CN108776158A - A kind of gas sensitive material and preparation method for environmental monitoring ammonia emission - Google Patents
A kind of gas sensitive material and preparation method for environmental monitoring ammonia emission Download PDFInfo
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- G—PHYSICS
- G01—MEASURING; TESTING
- 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
- G01N27/125—Composition of the body, e.g. the composition of its sensitive layer
- G01N27/126—Composition of the body, e.g. the composition of its sensitive layer comprising organic polymers
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- G—PHYSICS
- G01—MEASURING; TESTING
- 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
- G01N27/125—Composition of the body, e.g. the composition of its sensitive layer
- G01N27/127—Composition of the body, e.g. the composition of its sensitive layer comprising nanoparticles
Abstract
A kind of gas sensitive material and preparation method for environmental monitoring ammonia emission of the invention, the precursor solution of vanadic anhydride is prepared first, recycle electrostatic spinning that polyethylene pyrrole network alkanone/vanadic anhydride composite nano fiber is prepared, and it carries out calcination processing and obtains Vanadium pentoxide nanotubes fiber, finally surfactant and Vanadium pentoxide nanotubes fiber are added separately in aqueous solution, aniline monomer is added after stirring and stirs, is eventually adding FeCl3Aqueous solution reacts under stirring, and polyaniline/Vanadium pentoxide nanotubes composite gas sensitive material is obtained after filtering and cleaning.The present invention provides the above method, there is the shortcomings of easily being influenced by ambient temperature and humidity, long-time stability are poor and poor selectivity in the detection for overcoming existing ammonia, it is compound by Vanadium pentoxide nanotubes fiber and conducting high polymers object polyaniline, since the two acts synergistically, the sensitivity detected to ammonia is greatly improved.
Description
Technical field
The present invention relates to gas detection domains, and in particular to a kind of gas sensitive material for environmental monitoring ammonia emission and
Preparation method.
Background technology
Ammonia is a kind of colourless and with intense irritation stink gas.It has corrosion and stimulation to the tissue of contact
Effect makes histone be denaturalized, and makes tissue fat saponification, and the solubility for destroying cell membrane is high.So mainly to the upper of human body
Respiratory tract has stimulation and corrosiveness, weakens resistance of the human body to disease.In addition, ammonia can also pass through trigeminal neuralgia tip
Reflex and cause cardiac arrest and breathing stop.It is of great significance to the monitoring of ammonia concentration in environment, the inspection of ammonia
Survey is mainly used for chemical plant, freezer and intelligent public lavatory and aquaculture etc..
Sensor is a kind of defined device being measured and usable output signal is converted into according to certain rule of energy impression
Part or device, are usually made of sensing element and conversion element.Wherein, sensing element refers to energy direct feeling or sound in sensor
The part that should be tested；Conversion element refers to that sensing element impression or the measured of response can be converted into be suitable for transmission in sensor
Or the electric signal part measured.According to according to sensor operating principles, physical sensors and chemical sensor two major classes can be divided into.
Traditional inorganic semiconductor technology and electrochemical sensing technology are used to the test of this toxic gas of ammonia at present.
It is to make at present using the metal oxide semiconductor with huge advantage in terms of cost performance as the sensor of sensitive material
With widest sensor.Its principle responded is based on sensitive oxide material before and after absorption, and oxide conductivity can be sent out
Raw apparent variation, the size of variation is related with the concentration of gas, therefore the change by measuring sensitive layer oxide conductivity
Change can measured concentration size.Currently used semiconductor Gas dependent sensor sensitive materials have WO3Or SnO2Deng.However this
Class sensor selectivity is poor, when being existed simultaneously there are many reducibility gas, it is easy to interference is generated, to influence sensor
Detection to ammonia, furthermore, it is necessary to which detection gas could be used under the high temperature conditions.
Since it is contacted with ammonia matterization reaction occurs for conducting polymer, causes polymer resistive to increase, is a kind of ammonia
Gas sensitive.Conducting polymer gas sensitive can be deposited on various substrates, and can be by selecting different macromoleculars
Chain structure, and it is modified, to obtain different chemical-sensitive performances, improve its sensitivity and choosing that are responded to gas
Selecting property, it is most important that it can work at room temperature, but there is also easily by ambient temperature and humidity shadow for conducting polymer air-sensitive film
It rings, the shortcomings of long-time stability are poor and poor selectivity.Compound and mixed type Semiconductor gas sensors material is developed and developed, this is made
A little materials have the advantages that highly sensitive, highly selective, high stability is to improve the important way of sensor performance to gas with various
Diameter.
Chinese invention patent application number 200810161665.5 discloses a kind of polypyrrole and the compound gas of metal nanoparticle
Quick element and preparation method thereof has multipair interdigital gold electrode, in ceramic sheet matrix and interdigital gold electrode thereon using ceramics as matrix
Surface is coated with the composite air-sensitive film of polypyrrole and palladium nano-particles.Chinese invention patent application number 201610182054.3 is public
A kind of printable flexible ammonia gas sensor has been opened, it is quick to be prepared into ammonia using the compound system of conducting polymer and metal nanometer line
Feel layer, and used preparation method is low temperature solution polycondensation, thus manufactured ammonia gas sensor high sensitivity, reaction speed
Soon, stability is good.Chinese invention patent application number 201310127805.8 discloses water dispersible polyaniline/carbon nanotube compound electric
Resistance type film gas sensor and preparation method thereof, gas-sensitive film are that the in-situ polymerization by polyaniline in carbon nanotube is formed
Compound is formed.Although said program is compound by the nanometer of conducting polymer materials and large specific surface area, gas can be improved
The scattering and permeating of body, raising conducting polymer response sensitivity, raising polymer stabilisation and selectivity, however compound nanometer
Material itself does not have to ammonia gas-sensing properties, and carrier is only used as to provide high surface area, a large amount of to be examined using not only reduction ammonia
Performance is surveyed, and improves manufacturing cost.Therefore, by designing more suitable gas sensitive and structure, by itself and conducting polymer
Object is combined gas sensitive material, is expected to further promote the detectability of ammonia.
Invention content
For existing ammonia detection exist easily influenced by ambient temperature and humidity, long-time stability are poor and poor selectivity etc. lacks
Point, a kind of gas sensitive material and preparation method for environmental monitoring ammonia emission of the invention are special using having higher air-sensitive
Property Vanadium pentoxide nanotubes fiber and conducting high polymers object polyaniline are compound, and the spirit detected to ammonia is greatly improved
Sensitivity.
To solve the above problems, the present invention uses following technical scheme：
A kind of preparation method of gas sensitive material for environmental monitoring ammonia emission, which is characterized in that specific preparation method
For：
（1）It is 3-4 in mass ratio：6-7 weighs polyethylene pyrrole network alkanone and absolute ethyl alcohol, and the polyethylene pyrrole network alkanone is added
In the absolute ethyl alcohol, solution A is at the uniform velocity stirred to get；
（2）It is 1-2 in mass ratio：8-9 weighs soluble vanadic salts and n,N-Dimethylformamide, and the soluble vanadic salts is added
Into the n,N-Dimethylformamide, by the uniform velocity stirring, solution B is obtained；
（3）It is 1-3 by volume ratio:The solution A and solution B of 2-4 mixes, and the solution A is poured into the solution B, is added
Salpeter solution simultaneously stirs, and obtains the precursor solution of vanadic anhydride；
（4）Electrospinning device is added in the precursor solution of vanadic anhydride, by electrostatic spinning process, waits for that solvent volatilizees
Afterwards, composite nano fiber is obtained, then the composite nano fiber is subjected to calcination processing in air atmosphere, obtains five oxidations two
Vanadium nanotube fibers；
（5）By step（4）The deionized water solution containing surfactant in right amount is added in the Vanadium pentoxide nanotubes fiber of preparation
In, aniline monomer is then added, and stir evenly, makes aniline monomer uniform fold in the Vanadium pentoxide nanotubes fiber table
Face is eventually adding FeCl3Aqueous solution reacts under stirring, and after reacting 1-5h, filtering and cleaning obtain the oxygen of polyaniline/five
Change two vanadium nanotube composite gas sensitive materials.
Preferably, step（1）And step（2）In the speed at the uniform velocity stirred be 50-200rpm.
Preferably, step（3）Described in salpeter solution a concentration of 0.5-1.3mol/L；Addition is solution A and solution B
The 2% of gross mass.
Preferably, step（4）Described in electrostatic spinning process using air pump fltting speed be 0.1-0.5mL/min, spinning
Voltage is 40-60kV, and it is 20-50cm to collect distance.
Preferably, the calcination processing be under atmospheric pressure, using at 600-800 DEG C calcine 2-10h after naturally cool to
Room temperature.
Preferably, step（5）Described in FeCl3A concentration of 0.8-2.1mol/L of aqueous solution.
Preferably, step（5）Middle Vanadium pentoxide nanotubes fiber, surfactant, aniline monomer, FeCl3Aqueous solution
Mass ratio be 10:0.1:5：2.
The present invention further provides a kind of gas for environmental monitoring ammonia emission being prepared by the above method is quick
Feel material.
Vanadic anhydride is n-type semiconductor, and there is anion obtained by abjection oxygen atom more stablely in lattice
Hole, it is reversible in certain temperature range to lose oxygen, show good catalytic performance.For the detection sensing of existing ammonia
There is the shortcomings of easily being influenced by ambient temperature and humidity, long-time stability are poor and poor selectivity in material, existing nano material does not have
Catalytic performance is only used as catalyst carrier to provide high surface area, and the detection sensitivity of ammonia has further room for promotion.In view of
This, the present invention proposes a kind of gas sensitive material and preparation method for environmental monitoring ammonia emission, first with polyethylene pyrrole
Network alkanone and soluble vanadic salts are the precursor solution that vanadic anhydride is prepared in raw material；Electrostatic spinning is recycled to be prepared
Obtained composite nano fiber in air atmosphere is carried out calcination processing, obtains vanadic anhydride nanometer by composite nano fiber
Pipe fiber；Finally surfactant and Vanadium pentoxide nanotubes fiber are added separately in aqueous solution, aniline is added after stirring
Monomer simultaneously stirs, and is eventually adding FeCl3Aqueous solution prepares polyaniline/Vanadium pentoxide nanotubes composite gas sensitivity material
Material.Vanadic anhydride is prepared into nanotube fibers by the present invention, is conducive to coming into full contact between ammonia gas and active site,
Its gas-sensitive property is improved, and by the way that it is compound with conducting high polymers object polyaniline, since the two acts synergistically, greatly
Amplitude improves the sensitivity detected to ammonia.
A kind of gas sensitive material and conventional conductive polymer for environmental monitoring ammonia emission prepared by the present invention
It has a clear superiority in ammonia detection performance etc., as shown in table 1.
Table 1：
The present invention provides a kind of gas sensitive material and preparation method for environmental monitoring ammonia emission, with prior art phase
Than the feature and excellent effect protruded is：
1, the present invention proposes a kind of gas sensitive material and preparation method for environmental monitoring ammonia emission, by organic polymer
Conducting polymer and nanotube fibers metal oxide semiconductor combine the organic/inorganic semiconductor composite formed, comprehensive
The respective advantage of conductive polymer polyanaline and oxide semiconductor vanadic anhydride, since the two acts synergistically, in air-sensitive
Aspect imparts many excellent performances of material, greatly improves the detectivity to ammonia gas.
2, the present invention has gas-sensitive property using vanadic anhydride to ammonia, but gas-sensitive property is relatively low, is prepared into nanometer
Pipe fiber can obtain big specific surface area, be conducive to coming into full contact between ammonia gas and active site, be more advantageous to and carry
The gas sensing property of high gas sensitive material.
3, preparation method of the present invention is simple and easy to do, is easy to carry out industrialized development, when can be widely applied to environmental monitoring pair
In the accurate measurement and control of ammonia concentration.
Specific implementation mode
In the following, the present invention will be further described in detail by way of specific embodiments, but this should not be interpreted as to the present invention
Range be only limitted to example below.Without departing from the idea of the above method of the present invention, according to ordinary skill
The various replacements or change that knowledge and customary means are made, should be included in the scope of the present invention.
Embodiment 1
（1）It is 3 in mass ratio：7 weigh polyethylene pyrrole network alkanone and absolute ethyl alcohol, described in polyethylene pyrrole network alkanone addition
In absolute ethyl alcohol, the speed that stirring is arranged is 200rpm, at the uniform velocity stirs to get solution A；
（2）It is 1 in mass ratio：9 weigh soluble vanadic salts and n,N-Dimethylformamide, and the soluble vanadic salts is added to institute
It states in n,N-Dimethylformamide, the speed that stirring is arranged is 200rpm, at the uniform velocity stirs, obtains solution B；
（3）It is 1 by volume ratio:2 solution A and solution B mixing, the solution A is poured into the solution B, concentration is added
It for 0.5mol/L salpeter solutions and stirs, obtains the precursor solution of vanadic anhydride；Addition is solution A and the total matter of solution B
The 2% of amount.
（4）By step（3）Electrospinning device is added in the precursor solution of obtained vanadic anhydride, passes through electrostatic spinning
Technique is 0.3mL/min, spinning voltage 40kV using air pump fltting speed, and it is 50cm to collect distance, after the solvent is volatilized,
Composite nano fiber is obtained, then the composite nano fiber is subjected to calcination processing in air atmosphere, treatment conditions are big
Under air pressure, using cooled to room temperature after calcining 10h at 650 DEG C, Vanadium pentoxide nanotubes fiber is obtained；
（5）By step（4）The appropriate benzene sulfonic acid of base containing surfactant sodium dodecyl is added in the Vanadium pentoxide nanotubes fiber of preparation
In the deionized water solution of sodium, aniline monomer is then added, and stir evenly, makes aniline monomer uniform fold in five oxidation
Two vanadium nanotube fibers surfaces, are eventually adding the FeCl of a concentration of 0.8mol/L3Aqueous solution reacts under stirring, reaction
After 5h, filtering and cleaning are dry, obtain polyaniline/Vanadium pentoxide nanotubes composite gas sensitive material.Vanadic anhydride is received
Mitron fiber, surfactant, aniline monomer, FeCl3The mass ratio of aqueous solution is 10:0.1:5：2.
The sensitivity of the gas sensitive material of ammonia detection in the present embodiment is surveyed using intelligent air-sensitive analysis system
Examination, test temperature are（25±2）DEG C, relative humidity is（50 ± 2）%, response are defined as R=Rg/Ra, and Ra is gas
The aerial resistance of body sensitive material, Rg are that gas sensitive material is tested the resistance in gas in respective concentration.Test result
As shown in table 2.
Embodiment 2
（1）It is 4 in mass ratio：6 weigh polyethylene pyrrole network alkanone and absolute ethyl alcohol, described in polyethylene pyrrole network alkanone addition
In absolute ethyl alcohol, the speed that stirring is arranged is 100rpm, at the uniform velocity stirs to get solution A；
（2）It is 2 in mass ratio：8 weigh soluble vanadic salts and n,N-Dimethylformamide, and the soluble vanadic salts is added to institute
It states in n,N-Dimethylformamide, the speed that stirring is arranged is 100rpm, at the uniform velocity stirs, obtains solution B；
（3）It is 1 by volume ratio:3 solution A and solution B mixing, the solution A is poured into the solution B, concentration is added
It for 1.0mol/L salpeter solutions and stirs, obtains the precursor solution of vanadic anhydride；Addition is solution A and the total matter of solution B
The 2% of amount.
（4）By step（3）Electrospinning device is added in the precursor solution of obtained vanadic anhydride, passes through electrostatic spinning
Technique is 0.45mL/min, spinning voltage 50kV using air pump fltting speed, and it is 25cm to collect distance, after the solvent is volatilized,
Composite nano fiber is obtained, then the composite nano fiber is subjected to calcination processing in air atmosphere, treatment conditions are big
Under air pressure, using cooled to room temperature after calcining 8h at 680 DEG C, Vanadium pentoxide nanotubes fiber is obtained；
（5）By step（4）The deionization containing neopelex in right amount is added in the Vanadium pentoxide nanotubes fiber of preparation
In aqueous solution, aniline monomer is then added, and stir evenly, makes aniline monomer uniform fold in the Vanadium pentoxide nanotubes
Fiber surface is eventually adding the FeCl of a concentration of 2.0mol/L3Aqueous solution reacts under stirring, react 3h after, filtering and
Cleaning, it is dry, obtain polyaniline/Vanadium pentoxide nanotubes composite gas sensitive material.Vanadium pentoxide nanotubes fiber, table
Face activating agent, aniline monomer, FeCl3The mass ratio of aqueous solution is 10:0.1:5：2.
The sensitivity of the gas sensitive material of ammonia detection in the present embodiment is surveyed using intelligent air-sensitive analysis system
Examination, test temperature are（25±2）DEG C, relative humidity is（50 ± 2）%, response are defined as R=Rg/Ra, and Ra is gas
The aerial resistance of body sensitive material, Rg are that gas sensitive material is tested the resistance in gas in respective concentration.Test result
As shown in table 2.
Embodiment 3
（1）It is 3 in mass ratio：6.5 weigh polyethylene pyrrole network alkanone and absolute ethyl alcohol, and institute is added in the polyethylene pyrrole network alkanone
It states in absolute ethyl alcohol, the speed that stirring is arranged is 80rpm, at the uniform velocity stirs to get solution A；
（2）It is 2 in mass ratio：9 weigh soluble vanadic salts and n,N-Dimethylformamide, and the soluble vanadic salts is added to institute
It states in n,N-Dimethylformamide, the speed that stirring is arranged is 80rpm, at the uniform velocity stirs, obtains solution B；
（3）It is 1-3 by volume ratio:The solution A and solution B of 2-4 mixes, and the solution A is poured into the solution B, is added
A concentration of 0.9mol/L salpeter solutions simultaneously stir, and obtain the precursor solution of vanadic anhydride；Addition is solution A and solution B
The 2% of gross mass.
（4）By step（3）Electrospinning device is added in the precursor solution of obtained vanadic anhydride, passes through electrostatic spinning
Technique is 0.15mL/min, spinning voltage 60kV using air pump fltting speed, and it is 50cm to collect distance, after the solvent is volatilized,
Composite nano fiber is obtained, then the composite nano fiber is subjected to calcination processing in air atmosphere, treatment conditions are big
Under air pressure, using cooled to room temperature after calcining 8h at 750 DEG C, Vanadium pentoxide nanotubes fiber is obtained；
（5）By step（4）The deionization that appropriate phosphoric acid fat glycine betaine is added in the Vanadium pentoxide nanotubes fiber of preparation is water-soluble
In liquid, aniline monomer is then added, and stir evenly, makes aniline monomer uniform fold in the Vanadium pentoxide nanotubes fiber
Surface is eventually adding the FeCl of a concentration of 2.0mol/L3Aqueous solution reacts under stirring, after reacting 5h, filters and clear
It washes, obtains polyaniline/Vanadium pentoxide nanotubes composite gas sensitive material.Vanadium pentoxide nanotubes fiber, surface-active
Agent, aniline monomer, FeCl3The mass ratio of aqueous solution is 10:0.1:5：2.
The sensitivity of the gas sensitive material of ammonia detection in the present embodiment is surveyed using intelligent air-sensitive analysis system
Examination, test temperature are（25±2）DEG C, relative humidity is（50 ± 2）%, response are defined as R=Rg/Ra, and Ra is gas
The aerial resistance of body sensitive material, Rg are that gas sensitive material is tested the resistance in gas in respective concentration.Test result
As shown in table 2.
Embodiment 4
（1）It is 3.5 in mass ratio：6 weigh polyethylene pyrrole network alkanone and absolute ethyl alcohol, and institute is added in the polyethylene pyrrole network alkanone
It states in absolute ethyl alcohol, the speed that stirring is arranged is 180rpm, at the uniform velocity stirs to get solution A；
（2）It is 1 in mass ratio：8 weigh soluble vanadic salts and n,N-Dimethylformamide, and the soluble vanadic salts is added to institute
It states in n,N-Dimethylformamide, the speed that stirring is arranged is 180rpm, at the uniform velocity stirs, obtains solution B；
（3）It is 2.5 by volume ratio:3 solution A and solution B mixing, the solution A is poured into the solution B, is added dense
Degree is 1.1mol/L salpeter solutions and stirs, and obtains the precursor solution of vanadic anhydride；Addition is that solution A and solution B are total
The 2% of quality.
（4）By step（3）Electrospinning device is added in the precursor solution of obtained vanadic anhydride, passes through electrostatic spinning
Technique is 0.18mL/min, spinning voltage 60kV using air pump fltting speed, and it is 50cm to collect distance, after the solvent is volatilized,
Composite nano fiber is obtained, then the composite nano fiber is subjected to calcination processing in air atmosphere, treatment conditions are big
Under air pressure, using cooled to room temperature after calcining 2h at 800 DEG C, Vanadium pentoxide nanotubes fiber is obtained；
（5）By step（4）The Vanadium pentoxide nanotubes fiber of preparation is added in the deionized water solution containing imidazoline in right amount, so
After aniline monomer is added, and stir evenly, make aniline monomer uniform fold in the Vanadium pentoxide nanotubes fiber surface, most
The FeCl of a concentration of 1.5mol/L is added afterwards3Aqueous solution reacts under stirring, and after reacting 2h, filtering and cleaning are gathered
Aniline/Vanadium pentoxide nanotubes composite gas sensitive material.Vanadium pentoxide nanotubes fiber, surfactant, aniline list
Body, FeCl3The mass ratio of aqueous solution is 10:0.1:5：2.
The sensitivity of the gas sensitive material of ammonia detection in the present embodiment is surveyed using intelligent air-sensitive analysis system
Examination, test temperature are（25±2）DEG C, relative humidity is（50 ± 2）%, response are defined as R=Rg/Ra, and Ra is gas
The aerial resistance of body sensitive material, Rg are that gas sensitive material is tested the resistance in gas in respective concentration.Test result
As shown in table 2.
Embodiment 5
（1）It is 4 in mass ratio：6.3 weigh polyethylene pyrrole network alkanone and absolute ethyl alcohol, and institute is added in the polyethylene pyrrole network alkanone
It states in absolute ethyl alcohol, the speed that stirring is arranged is 160rpm, at the uniform velocity stirs to get solution A；
（2）It is 2 in mass ratio：9 weigh soluble vanadic salts and n,N-Dimethylformamide, and the soluble vanadic salts is added to institute
It states in n,N-Dimethylformamide, the speed that stirring is arranged is 160rpm, at the uniform velocity stirs, obtains solution B；
（3）It is 1 by volume ratio:2 solution A and solution B mixing, the solution A is poured into the solution B, concentration is added
It for 1.3mol/L salpeter solutions and stirs, obtains the precursor solution of vanadic anhydride；Addition is solution A and the total matter of solution B
The 2% of amount.
（4）By step（3）Electrospinning device is added in the precursor solution of obtained vanadic anhydride, passes through electrostatic spinning
Technique is 0.5mL/min, spinning voltage 55kV using air pump fltting speed, and it is 28cm to collect distance, after the solvent is volatilized,
Composite nano fiber is obtained, then the composite nano fiber is subjected to calcination processing in air atmosphere, treatment conditions are big
Under air pressure, using cooled to room temperature after calcining 4h at 600 DEG C, Vanadium pentoxide nanotubes fiber is obtained；
（5）By step（4）The Vanadium pentoxide nanotubes fiber of preparation is added to be contained in stearic deionized water solution in right amount, so
After aniline monomer is added, and stir evenly, make aniline monomer uniform fold in the Vanadium pentoxide nanotubes fiber surface, most
The FeCl of a concentration of 0.8mol/L is added afterwards3Aqueous solution reacts under stirring, and after reacting 1h, filtering and cleaning are gathered
Aniline/Vanadium pentoxide nanotubes composite gas sensitive material.Vanadium pentoxide nanotubes fiber, surfactant, aniline list
Body, FeCl3The mass ratio of aqueous solution is 10:0.1:5：2.
The sensitivity of the gas sensitive material of ammonia detection in the present embodiment is surveyed using intelligent air-sensitive analysis system
Examination, test temperature are（25±2）DEG C, relative humidity is（50 ± 2）%, response are defined as R=Rg/Ra, and Ra is gas
The aerial resistance of body sensitive material, Rg are that gas sensitive material is tested the resistance in gas in respective concentration.Test result
As shown in table 2.
Comparative example 1
Thickness is 20 micron conductive polymer polyanaline films.According to the test method in embodiment 1-5 to the sensing in comparative example 1
Material is tested, and test result is as shown in table 2.
Comparative example 2
Preparation grain size is 20nm vanadic anhydride nano-particles；Appropriate amount of deionized water solution is added in vanadic anhydride nano-particle
In, aniline monomer is then added, and stir evenly, makes aniline monomer uniform fold in the vanadic anhydride nanoparticle sublist
Face is eventually adding the FeCl of a concentration of 0.8mol/L3Aqueous solution reacts under stirring, after reacting 5h, filtering and cleaning,
Obtain polyaniline/vanadic anhydride Nanocomposites gas sensitive material.Vanadic anhydride nanoparticle, aniline monomer,
FeCl3The mass ratio of aqueous solution is 10:5：2.
The composite sensing material in comparative example 2 is tested according to the test method in embodiment 1-5, test result is such as
Shown in table 2.
For preferably qualitative relatively performance, gas sensitive material equivalent is filled for gas detection using under equal conditions
It sets, analyzes its sensitivity response value.
Table 2
Claims (8)
1. a kind of preparation method of gas sensitive material for environmental monitoring ammonia emission, which is characterized in that specific preparation side
Method is：
（1）It is 3-4 in mass ratio：6-7 weighs polyethylene pyrrole network alkanone and absolute ethyl alcohol, and the polyethylene pyrrole network alkanone is added
In the absolute ethyl alcohol, solution A is at the uniform velocity stirred to get；
（2）It is 1-2 in mass ratio：8-9 weighs soluble vanadic salts and n,N-Dimethylformamide, and the soluble vanadic salts is added
Into the n,N-Dimethylformamide, by the uniform velocity stirring, solution B is obtained；
（3）It is 1-3 by volume ratio:The solution A and solution B of 2-4 mixes, and the solution A is poured into the solution B, is added
Salpeter solution simultaneously stirs, and obtains the precursor solution of vanadic anhydride；
（4）Electrospinning device is added in the precursor solution of vanadic anhydride, by electrostatic spinning process, waits for that solvent volatilizees
Afterwards, composite nano fiber is obtained, then the composite nano fiber is subjected to calcination processing in air atmosphere, obtains five oxidations two
Vanadium nanotube fibers；
（5）By step（4）The deionized water solution containing surfactant in right amount is added in the Vanadium pentoxide nanotubes fiber of preparation
In, aniline monomer is then added, and stir evenly, makes aniline monomer uniform fold in the Vanadium pentoxide nanotubes fiber table
Face is eventually adding FeCl3Aqueous solution reacts under stirring, and after reacting 1-5h, filtering and cleaning obtain the oxygen of polyaniline/five
Change two vanadium nanotube composite gas sensitive materials.
2. a kind of preparation method of gas sensitive material for environmental monitoring ammonia emission according to claim 1,
It is characterized in that, step（1）And step（2）In the speed at the uniform velocity stirred be 50-200rpm.
3. a kind of preparation method of gas sensitive material for environmental monitoring ammonia emission according to claim 1,
It is characterized in that, step（3）Described in salpeter solution a concentration of 0.5-1.3mol/L；Addition is solution A and solution B gross mass
2%.
4. a kind of preparation method of gas sensitive material for environmental monitoring ammonia emission according to claim 1,
It is characterized in that, step（4）Described in electrostatic spinning process the use of air pump fltting speed is 0.1-0.5mL/min, spinning voltage is
40-60kV, it is 20-50cm to collect distance.
5. a kind of preparation method of gas sensitive material for environmental monitoring ammonia emission according to claim 1,
It is characterized in that, the calcination processing is under atmospheric pressure, using cooled to room temperature after calcining 2-10h at 600-800 DEG C.
6. a kind of preparation method of gas sensitive material for environmental monitoring ammonia emission according to claim 1,
It is characterized in that, step（5）Described in FeCl3A concentration of 0.8-2.1mol/L of aqueous solution.
7. a kind of preparation method of gas sensitive material for environmental monitoring ammonia emission according to claim 1,
It is characterized in that, step（5）Middle Vanadium pentoxide nanotubes fiber, surfactant, aniline monomer, FeCl3The quality of aqueous solution
Than being 10:0.1:5：2.
8. a kind of gas sensitive material for environmental monitoring ammonia emission, which is characterized in that by any one of claim 1-7 institutes
The method of stating is prepared.
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| CN201810833895.5A Pending CN108776158A (en) | 2018-07-26 | 2018-07-26 | A kind of gas sensitive material and preparation method for environmental monitoring ammonia emission |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115041149A (en) * | 2022-06-20 | 2022-09-13 | 扬州工业职业技术学院 | Composite material for efficiently adsorbing ammonia |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104458826A (en) * | 2014-10-28 | 2015-03-25 | 大连理工大学 | Novel ammonia sensor and preparation technology thereof |
| JP2016200547A (en) * | 2015-04-14 | 2016-12-01 | 富士電機株式会社 | Gas sensor and gas detector |
| CN106501322A (en) * | 2016-10-28 | 2017-03-15 | 中国石油大学(华东) | One kind is based on nanometer grid structure V2O5Gas sensor of thin film and preparation method thereof |
| CN107219269A (en) * | 2017-04-26 | 2017-09-29 | 北京科技大学 | With ammonia gas sensor at room temperature and preparation method thereof |
| CN107764871A (en) * | 2017-01-11 | 2018-03-06 | 郑州大学 | To NOXPPy/SnO with high selectivity2Nanotube composite air-sensitive material |
-
2018
- 2018-07-26 CN CN201810833895.5A patent/CN108776158A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104458826A (en) * | 2014-10-28 | 2015-03-25 | 大连理工大学 | Novel ammonia sensor and preparation technology thereof |
| JP2016200547A (en) * | 2015-04-14 | 2016-12-01 | 富士電機株式会社 | Gas sensor and gas detector |
| CN106501322A (en) * | 2016-10-28 | 2017-03-15 | 中国石油大学(华东) | One kind is based on nanometer grid structure V2O5Gas sensor of thin film and preparation method thereof |
| CN107764871A (en) * | 2017-01-11 | 2018-03-06 | 郑州大学 | To NOXPPy/SnO with high selectivity2Nanotube composite air-sensitive material |
| CN107219269A (en) * | 2017-04-26 | 2017-09-29 | 北京科技大学 | With ammonia gas sensor at room temperature and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| MUDASSIR HASAN 等: "Ammonia sensing and DC electrical conductivity studies of p-toluene sulfonic acid doped cetyltrimethylammonium bromide assisted V2O5@polyaniline composite nanofibers", 《JOURNAL OF INDUSTRIAL AND ENGINEERING CHEMISTRY》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115041149A (en) * | 2022-06-20 | 2022-09-13 | 扬州工业职业技术学院 | Composite material for efficiently adsorbing ammonia |
| CN115041149B (en) * | 2022-06-20 | 2023-08-25 | 扬州工业职业技术学院 | Composite material for efficiently adsorbing ammonia gas |
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