CN112986338A - Hydrogel gas sensor, gas detection device and gas detection method - Google Patents
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Abstract
The invention discloses a hydrogel gas sensor, a gas detection device and a gas detection method, wherein the hydrogel gas sensor comprises conductive hydrogel fixed on a carrier; the conductive hydrogel comprises at least the following components: polyvinyl alcohol, carrageenan and polyionic liquid; the polyionic liquid is at least one selected from alkenyl functionalized ionic liquids; the alkenyl functionalized ionic liquid at least comprises a vinyl ion pair. According to the invention, the polyion liquid is added into the conductive hydrogel, and the conductivity of the conductive hydrogel and the stability of a gel network are improved by introducing the vinyl ion pair, so that the detection sensitivity is improved. The detection method is suitable for real-time rapid detection of nitrogen dioxide because the three supermolecule acting forces in the conductive hydrogel, namely the hydrogen bond acting force, the molecular crystallization and the electrostatic interaction acting force, have higher responsiveness to the nitrogen dioxide.
Description
Technical Field
The invention belongs to the technical field of toxic volatile gas detection, and particularly relates to a hydrogel gas sensor, a gas detection device and a gas detection method.
Background
Nitrogen dioxide is an organic volatile gas with strong oxidizing property, and high concentration of nitrogen dioxide can affect the immune system, respiratory system and nervous system of people, thereby greatly increasing the risks of pneumonia, asthma and neurological diseases. If the nitrogen dioxide reacts with other VOCs gases, new pollutants are further generated, and the human body is more damaged. In recent years, with the increase of the emission of artificial nitrogen dioxide such as automobile exhaust gas and combustion exhaust gas, the health of people is more and more threatened. Therefore, how to effectively detect the nitrogen dioxide and monitor the nitrogen dioxide in situ in real time is urgent.
In recent years, the ionic conductive hydrogel base material is widely applied to the field of gas sensing. Compared with the existing gas sensing materials, such as carbon-based materials, metal materials and other silicon-based materials, the ion-conductive hydrogel base material not only has high conductivity, but also has a soft matrix and a multi-layer porous structure in the system, so that the ion-conductive hydrogel base material is more beneficial to gas sensing.
However, conventional conductive hydrogel gas sensors are mostly based on introducing a substance responsive to a target gas into a hydrogel system to increase the sensitivity of the gel gas sensor. The preparation process usually needs physical doping, and phase separation is easy to generate. Meanwhile, the hydrogel gas sensor is prepared from single raw material components, so that the use of other new gel materials is greatly limited. Therefore, it is necessary to prepare a novel multi-component conductive hydrogel-based gas sensor with high sensitivity and capable of being used for room temperature detection.
Disclosure of Invention
In order to solve the technical problems, the invention provides a hydrogel gas sensor, a gas detection device and a gas detection method, wherein the conductive hydrogel of the sensor is composed of multiple components, so that three supermolecule acting forces, namely hydrogen bond action, PVA molecular crystallization and electrostatic interaction, are formed in a system of the sensor, and the three supermolecule acting forces can form a certain adsorption-desorption process with gas to be detected under the synergistic action, so that the resistance is changed, and the concentration of the gas to be detected can be sensitively detected.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
in one aspect of the present invention, a hydrogel gas sensor is provided, which includes a conductive hydrogel fixed on a carrier;
the conductive hydrogel comprises at least the following components: polyvinyl alcohol, carrageenan and polyionic liquid;
the polyionic liquid is at least one selected from alkenyl functionalized ionic liquids;
the alkenyl functionalized ionic liquid at least comprises a vinyl ion pair.
Optionally, the mass ratio of the polyvinyl alcohol to the carrageenan is 1: 0.1-0.3;
the vinyl ion pair is a vinyl cationic monomer and a vinyl anionic monomer.
The dosage of the vinyl cationic monomer is 1 to 25 percent of the mass of the polyvinyl alcohol;
the molar ratio of the vinyl cationic monomer to the vinyl anionic monomer is 1: 1-10.
Specifically, the mass ratio of the polyvinyl alcohol to the carrageenan is independently selected from 1:0.1, 1:0.15, 1:0.2, 1:0.25 and 1: 0.3.
The amount of the vinyl cationic monomer is independently selected from 1%, 5%, 15%, 23%, 25% of the mass of the polyvinyl alcohol.
The molar ratio of the vinyl cationic monomer to the vinyl anionic monomer is independently selected from 1:1, 1:3, 1:5, 1:7, 1: 10.
Alternatively, the vinyl cationic monomer is 1-vinyl-3-butylimidazolium bromide;
the vinyl anion monomer is sodium p-styrene sulfonate hydrate.
The vinyl cationic monomer and the vinyl anionic monomer are subjected to a crosslinking reaction to obtain polyion liquid, and a crosslinking network is formed, so that the conductivity and the mechanical property of the gel are improved.
Optionally, the polymerization degree of the polyvinyl alcohol is 1600-1800;
the molecular weight of the carrageenan is 700-1000.
Optionally, the water content of the electrically conductive hydrogel is from 75 wt% to 90 wt%.
Specifically, the upper limit of the water content of the ion-conducting gel may be independently selected from 83 wt%, 86 wt%, 88 wt%, 90 wt%; the lower limit of the water content of the ion-conducting gel may be independently selected from 75 wt%, 78 wt%, 80 wt%, 82 wt%.
In another aspect of the present invention, a gas detection device is provided, which includes any one of the above hydrogel gas sensors, a sealed gas detection cavity, and a resistance detector;
the hydrogel gas sensor is positioned in the gas detection cavity;
the hydrogel gas sensor is respectively provided with two leads which are respectively and electrically connected with the resistance detector;
the gas detection cavity is provided with a gas inlet and a gas outlet.
In a third aspect of the present invention, a gas detection method is provided, where the gas detection device is used for gas detection, the method at least includes:
introducing gas with known concentration into the gas detection cavity to obtain the resistance change value of the gas with known concentration in response time;
making a working curve by using the resistance change value of the gas with known concentration;
introducing gas to be detected into the gas detection cavity to obtain a resistance change value of the gas to be detected within recovery time;
and comparing the resistance change value of the gas to be detected with the working curve, and calculating to obtain the concentration of the gas.
Optionally, a method of gas detection, comprising at least:
air is introduced into the gas detection cavity to obtain stable initial resistance R0；
Introducing gas with known concentration into the gas detection cavity to obtain the resistance change value of the gas with known concentration in response time;
making a working curve by using the resistance change value of the gas with known concentration;
introducing gas to be detected into the gas detection cavity to obtain a resistance change value delta R of the gas to be detected within response time;
introducing air into the gas detection cavity to obtain a recovery value of the resistance within the recovery time;
and comparing the resistance change value of the gas to be detected with the working curve, and calculating to obtain the concentration of the gas.
Optionally, the making of the working curve by using the resistance variation value of the gas with the known concentration at least comprises:
the gas concentration is used as an abscissa, and the resistance change value delta R and the initial resistance value R of the gas with the known concentration are used0The ratio of (A) to (B) is plotted on the ordinate to obtain a working curve.
Optionally, the response time is 100-1000 s;
the recovery time is 100-1000 s.
Optionally, the gas is nitrogen dioxide.
The invention has the beneficial effects that:
1. according to the hydrogel gas sensor, the polyion liquid is added into the conductive hydrogel, and the conductivity of the conductive hydrogel and the stability of a gel network are improved by introducing the vinyl ion pair, so that the detection sensitivity is improved.
2. The hydrogel gas sensor has excellent mechanical properties and good conductivity through the synergistic effect among three supermolecule acting forces in the conductive hydrogel, namely hydrogen bond action, PVA molecular crystallization and electrostatic interaction; meanwhile, the responsiveness of the sensor to gas is improved, so that the detection sensitivity is improved.
3. The hydrogel gas sensor has high selectivity on nitrogen dioxide, and can be used for detecting gas concentration at room temperature.
4. The detection method has high sensitivity and strong selectivity, and can quickly detect the gas concentration in real time.
Drawings
FIG. 1 is a schematic structural diagram of a gas detection device according to the present invention;
FIG. 2 is a graph showing the response of the hydrogel gas sensor to different concentrations of nitrogen dioxide in example 1 of the present invention;
FIG. 3 is a graph showing the operation curves obtained in example 1 of the present invention;
FIG. 4 is a graph showing the response and recovery of a hydrogel gas sensor to 40ppm nitrogen dioxide in example 2 of the present invention;
fig. 5 is a graph showing the results of the selectivity of the hydrogel gas sensor to nitrogen dioxide in example 3 of the present invention.
In the figure, 1, a gas detection cavity, 2, a hydrogel gas sensor, 3, conductive hydrogel, 4 and a resistance detector.
Detailed Description
The invention is further illustrated with reference to the following figures and specific examples.
The experimental methods used in the following examples are all conventional methods unless otherwise specified; reagents, materials and the like used in the following examples are commercially available unless otherwise specified.
The polyvinyl alcohol adopted in the embodiment of the invention is produced by Shanghai test, and the polymerization degree is 1750 +/-50; carrageenan, wherein the manufacturer is Shanghai alatin, and the molecular weight is 700-; the 1-vinyl-3-butyl imidazole bromide salt is from Lanzhou chemical and physical research institute of Chinese academy of sciences, and has a purity of 99 percent; the sodium p-styrenesulfonate hydrate is Shanghai Aladdin with purity of 98%.
The gas detection device of the invention has the structure shown in figure 1, and comprises a sealed gas detection cavity 1, a hydrogel gas sensor 2 and a resistance detector 4;
the hydrogel gas sensor 2 includes a carrier and a conductive hydrogel 3 fixed on the carrier. In the embodiment of the invention, the carrier adopts a glass slide, and the conductive hydrogel 3 is fixed on the glass slide by using a copper foil adhesive tape.
The hydrogel gas sensor 2 is positioned in the gas detection cavity 1;
the hydrogel gas sensor 2 is provided with two leads respectively, and the two leads are electrically connected with the resistance detector 4 respectively; in the embodiment of the invention, the resistance detector 4 adopts a universal meter, and the two leads are respectively connected with a red meter pen and a black meter pen of the universal meter. The distance between the two wires is usually no contact and can form a loop, and preferably, the distance between the two wires in the embodiment of the present invention is 3-5 cm.
The gas detection cavity 1 is provided with a gas inlet and a gas outlet.
The volume of the gas detection cavity in the embodiment of the invention is 5-36L.
In the embodiment of the invention, the preparation method of the conductive hydrogel in the hydrogel gas sensor specifically comprises the following steps:
1) adding polyvinyl alcohol and carrageenan into solvent deionized water according to the mass ratio of 1: 0.1-0.3: 5-20, and uniformly mixing at 70-160 ℃ to obtain a polyvinyl alcohol/carrageenan aqueous solution;
specifically, the mass ratio of the polyvinyl alcohol to the carrageenan can be independently selected from 1:0.1, 1:0.15, 1:0.2, 1:0.25 and 1: 0.3;
the mass ratio of the polyvinyl alcohol to the deionized water can be independently selected from: 1:5, 1:10, 1:15, 1:18, 1: 20.
2) Respectively weighing 1-vinyl-3-butylimidazole bromide and sodium p-styrenesulfonate hydrate, wherein the mass of the 1-vinyl-3-butylimidazole bromide is 1% -25% of that of polyvinyl alcohol, adding the 1-vinyl-3-butylimidazole bromide and the sodium p-styrenesulfonate hydrate (the molar ratio of the 1-vinyl-3-butylimidazole bromide to the sodium p-styrenesulfonate hydrate is 1: 1-10) into a polyvinyl alcohol/carrageenan aqueous solution, uniformly mixing at 90-180 ℃, adding a crosslinking agent N, N' -methylene bisacrylamide and an initiator ammonium persulfate, and stirring and reacting for 2-10 hours at 80-150 ℃;
the molar ratio of the 1-vinyl-3-butylimidazolium bromide salt to the sodium p-styrenesulfonate hydrate can be independently selected from 1:1, 1:3, 1:5, 1:7, and 1: 10.
Wherein the dosage of the cross-linking agent is 0.1-1% of the mass of the polyvinyl alcohol, and the dosage of the initiator is 1-15% of the mass of the polyvinyl alcohol.
Specifically, the amount of N, N' -methylenebisacrylamide can be independently selected from 0.1%, 0.15%, 0.5%, 0.7%, 1% by mass of polyvinyl alcohol;
specifically, the dosage of the ammonium persulfate can be independently selected from 1%, 1.25%, 5%, 10% and 15% of the mass of the polyvinyl alcohol;
3) pouring the reactant obtained in the step 2 into a silica gel mold, and storing at the low temperature of 0-5 ℃ for 1-80h to obtain pre-gel;
4) and performing circulating freezing-unfreezing treatment on the pre-gel to obtain the conductive hydrogel.
Wherein the freezing temperature is-40 to-20 deg.C, and the freezing time is at least 1h, preferably 1-15 h.
The thawing temperature is 0-20 deg.C, and the freezing time is at least 1h, preferably thawing time is 1-15 h.
The number of freeze-thaw cycles is 1-100.
Example 1
1) Drawing a working curve
4g of polyvinyl alcohol and 0.8g of carrageenan are dissolved in 40g of deionized water and stirred for 3 hours at 90 ℃ to obtain a homogeneous solution. 0.92g of 1-vinyl-3-butylimidazole bromide and 0.824g of sodium p-styrene sulfonate hydrate (the mass ratio of the two is 1:1) are sequentially added into the stirred polyvinyl alcohol/carrageenan solution and stirred for 1h at 100 ℃. Under the nitrogen atmosphere, 0.006g of N, N' -methylene bisacrylamide and 0.05g of ammonium persulfate are sequentially added into the solution, and after stirring for 6 hours at 120 ℃, the reaction solution is poured into a self-made silica gel pad mold with the length, width and thickness of 7 x 2 x 0.1cm to form the pre-gel.
And (3) storing the pre-gel at 4 ℃ for 24h, then transferring to-20 ℃ for freezing for 4h, then unfreezing at 4 ℃ for 4h, and carrying out 3 freezing-unfreezing cycles in total to obtain the conductive hydrogel. The water content of the conductive hydrogel was measured to be 82.52%.
Fixing the conductive hydrogel on a glass slide by using a copper foil adhesive tape, and fixing copper leads at two ends of the hydrogel by using the copper foil adhesive tape, namely preparing the hydrogel gas sensor.
Connecting the prepared sensor with a lead in a 10L gas detection cavity, connecting a universal meter to the other end of the connected lead, and detecting the gas concentration:
firstly, air is introduced for 1h to obtain stable R0The value is obtained. Then 5ppm nitrogen dioxide is introduced, a stopwatch is started for timing for 300s, and the resistance change value at specified time is recorded; and introducing air again, timing for 360s at the same time, recovering the resistance, and recording the resistance recovery value within the specified time.
The method is adopted to obtain corresponding data of 10ppm, 15ppm, 20ppm, 30ppm and 40ppm nitrogen dioxide in sequence. The collected resistance data is derived through a universal meter program, and the change of the resistance signal along with time can be obtainedValues, as shown in fig. 2. The nitrogen dioxide concentration is taken as the abscissa and the delta R/R is taken0The values are plotted on the ordinate, and a working curve is prepared, as shown in FIG. 3.
2) Detecting the concentration of nitrogen dioxide to be detected
Firstly, air is introduced into an 18L gas detection cavity for 1h to obtain stable R0The value is obtained. Then introducing nitrogen dioxide to be detected, starting a stopwatch for timing for 300s, and recording the resistance change value at the specified time; and introducing air again, timing for 360s at the same time, recovering the resistance, and recording the resistance recovery value within the specified time. The acquired resistance data is exported through a universal meter program, the change value of the resistance signal changing along with time can be obtained, and delta R/R is calculated0Substituting the value into the working curve in the step 1) to obtain the concentration of the nitrogen dioxide.
Example 2
Measuring the response time and the recovery time of the hydrogel gas sensor to nitrogen dioxide:
8g of polyvinyl alcohol and 1.6g of carrageenan are dissolved in 80g of deionized water and stirred for 6 hours at 95 ℃ to obtain a homogeneous solution. 1.84g of 1-vinyl-3-butylimidazole bromide and 1.648g of sodium p-styrene sulfonate hydrate (the mass ratio of the two is 1:1) are sequentially added into the stirred polyvinyl alcohol/carrageenan solution and stirred for 1h at 100 ℃. Under nitrogen atmosphere, 0.01g of N, N' -methylene bisacrylamide and 0.1g of ammonium persulfate are sequentially added into the solution, and after stirring for 8 hours at 120 ℃, the reaction solution is poured into a self-made silica gel pad mold with the length, width and thickness of 7 x 1.5 x 0.2cm to form the pre-gel.
And (3) storing the pre-gel at 4 ℃ for 24h, then transferring to-20 ℃ for freezing for 6h, then unfreezing at 4 ℃ for 6h, and carrying out 3 freezing-unfreezing cycles in total to obtain the conductive hydrogel.
And fixing the conductive hydrogel on a glass slide by using a copper foil adhesive tape, and fixing copper leads at two ends of the hydrogel by using the copper foil adhesive tape, thereby finishing the preparation of the hydrogel gas sensor.
Connecting the prepared sensor with a wire in a 15L gas detection cavity, and connecting the other end of the connected wire into a universal meter for detection:
introducing air for 1h at room temperature to obtainStable R0A value; then introducing 40ppm of nitrogen dioxide, immediately starting a stopwatch for timing for 300s, and recording the resistance change value at specified time; and introducing air again, timing for 360s at the same time, recovering the resistance, and recording the resistance recovery value within the specified time.
In the whole process, the time from the sensor to contact with the nitrogen dioxide to reach 50% of the stable resistance value is calculated and recorded as the response time t of the conductive hydrogel to the nitrogen dioxide1-50(ii) a Calculating the time from the sensor contacting the air to the time of reaching 50% of the stable resistance value, and recording as the recovery time t of the conductive hydrogel to the nitrogen dioxide2-50. With time as the abscissa and Δ R/R0The value is an ordinate, and a graph of the response time and the recovery time of the sensor to the nitrogen dioxide is obtained, as shown in fig. 4, the response time t of the sensor to the nitrogen dioxide1-50At 53s, recovery time t2-5046s, and the sensor has excellent responsiveness and recoverability at room temperature, and can be used for rapid sensing response detection of nitrogen dioxide at room temperature.
Example 3
The hydrogel gas sensor prepared in example 1 was selected for testing selectivity to gas:
taking methanol, ethanol, toluene, acetone and water respectively, taking methanol as an example, injecting the methanol into a gas cavity through an air inlet hole of the gas detection cavity, turning on an external heating power supply, adjusting the heating power to 5W, and heating for 90s to enable the concentration of the methanol in the 20L gas detection cavity to be 500 ppm. And then starting a stopwatch for timing for 300s, recording the resistance change value within the specified time, introducing air after the reaction is finished, timing for 360s at the same time, recovering the resistance, and recording the resistance recovery value within the specified time. The collected resistance data is exported through a multimeter, and a resistance signal change value changing along with time can be obtained. Other VOCs gas operations such as methanol testing operations. Calculating the DeltaR/R of each VOCs0A value and comparing this value with a.DELTA.R/R of 40ppm of nitrogen dioxide0The selectivity results are shown in figure 5, in comparison with the values. It can be seen that the sensor of the present invention has a significant response to nitrogen dioxide only, and substantially no response to other VOCs gases. Shows that the sensor of the invention has high selectivityThe method is suitable for detecting the nitrogen dioxide in the actual sample with the coexistence of various mixed VOCs gases.
Although the present application has been described with reference to a few embodiments, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the application as defined by the appended claims.
Claims (10)
1. A hydrogel gas sensor comprising an electrically conductive hydrogel immobilized on a support;
the conductive hydrogel at least comprises the following components: polyvinyl alcohol, carrageenan and polyionic liquid;
the polyion liquid is selected from at least one of alkenyl functionalized ionic liquid;
the alkenyl functionalized ionic liquid at least comprises a vinyl ion pair.
2. The hydrogel gas sensor according to claim 1,
the mass ratio of the polyvinyl alcohol to the carrageenan is 1: 0.1-0.3;
the vinyl ion pair is a vinyl cationic monomer and a vinyl anionic monomer.
The dosage of the vinyl cationic monomer is 1 to 25 percent of the mass of the polyvinyl alcohol;
the molar ratio of the vinyl cationic monomer to the vinyl anionic monomer is 1: 1-10.
3. The hydrogel gas sensor according to claim 1,
the vinyl cationic monomer is 1-vinyl-3-butylimidazolium bromide;
the vinyl anion monomer is sodium p-styrenesulfonate hydrate;
the polymerization degree of the polyvinyl alcohol is 1600-1800;
the molecular weight of the carrageenan is 700-1000.
4. The hydrogel gas sensor according to claim 1, wherein the water content of the electrically conductive hydrogel is 75 to 90 wt.%.
5. A gas detection device comprising the hydrogel gas sensor of any one of claims 1 to 3, a sealed gas detection chamber, and an electrical resistance detector;
the hydrogel gas sensor is positioned in the gas detection cavity;
the hydrogel gas sensor is provided with two leads respectively, and the two leads are electrically connected with the resistance detector respectively;
and the gas detection cavity is provided with a gas inlet and a gas outlet.
6. A gas detection method using the gas detection device according to claim 5, the method comprising at least:
introducing gas with known concentration into the gas detection cavity to obtain a resistance change value of the gas with known concentration within response time;
making a working curve by using the resistance change value of the gas with known concentration;
introducing gas to be detected into the gas detection cavity to obtain a resistance change value of the gas to be detected within the recovery time;
and comparing the resistance change value of the gas to be detected with the working curve, and calculating to obtain the concentration of the gas.
7. The gas detection method according to claim 6, characterized in that the method comprises at least:
introducing air into the gas detection cavity to obtain stable initial resistance R0；
Introducing gas with known concentration into the gas detection cavity to obtain a resistance change value of the gas with known concentration within response time;
making a working curve by using the resistance change value of the gas with known concentration;
introducing gas to be detected into the gas detection cavity to obtain a resistance change value delta R of the gas to be detected in the response time;
introducing air into the gas detection cavity to obtain a recovery value of the resistance within the recovery time;
and comparing the resistance change value of the gas to be detected with a working curve, and calculating to obtain the concentration of the gas.
8. The method according to claim 6 or 7, wherein the step of generating the operating curve by using the resistance variation value of the gas with the known concentration at least comprises:
the gas concentration is used as an abscissa, and the resistance change value Delta R and the initial resistance value R of the gas with the known concentration are used0The ratio of (A) to (B) is plotted on the ordinate to obtain a working curve.
9. The gas detection method according to claim 6 or 7,
the response time is 100-1000 s;
the recovery time is 100-1000 s.
10. The gas detection method according to claim 6 or 7, wherein the gas is nitrogen dioxide.
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