CN111254708B - CNTs/polyaniline-based flexible ammonia gas sensing material and preparation method thereof - Google Patents
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Abstract
The invention relates to a CNTs/polyaniline-based flexible ammonia sensing material and a preparation method thereof. The surface of the PET fiber is impregnated with an ethylenediamine solution to modify amino functional groups, the CNTs are combined with the surface of the PET fiber through an ultrasonic oscillation adsorption process, and the polyaniline is combined with the surface of the CNTs through an in-situ polymerization reaction. According to the invention, the flexible PET fiber is used as a substrate, and the surface of the PET fiber is modified with amino to improve the loading capacity of the CNTs on the PET surface, so that the gas-sensitive performance of the CNTs/polyaniline material to ammonia gas is improved. The ammonia sensing material obtained by the invention has good gas response and good ammonia gas selectivity.
Description
Technical Field
The invention belongs to the field of gas detection and gas-sensitive materials, and relates to a CNTs/polyaniline-based flexible ammonia gas sensing material and a preparation method thereof.
Background
Ammonia gas is a colorless gas with pungent odor, and is used as an important chemical reagent, and is often used as a precursor of many nitrides in the field of food, and ammonia gas is also often used as a protein detection agent, however, ammonia gas has flammable and toxic characteristics, and researches show that when the concentration of ammonia gas is more than 300ppm, the ammonia gas can cause serious damage to human organs, so that the ammonia gas is very important for detecting the existence and concentration of ammonia gas in industrial production and living application.
Currently, common ammonia sensing materials are mainly classified into three types: the first type is a metal oxide ammonia sensing material which has better response and recovery speed, better chemical stability and larger influence by environmental humidity; the second type is a nano carbon material ammonia sensing material which has better gas response, but has longer response and recovery time and higher preparation cost; the third type is transition metal dichalcogenide ammonia sensing material, which has wider gas detection range, but has poorer gas selectivity and yet needs to be improved in chemical stability. With the development of gas detection technology, requirements such as higher response, faster response recovery speed and better stability are provided for gas sensitive materials in gas sensors.
Among the above sensing materials, Carbon Nanotubes (CNTs) have been widely used because of their advantages such as large specific surface area, many active sites, and good conductivity, but their response to gas is still low and their selectivity to gas is poor. Aiming at the problems of low gas response and poor gas selectivity of CNTs and the like, an electron channel is formed by adopting an in-situ Polyaniline (PANI) mode and the CNTs, so that the migration capability of electrons is improved, and the gas response of the CNTs can be improved. On the basis of preparing the CNTs/polyaniline gas-sensitive material, the invention adopts the flexible PET fiber as the substrate, and increases the CNTs load by modifying amino on the surface of the PET fiber, thereby further enhancing the gas response and the gas selectivity of the CNTs/polyaniline gas-sensitive material.
Disclosure of Invention
Technical problem to be solved
In order to avoid the defects of the prior art, the invention provides a CNTs/polyaniline-based flexible ammonia gas sensing material and a preparation method thereof, so as to further improve the gas-sensitive performance of the prior art.
Technical scheme
A flexible ammonia sensing material based on CNTs/polyaniline is characterized in that: PET fibers are used as a material substrate, amino functional groups are modified on the PET fibers, and a CNTs layer and polyaniline are adsorbed on the surfaces of the PET fibers.
The preparation method of the CNTs/polyaniline-based flexible ammonia sensing material is characterized by comprising the following steps:
step 1: soaking PET fiber in 50-70 wt% concentration ethylene diamine solution at 40-70 deg.c for 10-30min to complete the surface modification of PET to obtain amino functional group;
step 2: soaking PET fibers into CNTs suspension with the concentration of 0.2-0.5g/L, and adsorbing for 1-3 hours by ultrasonic oscillation, wherein a CNTs layer is adsorbed on the surfaces of the PET fibers;
and step 3: soaking the PET fiber with the CNTs layer adsorbed on the surface into an aniline-hydrochloric acid solution, stirring for 1-2 hours at a low temperature of 0-4 ℃, then adding an ammonium persulfate-hydrochloric acid solution, and stirring for reacting for 4-8 hours; in the aniline-hydrochloric acid solution, the concentration of aniline in the solution is 2.5 wt%, and the concentration of hydrochloric acid is 1 mol/L; the concentration of ammonium persulfate in the ammonium persulfate-hydrochloric acid solution is 0.025g/ml, and the concentration of hydrochloric acid is 1 mol/L.
Advantageous effects
The invention provides a CNTs/polyaniline-based flexible ammonia sensing material and a preparation method thereof. The surface of the PET fiber is impregnated with an ethylenediamine solution to modify amino functional groups, the CNTs are combined with the surface of the PET fiber through an ultrasonic oscillation adsorption process, and the polyaniline is combined with the surface of the CNTs through an in-situ polymerization reaction. According to the invention, the flexible PET fiber is used as a substrate, and the surface of the PET fiber is modified with amino to improve the loading capacity of the CNTs on the PET surface, so that the gas-sensitive performance of the CNTs/polyaniline material to ammonia gas is improved. The ammonia sensing material obtained by the invention has good gas response and good ammonia gas selectivity.
According to the invention, the flexible PET fiber is used as the sensing material substrate, so that the specific surface area of the original flat substrate with the same size is increased, and the attachment area of the ammonia sensing material is increased; and the loading capacity of the CNTs on the PET surface is improved by modifying amino groups on the PET fiber surface, so that the gas-sensitive performance of the CNTs/polyaniline material is improved. The invention aims to provide a novel ammonia sensing material which has larger ammonia response and better ammonia gas selectivity and can be used for detecting ammonia gas in a wider range, and a preparation method of the novel ammonia sensing material.
Drawings
FIG. 1 is a flow chart of the preparation of the CNTs/polyaniline-based flexible ammonia sensing material in the invention;
FIG. 2 is a microstructure diagram of a CNTs/polyaniline-based flexible ammonia gas sensing material according to one embodiment of the present invention;
FIG. 3 is a gas response curve of a CNTs/polyaniline-based flexible ammonia gas sensing material according to one embodiment of the present invention;
FIG. 4 is a diagram showing the ammonia gas minimum detection limit of a CNTs/polyaniline-based flexible ammonia gas sensing material according to an embodiment of the present invention;
FIG. 5 is a gas selectivity peak diagram of a CNTs/polyaniline-based flexible ammonia gas sensing material according to one embodiment of the invention.
Detailed Description
The invention will now be further described with reference to the following examples and drawings:
the preparation method of the CNTs/polyaniline-based flexible ammonia sensing material is characterized by comprising the following steps:
step 1: the method of immersing PET fiber into ethylene diamine solution is adopted to modify amino on the surface of PET.
Step 2: and adsorbing the CNTs layer on the surface of the PET fiber by adopting an ultrasonic oscillation adsorption process.
And step 3: and preparing polyaniline on the CNTs layer by adopting in-situ polymerization reaction.
The process for modifying the surface of the PET fiber with the amino group in the step 1 comprises the following experimental raw materials and parameters: the ethylenediamine solution with surface modified amino group has ethylenediamine concentration of 50-70 wt%, soaking temperature of 40-70 deg.c and soaking time of 10-30 min.
The specific preparation process of the PET fiber surface modification amino comprises the following steps: ultrasonic treating PET fiber in absolute alcohol, soaking in 50-70 wt% concentration ethylene diamine solution at 40-70 deg.c for 10-30min to modify the surface of PET fiber with amino group.
The ultrasonic oscillation adsorption process in the step 2 comprises the following experimental raw materials and parameters: and (3) immersing the PET fibers into the CNTs suspension, and carrying out ultrasonic oscillation for adsorption for 1-3 hours. In the CNTs suspension, the concentration of CNTs is 0.5-0.5 g/L.
The specific preparation process of the ultrasonic oscillation adsorption process comprises the following steps: dispersing CNTs into an ethanol solution, carrying out ultrasonic vibration for 0.5-2 hours to form CNTs suspension, then arranging PET fibers into the CNTs suspension, and carrying out ultrasonic vibration for 1-3 hours, wherein the CNTs are attached to the surface of the PET.
The in-situ polymerization reaction of the step 3 comprises the following experimental raw materials and experimental parameters: and (2) immersing the PET fiber cloth into an aniline-hydrochloric acid solution, stirring for 1-2 hours, then dropwise adding an ammonium persulfate-hydrochloric acid solution, and stirring for reaction for 4-8 hours. The in-situ polymerization reaction is carried out at a low temperature of 0-4 ℃.
In the aniline-hydrochloric acid solution, the concentration of aniline in the solution is 2.5 wt%, and the concentration of hydrochloric acid is 1 mol/L.
In the ammonium persulfate-hydrochloric acid solution, the concentration of ammonium persulfate in the solution is 0.025g/ml, and the concentration of hydrochloric acid is 1 mol/L.
The preparation process of the in-situ polymerization reaction comprises the following steps: adding the aniline solution into hydrochloric acid solution with the concentration of 1mol/L to prepare aniline-hydrochloric acid solution with the aniline concentration of 2.5 wt%, then immersing the PET fiber into the aniline-hydrochloric acid solution, and stirring for 1-2 hours at the temperature of 0-4 ℃. And then adding ammonium persulfate into a hydrochloric acid solution with the concentration of 1mol/L to prepare 0.025g/ml ammonium persulfate-hydrochloric acid solution, dropwise adding the ammonium persulfate-hydrochloric acid solution into an aniline-hydrochloric acid solution soaked with PET fibers, and stirring the solution at the temperature of between 0 and 4 ℃ for 4 to 8 hours to generate the CNTs/polyaniline gas-sensitive material.
Example (b):
as shown in figure 1, PET fibers are used as a material substrate, amino functional groups are modified on the PET fibers, and a CNTs layer and polyaniline are adsorbed on the surfaces of the PET fibers.
The preparation method of the flexible ammonia gas sensing material based on the CNTs/polyaniline comprises the following steps:
step 1: the method of immersing PET fiber into ethylene diamine solution is adopted to modify amino on the surface of PET.
Step 2: and adsorbing the CNTs layer on the surface of the PET fiber by adopting an ultrasonic oscillation adsorption process.
And step 3: and preparing polyaniline on the CNTs layer by adopting in-situ polymerization reaction.
The process for modifying the surface of the PET fiber with the amino group in the step 1 comprises the following experimental raw materials and parameters: performing surface modification on the amino-modified ethylenediamine solution, wherein the concentration of ethylenediamine is 50 wt%, the impregnation temperature is 50 ℃, and the impregnation time is 15 min;
the specific preparation process of the PET fiber surface modification amino comprises the following steps: after the PET fiber is subjected to ultrasonic treatment in absolute ethyl alcohol, the PET fiber is immersed into an ethylenediamine solution with the concentration of 50 wt% at the temperature of 50 ℃, and amino groups can be modified on the surface of the PET fiber after immersion for 15 min.
Or the ethylene diamine solution in the step 1 accounts for 70 wt%, the dipping temperature is 40-70 ℃, and the dipping time is 10-30 min.
Or the ethylene diamine solution in the step 1 accounts for 40 wt%, the dipping temperature is 40-70 ℃, and the dipping time is 10-30 min.
The ultrasonic oscillation adsorption process in the step 2 comprises the following experimental raw materials and parameters: and (3) immersing the PET fibers into the CNTs suspension, and carrying out ultrasonic oscillation for 1 hour. The concentration of CNTs in the CNTs suspension was 0.2 g/L.
The specific preparation process of the ultrasonic oscillation adsorption process comprises the following steps: dispersing CNTs into an ethanol solution, performing ultrasonic oscillation for 0.5 hour to form CNTs suspension, then arranging PET fibers into the CNTs suspension, and performing ultrasonic oscillation for 2 hours, wherein the CNTs are attached to the surface of the PET.
Or the concentration of the CNTs suspension in the step 2 is 0.3g/L, and the ultrasonic vibration adsorption time is 1-3 hours;
or the concentration of the CNTs suspension in the step 2 is 0.5g/L, and the ultrasonic vibration adsorption time is 1-3 hours;
the in-situ polymerization reaction of the step 3 comprises the following experimental raw materials and experimental parameters: and (2) immersing the PET fiber cloth into an aniline-hydrochloric acid solution, stirring for 1 hour, then dropwise adding an ammonium persulfate-hydrochloric acid solution, and stirring for reaction for 4 hours. The in situ polymerization reaction is carried out at a low temperature of 4 ℃.
In the aniline-hydrochloric acid solution, the concentration of aniline in the solution is 2.5 wt%, and the concentration of hydrochloric acid is 1 mol/L.
In the ammonium persulfate-hydrochloric acid solution, the concentration of ammonium persulfate in the solution is 0.025g/ml, and the concentration of hydrochloric acid is 1 mol/L.
The preparation process of the in-situ polymerization reaction comprises the following steps: the aniline solution was added to a hydrochloric acid solution having a concentration of 1mol/L to prepare an aniline-hydrochloric acid solution having an aniline concentration of 2.5 wt%, and then the PET fiber was immersed in the aniline-hydrochloric acid solution and stirred at 4 ℃ for 1 hour. And then adding ammonium persulfate into a hydrochloric acid solution with the concentration of 1mol/L to prepare a 0.025g/ml ammonium persulfate-hydrochloric acid solution, dropwise adding the ammonium persulfate-hydrochloric acid solution into an aniline-hydrochloric acid solution soaked with PET fibers, and stirring the solution at the temperature of 4 ℃ for 4 hours to obtain the CNTs/polyaniline gas-sensitive material.
Or the concentration of aniline and hydrochloric acid in the aniline-hydrochloric acid solution in the step 3 is unchanged, the concentration of ammonium persulfate in the ammonium persulfate-hydrochloric acid solution is unchanged, the ammonium persulfate-hydrochloric acid solution is stirred for 2 hours at the low temperature of 0 ℃, and then the ammonium persulfate-hydrochloric acid solution is added to be stirred and reacted for 8 hours;
or the concentration of aniline and hydrochloric acid in the aniline-hydrochloric acid solution in the step 3 is unchanged, the concentration of ammonium persulfate in the ammonium persulfate-hydrochloric acid solution is unchanged, the ammonium persulfate-hydrochloric acid solution is stirred for 1.5 hours at the low temperature of 2 ℃, and then the ammonium persulfate-hydrochloric acid solution is added, and the stirring reaction is carried out for 6 hours.
FIG. 2 is a microstructure diagram of a CNTs/polyaniline-based flexible ammonia gas sensing material, wherein a diagram is an SEM magnified diagram of 2500 times, and a diagram B is an SEM magnified diagram of 50000 times.
FIG. 3 is a gas response curve of a CNTs/polyaniline-based flexible ammonia gas sensing material of the present invention and a comparative example. The CNTs/polyaniline-based flexible ammonia sensing material prepared by adopting the steps has the advantages that the resistance of the material is increased along with the increase of the concentration of introduced ammonia, the gas response is continuously improved, when the gas concentration is 100ppm, the output response value is 163.03%, and the gas response value is improved by 2.96 times compared with that of a proportional material.
FIG. 4 is a gas selective peak diagram of a CNTs/polyaniline-based flexible ammonia gas sensing material. The flexible ammonia sensing material based on the CNTs/polyaniline prepared by the steps has small response to gases such as methanol, ethanol, acetone, formaldehyde and the like, has a large response value to ammonia, and is greatly improved compared with the response value of the comparative ratio.
FIG. 5 shows the ammonia gas minimum detection limit of the flexible ammonia gas sensing material based on CNTs/polyaniline. The CNTs/polyaniline-based flexible ammonia sensing material prepared by the steps has the minimum detection concentration of 71ppb of ammonia.
Comparative example:
the preparation of the PET fiber without the surface modification of the amino group comprises the steps of adopting the PET fiber as a material substrate, and adsorbing a CNTs layer and polyaniline on the surface of the PET fiber.
The preparation method of the flexible ammonia gas sensing material based on the CNTs/polyaniline comprises the following steps:
step 1: and adsorbing the CNTs layer on the surface of the PET fiber by adopting an ultrasonic oscillation adsorption process.
Step 2: and preparing polyaniline on the CNTs layer by adopting in-situ polymerization reaction.
The ultrasonic oscillation adsorption process in the step 1 comprises the following experimental raw materials and parameters: and (3) immersing the PET fibers into the CNTs suspension, and carrying out ultrasonic oscillation for 1 hour. The concentration of CNTs in the CNTs suspension was 0.2 g/L.
The specific preparation process of the ultrasonic oscillation adsorption process comprises the following steps: dispersing CNTs into an ethanol solution, performing ultrasonic oscillation for 0.5 hour to form CNTs suspension, then arranging PET fibers into the CNTs suspension, and performing ultrasonic oscillation for 2 hours, wherein the CNTs are attached to the surface of the PET.
The in-situ polymerization reaction of the step 2 comprises the following experimental raw materials and experimental parameters: and (2) immersing the PET fiber cloth into an aniline-hydrochloric acid solution, stirring for 1 hour, then dropwise adding an ammonium persulfate-hydrochloric acid solution, and stirring for reaction for 4 hours. The in situ polymerization reaction is carried out at a low temperature of 4 ℃.
In the aniline-hydrochloric acid solution, the concentration of aniline in the solution is 2.5 wt%, and the concentration of hydrochloric acid is 1 mol/L.
In the ammonium persulfate-hydrochloric acid solution, the concentration of ammonium persulfate in the solution is 0.025g/ml, and the concentration of hydrochloric acid is 1 mol/L.
The preparation process of the in-situ polymerization reaction comprises the following steps: the aniline solution was added to a hydrochloric acid solution having a concentration of 1mol/L to prepare an aniline-hydrochloric acid solution having an aniline concentration of 2.5 wt%, and then the PET fiber was immersed in the aniline-hydrochloric acid solution and stirred at 4 ℃ for 1 hour. And then adding ammonium persulfate into a hydrochloric acid solution with the concentration of 1mol/L to prepare a 0.025g/ml ammonium persulfate-hydrochloric acid solution, dropwise adding the ammonium persulfate-hydrochloric acid solution into an aniline-hydrochloric acid solution soaked with PET fibers, and stirring the solution at the temperature of 4 ℃ for 4 hours to obtain the CNTs/polyaniline gas-sensitive material.
As can be seen from the above examples, comparative examples and the description of the drawings, the flexible ammonia gas sensing material based on CNTs/polyaniline has a larger ammonia gas response and a good ammonia gas selectivity, can effectively detect the ammonia gas concentration, and has a more excellent detection sensitivity.
Claims (2)
1. A flexible ammonia sensing material based on CNTs/polyaniline is characterized in that: PET fibers are used as a material substrate, amino functional groups are modified on the PET fibers, and a CNTs layer and polyaniline are adsorbed on the surfaces of the PET fibers.
2. The preparation method of the CNTs/polyaniline-based flexible ammonia sensing material according to claim 1, which is characterized by comprising the following steps:
step 1: soaking PET fiber in 50-70 wt% concentration ethylene diamine solution at 40-70 deg.c for 10-30min to complete the surface modification of PET to obtain amino functional group;
step 2: soaking PET fibers into CNTs suspension with the concentration of 0.2-0.5g/L, and adsorbing for 1-3 hours by ultrasonic oscillation, wherein a CNTs layer is adsorbed on the surfaces of the PET fibers;
and step 3: soaking the PET fiber with the CNTs layer adsorbed on the surface into an aniline-hydrochloric acid solution, stirring for 1-2 hours at a low temperature of 0-4 ℃, then adding an ammonium persulfate-hydrochloric acid solution, and stirring for reacting for 4-8 hours; in the aniline-hydrochloric acid solution, the concentration of aniline in the solution is 2.5 wt%, and the concentration of hydrochloric acid is 1 mol/L; the concentration of ammonium persulfate in the ammonium persulfate-hydrochloric acid solution is 0.025g/ml, and the concentration of hydrochloric acid is 1 mol/L.
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