CN101706485A - Doped nano sensitive material for monitoring benzene - Google Patents
Doped nano sensitive material for monitoring benzene Download PDFInfo
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- CN101706485A CN101706485A CN 200910223546 CN200910223546A CN101706485A CN 101706485 A CN101706485 A CN 101706485A CN 200910223546 CN200910223546 CN 200910223546 CN 200910223546 A CN200910223546 A CN 200910223546A CN 101706485 A CN101706485 A CN 101706485A
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Abstract
The invention relates to a doped nano sensitive material for monitoring benzene, which is characterized in that: the doped nano sensitive material consists of Ag atom-doped TiO2, Fe2O3 and Al2O3 powder, wherein the content ranges of the components are that: the content range of Ag is 10 to 12 percent, the content range of TiO2 is 30 to 40 percent, the content range of Fe2O3 is 25 to 35 percent, and the content range of Al2O3 is 15 to 25 percent; and the grain diameter is less than 30nm. Benzene sensors prepared from the sensitive material provided by the invention have wide linear range, good selectivity and high sensitivity, can monitor micro benzene in the air on line, and are not influenced by coexisting substances.
Description
Technical field
The present invention relates to a kind of dopen Nano sensitive material for the monitoring benzene homologues, the TiO that is especially mixed up by the Ag atom
2, Fe
2O
3And Al
2O
3The sensitive material that nano-powder forms belongs to field of sensing technologies.
Background technology
The benzene series thing generally is meant volatile organic compounds such as benzene, toluene, ethylbenzene, dimethylbenzene (adjacent, and contraposition), isopropyl benzene and styrene, the most common with benzene, toluene and (adjacent, and contraposition) dimethylbenzene especially in the air, the benzene series thing is defined as strong carcinogen by the World Health Organization (WHO).Airborne benzene series owner will derive from building coating, paint for decoration, adhesive solvent and vehicle exhaust etc.The benzene series thing is one of major pollutants in the room air, and health is had very big threat.It mainly is that skin, eyes and the upper respiratory tract are had spread effect that chronic benzene homologues is poisoned; Frequent Benzene Exposure, skin can be because of degreasing desiccation furfur, the appearance allergic eczema that has; The long-term benzene homologues that sucks can cause alpastic anemia; As seen, setting up Minim Benzene in Gas Phase is that the rapid analysis of thing has very strong realistic meaning.
Determination methods for benzene compounds mainly contains vapor-phase chromatography, infra-red sepectrometry, gas chromatography mass spectrometry method and spectrophotometric method etc., because these methods all need preconcentration and suitable processing to finish mensuration by large-sized analytic instrument, therefore length consuming time is difficult for on-the-spot the realization.The inventor uses nanosized copper ferromanganese (atomic ratio 4: 3: the 1) composite oxides can online detection 1~80mg/m as sensitive material in the paper of delivering on " assay office " in 2006 that is entitled as " nano composite material catalytic luminescence method is measured airborne benzene series thing "
3The benzene series thing, detection limit can reach 0.5mg/m
3But formaldehyde, methyl alcohol, ethanol and acetone have certain interference to Determination of benzene hydrocarbon, show that the selectivity of sensitive material has much room for improvement.
Summary of the invention
The objective of the invention is to overcome the deficiency of conventional art, provide that a kind of range of linearity is wideer, detection limit is lower, selectivity is better monitored dopen Nano sensitive material of benzene series thing and preparation method thereof.The sensor of the monitoring benzene homologues of making of this sensitive material can be at the scene fast, the airborne micro-benzene homologues of Accurate Determining and be not subjected to the interference of other concurrent.
Dopen Nano sensitive material of the present invention is the TiO that is mixed up by the Ag atom
2, Fe
2O
3And Al
2O
3Nano-powder forms, and its preparation method is:
(1) an amount of butyl titanate is added in the absolute ethyl alcohol, stir, make butyl titanate-alcohol mixed solution, under the high-speed stirred condition, add the aqueous solution of molysite and aluminum contained compound, continue to stir, still aging, make transparent faint yellow colloidal sol;
(2) pretreated active carbon is immersed in the above-mentioned colloidal sol that configures, vibration leaches active carbon and places drying box to dry till do not have bubble and occur, and puts into muffle furnace heat treatment after fully grinding, and obtains TiO
2, Fe
2O
3And Al
2O
3Nano-powder;
(3) an amount of silver nitrate and glucose is soluble in water, under constantly stirring, the above-mentioned nano-powder that ultrasonic wave was disperseed adds wherein, continue to mix, directly place drying box to dry, 160~200 ℃ of lower heat reductions 5~10 minutes, namely get the TiO that the Ag atom mixes up
2, Fe
2O
3And Al
2O
3Nano-powder.
Wherein, the molysite that uses in the step (1) can be inorganic molysites such as iron chloride, ferric perchlorate, iron sulfate, ferric nitrate, aluminum contained compound can be inorganic molysite and organo-aluminum compound. will heat reduction temperature in the step (3) and be controlled at 160~200 ℃, can guarantee that silver ion can be by the glucose fast restore when this temperature and not oxidized.
When the particle diameter of nanometer powder that makes is no more than 30nm, and each component satisfies Ag (10-12%), TiO
2(30-40%), Fe
2O
3(25-35%) and Al
2O
3In the time of (15-25%), be used for having very high sensitivity and selective as the sensitive material of monitoring benzene homologues.
Embodiment
Embodiment 1
(1) under the room temperature, the 20g butyl titanate is added in the 50mL absolute ethyl alcohol, stir, make butyl titanate-alcohol mixed solution, under the high-speed stirred condition, add 28mL1.6mol/LFe (NO
3)
3The aqueous solution continues to stir 30min, and still aging 6h makes transparent faint yellow A colloidal sol; In the deionized water with 30mL80 ℃ of 10g aluminium isopropoxide adding, adding 2mL concentration behind the hydrolysis 1h is the HNO of 2mol/L
3Solution in 80 ℃ of lower 3h that stir, forms transparent B colloidal sol; Under the high-speed stirred A colloidal sol is added in the B colloidal sol, continue to stir 3h, obtain uniform mixed sols;
(2) active carbon that 10g is pretreated immerses in the above-mentioned mixed sols that configures, and vibration leaches active carbon and places 80 ℃ of drying boxes to dry till do not have bubble and occur, and after fully grinding, puts into 460 ℃ of muffle furnace roasting 4h, obtains TiO
2, Fe
2O
3And Al
2O
3Nano-powder;
(3) 10g silver nitrate and 10g glucose are dissolved in the 100ml deionized water, under constantly stirring, the above-mentioned nano-powder that ultrasonic dispersing is crossed adds wherein, continue to mix, directly place drying box to dry, heated 6 minutes down, promptly get powder body material at 180 ℃.
Analyze: with this powder body material of transmissioning electric mirror test, its maximum particle diameter is no more than 20nm, and average grain diameter is about 15nm; It is carried out constituent analysis, record and consist of 11.8%Ag, 38.4%TiO
2, 29.7%Fe
2O
3And 20.1%Al
2O
3
Use: measure airborne benzene homologues with this powder body material as sensitive material, the range of linearity 0.5~150mg/m
3, detection limit can reach 0.1mg/m
3, concurrent does not disturb.
Embodiment 2
(1) under the room temperature, the 20g butyl titanate is added in the 50ml absolute ethyl alcohol, stir, make titanium-alcohol mixed solution, under the high-speed stirred condition, slowly add and contain 1.6mol/L FeCl
3With 1.8mol/L Al (NO
3)
3Aqueous solution 30ml continues to stir 20min, and still aging 7h makes transparent faint yellow colloidal sol;
(2) active carbon that 10g is pretreated immerses in the above-mentioned mixed sols that configures, and vibration leaches active carbon and places 80 ℃ of drying boxes to dry till do not have bubble and occur, and after fully grinding, puts into 480 ℃ of muffle furnace roasting 3h, obtains TiO
2, Fe
2O
3And Al
2O
3Nano-powder;
(3) 10g silver nitrate and 10g glucose are dissolved in the 100ml pure water, under constantly stirring, the above-mentioned nano-powder that ultrasonic dispersing is crossed all adds wherein, continue to mix, directly place drying box to dry, heated 6 minutes down, promptly get powder body material at 190 ℃.
Analyze: with this powder body material of transmissioning electric mirror test, its maximum particle diameter is no more than 30nm, and average grain diameter is about 20nm; It is carried out constituent analysis, record and consist of 10.1%Ag, 35.4%TiO
2, 32.1%Fe
2O
3And 22.3%Al
2O
3
Use: measure airborne benzene homologues with this powder body material as sensitive material, the range of linearity 1~130mg/m
3, detection limit can reach 0.3mg/m
3, concurrent does not disturb.
Claims (3)
1. a dopen Nano sensitive material of monitoring benzene homologues is characterized in that the TiO that is mixed up by the Ag atom
2, Fe
2O
3And Al
2O
3Nano-powder forms, and wherein each constituent content is Ag (10-12%), TiO
2(30-40%), Fe
2O
3(25-35%) and Al
2O
3(15-25%), its preparation method is:
(1) an amount of butyl titanate is added in the absolute ethyl alcohol, stir, make butyl titanate-alcohol mixed solution, under the high-speed stirred condition, add the aqueous solution of molysite and aluminum contained compound, continue to stir, still aging, make transparent faint yellow colloidal sol;
(2) an amount of active carbon is immersed in the above-mentioned colloidal sol that configures, vibration leaches active carbon and places drying box to dry till do not have bubble and occur, and puts into muffle furnace heat treatment after fully grinding, and obtains TiO
2, Fe
2O
3And Al
2O
3Nano-powder;
(3) an amount of silver nitrate and glucose is soluble in water, under constantly stirring, the above-mentioned nano-powder that ultrasonic wave was disperseed adds wherein, continue to mix, directly place drying box to dry, 160~200 ℃ of lower heating 5~10 minutes, namely get the TiO that the Ag atom mixes up
2, Fe
2O
3And Al
2O
3Nano sensitive material.
2. a kind of dopen Nano sensitive material of monitoring the benzene series thing according to claim 1, it is characterized in that described molysite can be inorganic molysites such as iron chloride, ferric perchlorate, iron sulfate, ferric nitrate, aluminum contained compound can be inorganic molysite and organo-aluminum compound.
3. a kind of dopen Nano sensitive material of monitoring the benzene series thing according to claim 1, the particle diameter that it is characterized in that described nano sensitive material is less than 30nm.
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CN101706485A true CN101706485A (en) | 2010-05-12 |
CN101706485B CN101706485B (en) | 2013-06-26 |
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