CN108918600A - It is a kind of for detecting the highly selective composite air-sensitive material of acetic acid gas in air - Google Patents
It is a kind of for detecting the highly selective composite air-sensitive material of acetic acid gas in air Download PDFInfo
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- CN108918600A CN108918600A CN201810454942.5A CN201810454942A CN108918600A CN 108918600 A CN108918600 A CN 108918600A CN 201810454942 A CN201810454942 A CN 201810454942A CN 108918600 A CN108918600 A CN 108918600A
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- 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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Abstract
The invention discloses a kind of for detecting the highly selective composite air-sensitive material of acetic acid gas in air, belongs to gas sensitive technical field.Composite air-sensitive material composition is C3N4- ZnO, wherein C3N4Quality account for the 5-20% of material gross mass.Using the composite material as heater-type gas sensor made of sensitive material, under 300 DEG C of operating temperatures, to the sensitivity of 0.1ppm acetic acid between 1.2-1.4, element reaches 290-350 up to sensitivity to 1000ppm acetic acid, and the sensitivity of the acetone to identical 1000ppm, formaldehyde, ethyl alcohol, acetaldehyde and ammonia 31 hereinafter, showing C3N4Zinc oxide is not only increased to acetic acid gas sensitivity, and improves zinc oxide to acetic acid gas air-sensitive selectivity, the quick detection of acetic acid concentration in air may be implemented, eliminate the interference of the gases such as acetone, formaldehyde, ethyl alcohol, acetaldehyde and ammonia.
Description
Technical field
The invention belongs to gas sensitive fields, and in particular to a kind of for detecting the composite air-sensitive material of acetic acid gas in air
Material, the material for making gas sensor, manufactured gas sensor to low concentration of acetic acid in air have high sensitivity and compared with
Good selectivity.
Background technique
Acetic acid is a kind of colourless liquid volatile, with intense irritation smell, has compared with strong corrosive, can lead to skin
Skin, mucous membrane blistering, red and swollen symptom, cause rhinitis, bronchitis, acute chemical pneumonia can occur for severe one when concentration is higher.Mesh
Acetic acid purposes is wide in preceding chemical company, and the enterprise that acetic acid concentration is monitored involved in environmental impact assessment and Acceptance Monitoring is more and more.Beauty
The sanitary standard of the states such as state, Japan is 25mg/m3(about 9.3ppm), China do not formulate the limit of acetic acid in the air of working place
Value.The method of acetic acid concentration mainly uses gas chromatography and chromatography of ions etc. in measurement air at present, these methods need
Instrument and equipment costly, sampling analysis needs consume a longer time.
Summary of the invention
In order to overcome the deficiencies of the prior art, the technical problem to be solved in the present invention is to provide one kind for detecting second in air
The highly selective composite air-sensitive material of acid gas, can eliminate acetone, formaldehyde, ethyl alcohol, acetaldehyde and ammonia to the composite material
Deng interference, can quickly detect the concentration of acetic acid gas in air.
The present invention is achieved by the following technical programs.
The present invention provides a kind of for detecting the highly selective composite gas sensitive material of acetic acid gas in air, the material
Material composition is ZnO and C3N4, wherein：C3N4Quality account for the 5-20% of material gross mass.
Above-mentioned C3N4Preparation method and process are：2 grams of melamines are placed in crucible, with 5 DEG C/min in Muffle furnace
Rate be increased to 520 DEG C, and keep the temperature 5 hours under 520 DEG C of constant temperature.After cooled to room temperature, product deionized water, nothing
Water-ethanol washs three times respectively, and 24 hours dry at 60 DEG C, is ground into powder stand-by.
Above-mentioned C3N4- ZnO composite material preparation process is：A certain amount of C is weighed respectively3N4In the deionized water of 20ml,
Ultrasonic treatment 1 hour, obtains C3N4Suspension, then claim a certain amount of Zn (NO3)2·6H2O is added to C while stirring3N4It suspends
In liquid, be sufficiently stirred 30 minutes, be then slowly added dropwise into suspension the NaOH solution of 1mol/L by mixed solution adjust pH to
10.0, then plus deionized water to volume of mixture be 70ml, reaction solution is moved in 100ml hydrothermal reaction kettle anti-at 180 DEG C
It answers 12 hours, obtained sediment is washed three times with dehydrated alcohol, and product dries 24 hours at 80 DEG C.
Material of the invention can be used as the sensitive material of acetic acid gas detecting element, make heater-type gas using the material
The method of quick element is：Slurry is made in 0.1 gram of material and 0.5 gram of terpinol mixed grinding, slurry is coated onto oxygen with small brushes
Change the surface of aluminium ceramic tube；The size of alumina ceramic tube is：It is 6 millimeters long, 1.6 millimeters of internal diameter, 2 millimeters of outer diameter, in aluminium oxide
Pipe both ends gold medal makees electrode, spun gold is welded on electrode as lead, distance is 1 millimeter between electrode；It is put in alumina tube
Nichrome wire is set as heater strip, can control aluminium oxide by controlling the electric current for flowing through heater strip and heater strip both end voltage
The temperature of pipe surface sensitive material；The alumina tube for being coated with sensitive material slurry is placed under infrared lamp and is dried to get indirect heat is arrived
Formula gas sensor.Element is that at the working temperature, resistance and element are being tested element in air to the sensitivity of certain gas
The ratio of resistance in gas.
Compared with prior art, the present invention has the following technical effects：
Using the material as heater-type gas sensor made of gas sensitive material, when operating temperature is 300 DEG C, member
Part reaches 290-350 up to sensitivity to 1000ppm acetic acid, and the acetone to same concentrations, formaldehyde, ethyl alcohol, acetaldehyde and ammonia
Sensitivity is 31 hereinafter, showing C3N4Zinc oxide is not only increased to acetic acid gas sensitivity, and improves zinc oxide to acetic acid
Gas air-sensitive selectivity；1.2-1.4, and the response to 0.1ppm acetic acid gas are reached to the sensitivity of 0.1ppm acetic acid gas
It is no more than 20s with recovery time.The material is short to acetic acid gas response recovery time, and acetic acid concentration in air may be implemented
Quickly detection.
Specific embodiment
The present invention is described in detail below in conjunction with specific embodiment, but the present invention is not limited to following embodiments.
Embodiment 1
0.04 gram of C is weighed respectively3N4In the deionized water of 20ml, it is ultrasonically treated 1 hour, obtains C3N4Suspension, then claim
2.97 grams of Zn (NO3)2·6H2O is added to C while stirring3N4In suspension, it is sufficiently stirred 30 minutes, then delays into suspension
Mixed solution is adjusted pH to 10.0 by the slow NaOH solution that 1mol/L is added dropwise, then plus deionized water to volume of mixture be 70ml,
Reaction solution is moved in 100ml hydrothermal reaction kettle and is reacted 12 hours at 180 DEG C, obtained sediment washs three with dehydrated alcohol
Secondary, product dries 24 hours at 80 DEG C.It obtains containing 5wt%C3N4- ZnO composite material.
Heater-type element is made in material, measures element under 300 DEG C of operating temperatures to 0.1,1,10,100,1000ppm
The maximum sensitivity of acetic acid gas is respectively 1.2,2.0,7.2,25.8,81.5,290.0；To 1000ppm acetone, formaldehyde, second
The sensitivity of alcohol, acetaldehyde and ammonia is below 20.1；The acetic acid response time of 0.1ppm and recovery time are no more than 20 seconds.
Embodiment 2
0.08 gram of C is weighed respectively3N4In the deionized water of 20ml, it is ultrasonically treated 1 hour, obtains C3N4Suspension, then claim
2.97 grams of Zn (NO3)2·6H2O is added to C while stirring3N4In suspension, it is sufficiently stirred 30 minutes, then delays into suspension
Mixed solution is adjusted pH to 10.0 by the slow NaOH solution that 1mol/L is added dropwise, then plus deionized water to volume of mixture be 70ml,
Reaction solution is moved in 100ml hydrothermal reaction kettle and is reacted 12 hours at 180 DEG C, obtained sediment washs three with dehydrated alcohol
Secondary, product dries 24 hours at 80 DEG C.It obtains containing 10wt%C3N4- ZnO composite material.
Heater-type element is made in material, measures element under 300 DEG C of operating temperatures to 0.1,1,10,100,1000ppm
The maximum sensitivity of acetic acid gas is respectively 1.3,2.5,9.2,40.7,168.6,312.3；To 1000ppm acetone, formaldehyde, second
The sensitivity of alcohol, acetaldehyde and ammonia is below 23.0；The acetic acid response time of 0.1ppm and recovery time are no more than 18 seconds.
Embodiment 3
0.12 gram of C is weighed respectively3N4In the deionized water of 20ml, it is ultrasonically treated 1 hour, obtains C3N4Suspension, then claim
2.97 grams of Zn (NO3)2·6H2O is added to C while stirring3N4In suspension, it is sufficiently stirred 30 minutes, then delays into suspension
Mixed solution is adjusted pH to 10.0 by the slow NaOH solution that 1mol/L is added dropwise, then plus deionized water to volume of mixture be 70ml,
Reaction solution is moved in 100ml hydrothermal reaction kettle and is reacted 12 hours at 180 DEG C, obtained sediment washs three with dehydrated alcohol
Secondary, product dries 24 hours at 80 DEG C.It obtains containing 15wt%C3N4- ZnO composite material.
Heater-type element is made in material, measures element under 300 DEG C of operating temperatures to 0.1,1,10,100,1000ppm
The maximum sensitivity of acetic acid gas is respectively 1.4,3.8,13.4,56.8,212.4,350.0；To 1000ppm acetone, formaldehyde, second
The sensitivity of alcohol, acetaldehyde and ammonia is below 31.0；The acetic acid response time of 0.1ppm and recovery time are no more than 16 seconds.
Embodiment 4
0.16 gram of C is weighed respectively3N4In the deionized water of 20ml, it is ultrasonically treated 1 hour, obtains C3N4Suspension, then claim
2.97 grams of Zn (NO3)2·6H2O is added to C while stirring3N4In suspension, it is sufficiently stirred 30 minutes, then delays into suspension
Mixed solution is adjusted pH to 10.0 by the slow NaOH solution that 1mol/L is added dropwise, then plus deionized water to volume of mixture be 70ml,
Reaction solution is moved in 100ml hydrothermal reaction kettle and is reacted 12 hours at 180 DEG C, obtained sediment washs three with dehydrated alcohol
Secondary, product dries 24 hours at 80 DEG C.It obtains containing 20wt%C3N4- ZnO composite material.
Heater-type element is made in material, measures element under 300 DEG C of operating temperatures to 0.1,1,10,100,1000ppm
The maximum sensitivity of acetic acid gas is respectively 1.2,2.9,10.2,38.6,123.4,312.4；To 1000ppm acetone, formaldehyde, second
The sensitivity of alcohol, acetaldehyde and ammonia is below 24.0；The acetic acid response time of 0.1ppm and recovery time are no more than 20 seconds.
Claims (2)
1. a kind of for detecting the highly selective composite air-sensitive material of acetic acid gas in air, which is characterized in that the gas sensitive
Composition is C3N4- ZnO, wherein：C3N4Quality account for the 5-20% of material gross mass；The gas sensitive through the following steps that
It is prepared：
(1) C of 0.04~0.16g is weighed3N4In the deionized water of 20ml, it is ultrasonically treated 1 hour, obtains C3N4Suspension；
(2) Zn (NO of 2.97g is weighed3)2·6H2O is added to above-mentioned C while stirring3N4In suspension, it is sufficiently stirred 30 minutes；
(3) NaOH solution of 1mol/L then is slowly added dropwise into the suspension after step (2) stirring, adjust mixed solution pH to
10.0, then plus deionized water, obtain volume be 70ml reaction solution；
(4) above-mentioned reaction solution is moved in 100ml hydrothermal reaction kettle and reacts 12h at 180 DEG C, the anhydrous second of obtained sediment
Alcohol washing, product dry for 24 hours at 80 DEG C.
2. composite air-sensitive material as described in claim 1 is as answering in acetic acid gas detecting element made of sensitive material
With.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110044971A (en) * | 2019-04-16 | 2019-07-23 | 蚌埠学院 | A kind of gas sensitive, preparation method and its application in gas sensor |
| CN110346430A (en) * | 2019-06-17 | 2019-10-18 | 福建师范大学 | A kind of Na+Adulterate g-C3N4Composite material, electrochemical sensor and preparation method thereof, purposes |
| CN112362702A (en) * | 2020-11-13 | 2021-02-12 | 安徽工业大学 | Composite gas-sensitive material with high gas-sensitive selectivity and low detection limit for toluene at room temperature |
| CN115772284A (en) * | 2022-11-17 | 2023-03-10 | 华南师范大学 | Acetic acid gas sensitive film and preparation method and application thereof |
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| CN104297323A (en) * | 2014-11-01 | 2015-01-21 | 济南大学 | Preparation and application of ZnO@CdTe-carboxylation C3N4 photoelectric DNA sensor |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110044971A (en) * | 2019-04-16 | 2019-07-23 | 蚌埠学院 | A kind of gas sensitive, preparation method and its application in gas sensor |
| CN110044971B (en) * | 2019-04-16 | 2021-11-23 | 蚌埠学院 | Gas-sensitive material, preparation method and application thereof in gas-sensitive sensor |
| CN110346430A (en) * | 2019-06-17 | 2019-10-18 | 福建师范大学 | A kind of Na+Adulterate g-C3N4Composite material, electrochemical sensor and preparation method thereof, purposes |
| CN110346430B (en) * | 2019-06-17 | 2021-06-04 | 福建师范大学 | Na+Doping with g-C3N4Composite material, electrochemical sensor, preparation method and application thereof |
| CN112362702A (en) * | 2020-11-13 | 2021-02-12 | 安徽工业大学 | Composite gas-sensitive material with high gas-sensitive selectivity and low detection limit for toluene at room temperature |
| CN115772284A (en) * | 2022-11-17 | 2023-03-10 | 华南师范大学 | Acetic acid gas sensitive film and preparation method and application thereof |
| CN115772284B (en) * | 2022-11-17 | 2023-12-26 | 华南师范大学 | Acetic acid gas sensitive film and preparation method and application thereof |
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