CN101706485B - Doped nano sensitive material for monitoring benzene - Google Patents
Doped nano sensitive material for monitoring benzene Download PDFInfo
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- CN101706485B CN101706485B CN 200910223546 CN200910223546A CN101706485B CN 101706485 B CN101706485 B CN 101706485B CN 200910223546 CN200910223546 CN 200910223546 CN 200910223546 A CN200910223546 A CN 200910223546A CN 101706485 B CN101706485 B CN 101706485B
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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
Benzene homologues generally refers to the volatile organic compounds such as benzene, toluene, ethylbenzene, dimethylbenzene (adjacent, and contraposition), isopropyl benzene and styrene, especially common with benzene, toluene and (adjacent, and contraposition) dimethylbenzene in air, benzene homologues is defined as strong carcinogen by the World Health Organization (WHO).Airborne benzene homologues is mainly derived from building coating, paint for decoration, adhesive solvent and vehicle exhaust etc.Benzene homologues is one of major pollutants in room air, and health is had very large threat.Chronic benzene homologues is poisoning is mainly that skin, eyes and the upper respiratory tract are had spread effect; Frequent Benzene Exposure, skin can be because of degreasing desiccation furfur, some appearance allergic eczemas; The long-term benzene homologues that sucks can cause alpastic anemia; As seen, set up the express-analysis that is thing to Minim Benzene in Gas Phase and have very strong realistic meaning.
The assay method of benzene homologues mainly contains vapor-phase chromatography, infra-red sepectrometry, gas chromatography mass spectrometry method and spectrophotometric method etc., could complete mensuration by large-sized analytic instrument because these methods all need preconcentration and suitable processing, therefore length consuming time is difficult for on-the-spot the realization.The inventor uses nanosized copper ferromanganese (atomic ratio 4: 3: 1) composite oxides can detect online 1～80mg/m as sensitive material in the paper that is entitled as " nano composite material catalytic luminescence method is measured airborne benzene homologues " of delivering on " assay office " in 2006
3Benzene homologues, detection limit can reach 0.5mg/m
3But formaldehyde, methyl alcohol, ethanol and acetone have certain interference to the mensuration of benzene homologues, 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 wider, detection limit is lower, selectivity is better monitored dopen Nano sensitive material of benzene homologues 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) appropriate butyl titanate is added in 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 activated charcoal is immersed in the above-mentioned colloidal sol that configures, vibration leaches activated charcoal and is placed in drying box and dry to without till the bubble appearance, puts into muffle furnace thermal treatment after fully grinding, and obtains TiO
2, Fe
2O
3And Al
2O
3Nano-powder;
(3) appropriate silver nitrate and glucose is soluble in water, under constantly stirring, the above-mentioned nano-powder that ultrasound wave was disperseed adds wherein, continue to mix, directly be placed in drying box and 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 step (1) can be the inorganic molysites such as iron chloride, ferric perchlorate, iron sulfate, ferric nitrate, and aluminum contained compound can be inorganic molysite and organo-aluminum compound.In step (3), the heat reduction temperature is controlled at 160～200 ℃, can guarantees 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 selectivity as the sensitive material of monitoring benzene homologues.
Embodiment
Embodiment 1
(1) under 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)
3Aqueous solution continues to stir 30min, and still aging 6h makes transparent faint yellow A colloidal sol; The 10g aluminium isopropoxide is added in the deionized water of 30mL80 ℃, adding 2mL concentration after hydrolysis 1h is the HNO of 2mol/L
3Solution stirs 3h under 80 ℃, form transparent B colloidal sol; Under high-speed stirred, A colloidal sol is added in B colloidal sol, continue to stir 3h, obtain uniform mixed sols;
(2) activated charcoal that 10g is pretreated immerses in the above-mentioned mixed sols that configures, and vibration leaches activated charcoal and is placed in 80 ℃ of drying boxes and dry to without till the bubble appearance, 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 ultrasound wave was disperseed adds wherein, continue to mix, directly be placed in drying box and dry, heating is 6 minutes under 180 ℃, namely gets powder body material.
Analyze: with this powder body material of transmissioning electric mirror test, its maximum particle diameter is no more than 20nm, and mean grain size 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, the range of linearity 0.5～150mg/m with this powder body material as sensitive material
3, detection limit can reach 0.1mg/m
3, concurrent does not disturb.
Embodiment 2
(1) under 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) activated charcoal that 10g is pretreated immerses in the above-mentioned mixed sols that configures, and vibration leaches activated charcoal and is placed in 80 ℃ of drying boxes and dry to without till the bubble appearance, 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 ultrasound wave was disperseed all adds wherein, continue to mix, directly be placed in drying box and dry, heating is 6 minutes under 190 ℃, namely gets powder body material.
Analyze: with this powder body material of transmissioning electric mirror test, its maximum particle diameter is no more than 30nm, and mean grain size 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, the range of linearity 1～130mg/m with this powder body material as sensitive material
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 component concentration is 10-12%Ag, 30-40%TiO
2, 25-35%Fe
2O
3And 15-25%Al
2O
3, its preparation method is:
(1) appropriate butyl titanate is added in 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) appropriate activated charcoal is immersed in the above-mentioned colloidal sol that configures, vibration leaches activated charcoal and is placed in drying box and dry to without till the bubble appearance, puts into muffle furnace thermal treatment after fully grinding, and obtains TiO
2, Fe
2O
3And Al
2O
3Nano-powder;
(3) appropriate silver nitrate and glucose is soluble in water, under constantly stirring, the above-mentioned nano-powder that ultrasound wave was disperseed adds wherein, continue to mix, directly be placed in drying box and dry, heated under 160～200 ℃ 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 benzene homologues according to claim 1, is characterized in that described molysite is iron chloride, ferric perchlorate, iron sulfate and ferric nitrate, and aluminum contained compound is inorganic aluminate and organo-aluminum compound.
3. a kind of dopen Nano sensitive material of monitoring benzene homologues according to claim 1, is characterized in that the particle diameter of described nano sensitive material is less than 30nm.
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|---|---|---|---|
| CN 200910223546 CN101706485B (en) | 2009-11-23 | 2009-11-23 | Doped nano sensitive material for monitoring benzene |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200910223546 CN101706485B (en) | 2009-11-23 | 2009-11-23 | Doped nano sensitive material for monitoring benzene |
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| Publication Number | Publication Date |
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| CN101706485A CN101706485A (en) | 2010-05-12 |
| CN101706485B true CN101706485B (en) | 2013-06-26 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103969249A (en) * | 2014-04-14 | 2014-08-06 | 北京联合大学生物化学工程学院 | Composite oxide sensitive material used for monitoring formaldehyde and ammonia simultaneously |
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| CN101887057B (en) * | 2010-06-30 | 2013-04-24 | 北京联合大学生物化学工程学院 | Nano sensitive material of carbamic acid ester pesticides |
| CN102879521B (en) * | 2011-07-11 | 2014-10-22 | 北京联合大学生物化学工程学院 | Nano-sensitive material for monitoring hexachlorocyclohexanes |
| CN102809554B (en) * | 2011-11-08 | 2015-08-12 | 北京联合大学生物化学工程学院 | The nano sensitive material of biconjugate chlorphenyl trichloroethanes agricultural chemicals |
| CN102809555B (en) * | 2012-01-18 | 2015-08-12 | 北京联合大学生物化学工程学院 | A kind of nano sensitive material of monitoring carbon monoxide |
| CN102809557B (en) * | 2012-01-18 | 2015-01-28 | 北京联合大学生物化学工程学院 | Nanometer sensitive material for detecting hydrogen sulfide |
| CN102809628B (en) * | 2012-05-29 | 2014-10-22 | 北京联合大学生物化学工程学院 | Nano-sensitive material for trimethylamine |
| CN103275709B (en) * | 2013-03-29 | 2014-10-22 | 北京联合大学生物化学工程学院 | Catalysis sensitive material of acetaldehyde |
| CN103792227B (en) * | 2014-01-22 | 2017-02-15 | 北京联合大学生物化学工程学院 | Nano composite oxide sensitive material for formaldehyde and benzene |
| CN104849402B (en) * | 2015-04-20 | 2016-11-23 | 北京联合大学 | A kind of cross sensitivity material of benzene, toluene and ethylbenzene |
| CN104897845B (en) * | 2015-06-23 | 2017-01-11 | 北京联合大学 | catalytic oxidation catalyst of formaldehyde, methanol and ethanol |
| CN107021730A (en) * | 2017-03-24 | 2017-08-08 | 合肥羿振电力设备有限公司 | A kind of benzene homologues sensitive resistance material and preparation method thereof |
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| CN103969249B (en) * | 2014-04-14 | 2016-07-13 | 北京联合大学生物化学工程学院 | For monitoring the composite oxides sensitive material of formaldehyde and ammonia simultaneously |
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| CN101706485A (en) | 2010-05-12 |
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