CN106018700A - Gas-sensitive material capable of being used for detecting multiple volatile organic compounds simultaneously as well as preparation method and application of gas-sensitive material - Google Patents
Gas-sensitive material capable of being used for detecting multiple volatile organic compounds simultaneously as well as preparation method and application of gas-sensitive material Download PDFInfo
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- CN106018700A CN106018700A CN201610471019.3A CN201610471019A CN106018700A CN 106018700 A CN106018700 A CN 106018700A CN 201610471019 A CN201610471019 A CN 201610471019A CN 106018700 A CN106018700 A CN 106018700A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/0004—Gaseous mixtures, e.g. polluted air
- G01N33/0009—General constructional details of gas analysers, e.g. portable test equipment
- G01N33/0027—General constructional details of gas analysers, e.g. portable test equipment concerning the detector
- G01N33/0031—General constructional details of gas analysers, e.g. portable test equipment concerning the detector comprising two or more sensors, e.g. a sensor array
Abstract
The invention discloses a gas-sensitive material capable of being used for detecting multiple volatile organic compounds simultaneously as well as a preparation method and an application of the gas-sensitive material. The gas-sensitive material capable of being used for detecting the multiple volatile organic compounds simultaneously is prepared from raw materials including Ag-LaFeO3 gel, template molecules, functional monomers and an initiator in the mass ratio being 1: (0.05-0.5): (0.01-0.5): (0.05-0.4). The preparation method comprises steps including solution mixing, microwave reaction, ultrasonic vibration, microwave synthesis, drying, grinding, sintering and the like. The application refers to an application of the gas-sensitive material capable of being used for detecting the multiple volatile organic compounds simultaneously in preparation of a gas sensor or a gas-sensitive tester for detecting the multiple volatile organic compounds simultaneously. On the basis of provided raw materials and matching ratios, the method for preparing the material sensitive to different volatile organic compounds, and the gas-sensitive tester capable of detecting the multiple volatile organic compounds simultaneously is obtained.
Description
Technical field
The invention belongs to field of material technology, be specifically related to one and can be used for detecting multiple VOC (volatile organic simultaneously
Compounds, VOCs) gas sensitive and preparation method and application.
Background technology
In recent years, along with the fast development of China's economy, particularly growth in the living standard, and the high speed development of the indoor decorating industry thus brought, building materials, decorations the pollution caused has become the main source of indoor environmental pollution.In addition in order to energy-conservation, building structure is generally of good sealing function, more exacerbates the deterioration of IAQ (indoor air quality).During at present indoor formaldehyde, benzene and benzene homologues, ammonia and radioactivity four are polluted greatly, harm is maximum, be most difficult to radical cure is formaldehyde pollution and benzene pollution.Secondly the room air of some laboratorys and factory there is also some harmful volatile organic matters.Acetone and methanol are two kinds of solvents that laboratory is conventional, and acetone still for cleaning effective cleaning agent of some glass apparatus, can be widely used at laboratory and some factories.But acetone and methanol are harmful to human body, methanol have harm, new research to show the blood system of human body and nervous system it also has harm to optic nerve and retina；And central nervous system is mainly had suppression, anesthetic action, high concentration contact existing liver, kidney and pancreas may be had infringement by acetone.To in the detection of the exhaled gas that the detection of acetone can also be applied to people to judge whether this people suffers from diabetes.To detect a kind of specific gas at present and need a kind of specific material, but some material is not preferable gas sensitive, during application, performance is not the most preferable.Therefore, develop a kind of gas sensitive that can solve above-mentioned technical problem to be very important.
Summary of the invention
The first object of the present invention is to provide a kind of gas sensitive that can be used for simultaneously detecting multiple VOC；Second purpose is to provide the described preparation method that can be used for simultaneously detecting the gas sensitive of multiple VOC；3rd purpose is to provide the described application that can be used for simultaneously detecting the gas sensitive of multiple VOC.
The first object of the present invention is achieved in that the described gas sensitive that can be used for simultaneously detecting multiple VOC includes raw material A g-LaFeO3(Ag doping cadmium ferrite) gel, template molecule, function monomer, initiator, through preparing, its material molar ratio is 1:(0.05～0.5): (0.01～0.5): (0.05～0.4).
The second object of the present invention is achieved in that and comprises the following steps:
A, by sonic oscillation after the template molecule of formulation ratio and function monomer mixing, stand 5 ~ 20h and obtain solution a；
B, by the gel of formulation ratio and solution a mix homogeneously, add the initiator of formulation ratio, at 40 ~ 100 DEG C, polyreaction 12 ~ 48h obtains reactant liquor b；
C, reactant liquor b is dried to moisture content be 2 ~ 7%, grind, sintering obtain object；
D, the object gas sensitive obtained is coated on the most etched ITO, forms gas sensor array.
The third object of the present invention is achieved in that and described can be used for the gas sensitive simultaneously detecting multiple VOC application in preparation detects the gas sensor of multiple VOC or air-sensitive tester simultaneously.
The present invention also can be used in the identification of organic molecule by the molecular imprinting of separation and identification that discovery is originally used for macromole.Molecular imprinting has structure effect precordainment, and can build only site to target molecule specific identification, these sites and target molecule according to target molecule to be identified is complementary at aspects such as structure, shape, size, functional groups.So, we may be selected by a kind of preferably gas sensitive, regulates its selectivity to variety classes gas by molecular imprinting, just can apply it to different fields.
In numerous metal-oxide semiconductor (MOS)s, perovskite ABO3Type LaFeO3Good conductivity, Heat stability is good, prepare simple, preparation cost is low is considered as a kind of potential gas sensitive, uses Ag+Its doping is replaced the La of A position3+After can reduce the material of material further, certain space has also been vacateed for adsorbed gas in the room that doping introduces, the beneficially raising of air-sensitive performance.Reported in literature shows, LaFeO3Air-sensitive performance relatively ZnO, SnO2、In2O3Good many Deng single oxide.Therefore the present invention selects Ag-LaFeO3This preferable gas sensitive is modified further, uses molecular imprinting to be adjusted its selectivity so that it is can be applied in the detection of more toxic and harmful.The present invention is respectively adopted acetone, benzene, methanol and formaldehyde as template molecule, has selected corresponding function monomer, has prepared Ag-LaFeO3Benzylacetone gas sensitive, Ag-LaFeO3Base benzene gas sensitive, Ag-LaFeO3Base methanol gas sensitive, Ag-LaFeO3Base formaldehyde gas sensitive material.Subsequently, several or four kinds of materials in four kinds of materials are made sensor array, can realize detecting to acetone, benzene, methanol and four kinds of gases of formaldehyde or to while wherein combination in any.
Owing to sensor sensing material shows instability under the influence of extraneous factor such as temperature, chemical reagent, and lack suitable target induction substance in some conditions.Utilize molecular imprinting, can synthesize stable, certain material is had the material of special role, by these materials application to sensing technology, can be made up these not enough.
Owing to molecular imprinting has the structure effect feature such as precordainment, specific recognition, in catalysis, separate and the field such as analysis is paid close attention to, but its application at present is mainly on organic macromolecule identification and separating, the molecular imprinting method recognition detection of organic molecule gas such as acetone, benzene etc. be there is no to product and the report of this aspect.
First the present invention is to provide preparation Ag-LaFeO3The raw material of base molecularly imprinted polymer and proportioning, and provide one to prepare Ag-LaFeO based on the raw material provided and proportioning3Base molecularly imprinted polymer acetone, benzene, methanol and the method for formaldehyde gas sensitive material, and provide a kind of method that four kinds of gas sensitives are fabricated to gas sensor array, thus obtain can the gas sensitive simultaneously detecting multiple VOC and preparation method thereof.
Sensor prepared by the gas sensitive that can simultaneously detect multiple VOC that the present invention provides has the positive effect that:
(1) detect multiple VOCs: can the combination of four kind gases whole to acetone, benzene, methanol and formaldehyde or wherein any kind detect simultaneously simultaneously.
(2) sensitivity to acetone, benzene, methanol and formaldehyde gas is the highest: the Ag-LaFeO prepared by molecular imprinting regulation selectivity3Benzylacetone, benzene, methanol and formaldehyde gas sensitive material, can detect that 0.1ppm, 0.1ppm, 0.05ppm and the light concentration gas of 0.005 ppm respectively.
(3) selectivity is good: the Ag-LaFeO prepared by molecular imprinting regulation selectivity3Benzylacetone, benzene, methanol and formaldehyde gas sensitive material, to the sensitivity of acetone, benzene, methanol and formaldehyde gas under same concentrations far above to toluene or gasoline or water or the sensitivity of ammonia.
(4) the response-recovery time is fast: the Ag-LaFeO prepared by molecular imprinting regulation selectivity3Benzylacetone, benzene, methanol and formaldehyde gas sensitive material, be below 1 minute the response-recovery time of acetone, benzene, methanol and formaldehyde gas, is suitable for quickly checking formaldehyde gas.
To sum up, the Ag-LaFeO that the present invention is prepared by molecular imprinting regulation selectivity3Benzylacetone, benzene, methanol and the formaldehyde gas sensitive material sensitivity to acetone, benzene, methanol and formaldehyde gas, especially sensitivity and selectivity is all higher than the technical merit of currently known single-sensor, and have raising by a relatively large margin, can directly with its make that sensor array detects in acetone, benzene, methanol and formaldehyde simultaneously several or whole, or be respectively prepared acetone, benzene, methanol and formaldehyde gas sensor.
First the present invention is to provide raw material and the proportioning preparing the material sensitive to different volatile organic matters based on modified cadmium ferrite, and provide a kind of method preparing the material sensitive to different volatile organic matters based on the raw material provided and proportioning, it is thus achieved that a kind of air-sensitive tester that can simultaneously detect multiple volatile organic matter.
The air-sensitive tester detecting multiple volatile organic matter while gas sensitive of the present invention preparation includes several gas sensors, it is independent between each element, the detection of a kind of VOC is responsible for by each element, and different elements lines up array to realize detecting different VOCs simultaneously.Prepare the gas sensitive of different elements by Ag doping cadmium ferrite (Ag-LaFeO3) obtain after molecular imprinting modulation selectivity.
This air-sensitive tester can also react in same system by choosing various template molecule and corresponding function monomer simultaneously, is directly synthesized out and multiple gases is respectively provided with selective material.This kind of method this can be implemented so that by environmental demand to be measured, determines that several template molecule, every kind be selected template molecule and its corresponding function monomer react the most alone, after forming firm chemical bonded refractory therebetween and getting togather, is added simultaneously to Ag-LaFeO3In gel, under the conditions of uniform temperature, carry out polyreaction with gel so that the combination of each template-monomer and Ag-LaFeO3Gel mixes uniformly and is polymerized, afterwards by being dried by reactant liquor and heat treatment removal template molecule, only at Ag-LaFeO3In leave the site simultaneously having different templates Selective recognition, gas with various can be detected by the material being prepared out, and has preferable selectivity.
Accompanying drawing explanation
Fig. 1 is the sensitivity to variable concentrations acetone, benzene, methanol and formaldehyde gas of the sensor array prepared by the present invention；
In figure, abscissa is concentration of formaldehyde, and unit is ppm, and vertical coordinate is sensitivity；
Fig. 2 is the sensitivity to gas with various of the prepared sensor array；
In visible array, different units is to the sensitivity of acetone, benzene, methanol and formaldehyde far above the sensitivity to other gases, shows that the unit in sensor permutation concurrently and independently works and realizes detection while multiple gases；
Fig. 3 is prepared sensor array schematic diagram.
Detailed description of the invention
Below in conjunction with embodiment and accompanying drawing, the present invention is further illustrated, but is any limitation as the present invention never in any form, based on present invention teach that any conversion or replacement made, belongs to protection scope of the present invention.
The gas sensitive that can be used for simultaneously detecting multiple VOC of the present invention includes raw material A g-LaFeO3Gel, template molecule, function monomer, initiator, through preparing, its material molar ratio is 1:(0.05～0.5): (0.01～0.5): (0.05～0.4).
Described template molecule is acetone, benzene, formaldehyde, acetaldehyde or methanol.
Described function monomer is N,N methylene bis acrylamide, acrylic acid and derivant thereof, methylene-succinic acid, N-acryloyl group alanine, acrylamide, formaldehyde, methacrylic acid or vinylpyridine.
Described initiator is azodiisobutyronitrile or 2,2'-Azobis(2,4-dimethylvaleronitrile).
The preparation method that can be used for simultaneously detecting the gas sensitive of multiple VOC of the present invention, it is characterised in that comprise the following steps:
A, by sonic oscillation after the template molecule of formulation ratio and function monomer mixing, stand 5 ~ 20h and obtain solution a；
B, by the gel of formulation ratio and solution a mix homogeneously, add the initiator of formulation ratio, at 40 ~ 100 DEG C, polyreaction 12 ~ 48h obtains reactant liquor b；
C, reactant liquor b is dried to moisture content be 2 ~ 7%, grind, sintering obtain object；
D, the object gas sensitive obtained is coated on the most etched ITO, forms gas sensor array.
The frequency of the sonic oscillation described in step A is 10 ~ 40KHz, and the ultrasonic vibration time is 30 ~ 60min.
Dry described in step C is that reactant liquor b is dried at 50 ~ 250 DEG C 1 ~ 2d.
The granularity of the grinding described in step C is 40 ~ 100nm.
Sintering described in step C is sintering 2 ~ 4h at 600 ~ 900 DEG C.
The applying of gas sensitive that can be used for simultaneously detecting multiple VOC of the present invention can be used for the gas sensitive simultaneously detecting multiple VOC application in preparing the gas sensor or air-sensitive tester simultaneously detecting multiple VOC for described.
To be embodied as case, the present invention will be further described below:
Embodiment 1
Material composition is Ag-LaFeO3Gel, acetone, N,N methylene bis acrylamide and azodiisobutyronitrile mol ratio corresponding with this material composition is 1 0.05 0.1 0.1.
Take the Ag-LaFeO of 100mL 1mol/L3Gel, stand-by；Measure sonic oscillation 30min after acetone 50 μ L, N,N methylene bis acrylamide 100 μ L mixing, stand 8h；Afterwards and Ag-LaFeO3Gel mixes, and adds azodiisobutyronitrile 0.16g, polyreaction 12h at 60 DEG C, it is dried at 80 DEG C afterwards, grinds, and sinters 2h and obtain Ag-LaFeO at 700 DEG C3Base acetone sensitive material.
Embodiment 2
Material composition is Ag-LaFeO3Gel, benzene, formaldehyde and azodiisobutyronitrile mol ratio corresponding with this material composition is 1 0.06 0.36 0.1.
Take the Ag-LaFeO of 100mL 1mol/L3Gel, stand-by；Measure sonic oscillation 60min after benzene 50 μ L, formaldehyde 300 μ L mixing, stand 12h；Afterwards and Ag-LaFeO3Gel mixes, and adds azodiisobutyronitrile 0.16g, polyreaction 20h at 80 DEG C, it is dried at 80 DEG C afterwards, grinds, and sinters 2h and obtain Ag-LaFeO at 750 DEG C3Base benzene sensitive material.
Embodiment 3
Material composition is Ag-LaFeO3Gel, methanol, methacrylic acid and azodiisobutyronitrile mol ratio corresponding with this material composition is 1 0.1 0.4 0.1.
Take the Ag-LaFeO of 100mL 1mol/L3Gel, stand-by；Measure sonic oscillation 45min after methanol 100 μ L, methacrylic acid 400 μ L mixing, stand 8h；Afterwards and Ag-LaFeO3Gel mixes, and adds azodiisobutyronitrile 0.16g, polyreaction 24h at 75 DEG C, it is dried at 80 DEG C afterwards, grinds, and sinters 4h and obtain Ag-LaFeO at 850 DEG C3Base methanol sensitive material.
Embodiment 4
Material composition is Ag-LaFeO3Gel, formaldehyde, acrylamide and azodiisobutyronitrile mol ratio corresponding with this material composition is 1 0.1 0.5 0.1.
Take the Ag-LaFeO of 100mL 1mol/L3Gel, stand-by；Measure sonic oscillation 60min after formaldehyde 100 μ L, acrylamide 0.27g mixing, stand 12h；Afterwards and Ag-LaFeO3Gel mixes, and adds azodiisobutyronitrile 0.16g, polyreaction 15h at 80 DEG C, it is dried at 80 DEG C afterwards, grinds, and sinters 2h and obtain Ag-LaFeO at 800 DEG C3Base formaldehyde sensitive material.
Embodiment 5
The Ag-LaFeO that embodiment 1 ~ 4 is prepared3Base acetone sensitive material, Ag-LaFeO3Base benzene sensitive material, Ag-LaFeO3Base methanol sensitive material and Ag-LaFeO3Base formaldehyde sensitive material is coated on the most etched ITO, forms gas sensor array, with spun gold extraction electrode, to acetone, benzene, methanol and four kinds of gases of formaldehyde or can detect wherein combination in any simultaneously.
Embodiment 6
Material composition is Ag-LaFeO3Gel, formaldehyde, acrylamide, acetone, N,N methylene bis acrylamide and azodiisobutyronitrile mol ratio corresponding with this material composition is 1 0.1 0.5 0.1 0.2 0.1.
Take 200mL
The Ag-LaFeO of 1mol/L3Gel, stand-by；Measure formaldehyde 100 μ L and weigh sonic oscillation 60min after acrylamide 0.27g mixing；Similarly, measure sonic oscillation 60min after acetone 100 μ L, N,N methylene bis acrylamide 200 μ L mixing, stand 12h；Afterwards and Ag-LaFeO3Gel mixes, and adds azodiisobutyronitrile 0.32g, polyreaction 18h at 75 DEG C, it is dried at 80 DEG C afterwards, grinds, and sinters 4h and obtain based on Ag-LaFeO at 850 DEG C3While respond formaldehyde and the sensitive material of acetone.
Claims (10)
1. the gas sensitive that can be used for simultaneously detecting multiple VOC, it is characterised in that the described gas sensitive that can be used for simultaneously detecting multiple VOC includes raw material A g-LaFeO3Gel, template molecule, function monomer, initiator, through preparing, its material molar ratio is 1:(0.05～0.5): (0.01～0.5): (0.05～0.4).
The gas sensitive that can be used for simultaneously detecting multiple VOC the most according to claim 1, it is characterised in that described template molecule is acetone, benzene, formaldehyde, acetaldehyde or methanol.
The gas sensitive that can be used for simultaneously detecting multiple VOC the most according to claim 1; it is characterized in that described function monomer is N,N methylene bis acrylamide, acrylic acid and derivant thereof, methylene-succinic acid, N-acryloyl group alanine, acrylamide, formaldehyde, methacrylic acid or vinylpyridine.
The gas sensitive that can be used for simultaneously detecting multiple VOC the most according to claim 1, it is characterised in that described initiator is azodiisobutyronitrile or 2,2'-Azobis(2,4-dimethylvaleronitrile).
5. a claim 1 ~ 4 is arbitrary described can be used for detecting the preparation method of the gas sensitive of multiple VOC simultaneously, it is characterised in that comprise the following steps:
A, by sonic oscillation after the template molecule of formulation ratio and function monomer mixing, stand 5 ~ 20h and obtain solution a；
B, by the gel of formulation ratio and solution a mix homogeneously, add the initiator of formulation ratio, at 40 ~ 100 DEG C, polyreaction 12 ~ 48h obtains reactant liquor b；
C, reactant liquor b is dried to moisture content be 2 ~ 7%, grind, sintering obtain object；
D, the object gas sensitive obtained is coated on the most etched ITO, forms gas sensor array.
Preparation method the most according to claim 5, it is characterised in that the frequency of the sonic oscillation described in step A is 10 ~ 40KHz, the ultrasonic vibration time is 30 ~ 60min.
Preparation method the most according to claim 5, it is characterised in that dry described in step C is that reactant liquor b is dried at 50 ~ 250 DEG C 1 ~ 2d.
Preparation method the most according to claim 5, it is characterised in that the granularity of the grinding described in step C is 40 ~ 100nm.
Preparation method the most according to claim 5, it is characterised in that the sintering described in step C is sintering 2 ~ 4h at 600 ~ 900 DEG C.
10. a claim 1 ~ 4 is arbitrary described can be used for detecting the application of the gas sensitive of multiple VOC simultaneously, it is characterised in that described can be used for the gas sensitive simultaneously detecting multiple VOC application in preparation detects the gas sensor of multiple VOC or air-sensitive tester simultaneously.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106749809A (en) * | 2016-12-26 | 2017-05-31 | 云南大学 | A kind of high selectivity acetone air-sensitive material and preparation method and application |
| CN107121454A (en) * | 2017-04-17 | 2017-09-01 | 云南大学 | A kind of different element doping graphene quantum dots are respectively with molecular engram compound gas sensitive and preparation method and application |
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| CN105347403A (en) * | 2015-12-11 | 2016-02-24 | 云南大学 | High-selectivity formaldehyde gas-sensitive material and preparation method and application thereof |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105347403A (en) * | 2015-12-11 | 2016-02-24 | 云南大学 | High-selectivity formaldehyde gas-sensitive material and preparation method and application thereof |
Non-Patent Citations (1)
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| 林毓韬等: "Ａｇ－ＬａＦｅＯ３的制备及甲醛气敏性能研究", 《功能材料》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106749809A (en) * | 2016-12-26 | 2017-05-31 | 云南大学 | A kind of high selectivity acetone air-sensitive material and preparation method and application |
| CN107121454A (en) * | 2017-04-17 | 2017-09-01 | 云南大学 | A kind of different element doping graphene quantum dots are respectively with molecular engram compound gas sensitive and preparation method and application |
| CN107121454B (en) * | 2017-04-17 | 2019-08-30 | 云南大学 | A kind of difference element doping graphene quantum dot is respectively with molecular engram compound gas sensitive and the preparation method and application thereof |
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