst containing 10 wt% of C3N4-a ZnO composite.
The material is made into an indirectly heated element, and the highest sensitivity of the indirectly heated element to 0.1, 1, 10, 100 and 1000ppm acetic acid gas at the working temperature of 300 ℃ is respectively 1.3, 2.5, 9.2, 40.7, 168.6 and 312.3; the sensitivity to 1000ppm acetone, formaldehyde, ethanol, acetaldehyde and ammonia gas is below 23.0; response time and recovery time for 0.1ppm acetic acid did not exceed 18 seconds.
Example 3
0.12 g of C was weighed out separately3N4Sonication in 20ml of deionized water for 1 hour to give C3N4The suspension, in turn weighed 2.97g of Zn (NO)3)2·6H2O, adding to C while stirring3N4And fully stirring the suspension for 30 minutes, then slowly dropwise adding 1mol/L NaOH solution into the suspension to adjust the pH of the mixed solution to 10.0, then adding deionized water until the volume of the mixture is 70ml, transferring the reaction solution into a 100ml hydrothermal reaction kettle to react for 12 hours at 180 ℃, washing the obtained precipitate with absolute ethyl alcohol for three times, and drying the product for 24 hours at 80 ℃. To obtain a catalyst containing 15 wt% of C3N4-a ZnO composite.
The material is made into an indirectly heated element, and the highest sensitivity of the indirectly heated element to 0.1, 1, 10, 100 and 1000ppm acetic acid gas at the working temperature of 300 ℃ is respectively 1.4, 3.8, 13.4, 56.8, 212.4 and 350.0; the sensitivity to 1000ppm acetone, formaldehyde, ethanol, acetaldehyde and ammonia gas is below 31.0; response time and recovery time for 0.1ppm acetic acid did not exceed 16 seconds.
Example 4
0.16g of C was weighed out separately3N4Sonication in 20ml of deionized water for 1 hour to give C3N4The suspension, in turn weighed 2.97g of Zn (NO)3)2·6H2O, adding to C while stirring3N4And fully stirring the suspension for 30 minutes, then slowly dropwise adding 1mol/L NaOH solution into the suspension to adjust the pH of the mixed solution to 10.0, then adding deionized water until the volume of the mixture is 70ml, transferring the reaction solution into a 100ml hydrothermal reaction kettle to react for 12 hours at 180 ℃, washing the obtained precipitate with absolute ethyl alcohol for three times, and drying the product for 24 hours at 80 ℃. Obtaining a catalyst containing 20 wt% of C3N4-a ZnO composite.
The material is made into an indirectly heated element, and the highest sensitivity of the indirectly heated element to 0.1, 1, 10, 100 and 1000ppm acetic acid gas at the working temperature of 300 ℃ is measured to be 1.2, 2.9, 10.2, 38.6, 123.4 and 312.4 respectively; the sensitivity to 1000ppm acetone, formaldehyde, ethanol, acetaldehyde and ammonia gas is below 24.0; the response time and recovery time for 0.1ppm acetic acid did not exceed 20 seconds.
Claims (2)
1. A high-selectivity composite gas-sensitive material for detecting acetic acid gas in air is characterized in that the gas-sensitive material consists of C3N4-ZnO, wherein: c3N4The mass of (A) is 5-20% of the total mass of the material; the gas sensitive material is prepared by the following steps:
(1) weighing 0.04-0.16 g of C3N4Sonication in 20ml of deionized water for 1 hour to give C3N4A suspension;
(2) 2.97g of Zn (NO) are weighed out3)2·6H2O, added to the above C while stirring3N4Fully stirring the suspension for 30 minutes;
(3) slowly dropwise adding 1mol/L NaOH solution into the suspension stirred in the step (2), adjusting the pH of the mixed solution to 10.0, and adding deionized water to obtain reaction liquid with the volume of 70 ml;
(4) and (3) transferring the reaction solution to a 100ml hydrothermal reaction kettle, reacting for 12h at 180 ℃, washing the obtained precipitate with absolute ethyl alcohol, and drying the product for 24h at 80 ℃.
2. The use of the composite gas-sensitive material of claim 1 in an acetic acid gas sensor made as a sensitive material.
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