CN103275709A - Catalysis sensitive material for monitoring acetaldehyde - Google Patents
Catalysis sensitive material for monitoring acetaldehyde Download PDFInfo
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- CN103275709A CN103275709A CN2013101226091A CN201310122609A CN103275709A CN 103275709 A CN103275709 A CN 103275709A CN 2013101226091 A CN2013101226091 A CN 2013101226091A CN 201310122609 A CN201310122609 A CN 201310122609A CN 103275709 A CN103275709 A CN 103275709A
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- acetaldehyde
- sensitive material
- titanium
- monitoring
- catalysis sensitive
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Abstract
The invention relates to a catalysis sensitive material for monitoring acetaldehyde. The catalysis sensitive material comprises, by weight, 25 to 40% of Al2O3, 35 to 50% of TiO2 and 10 to 25% of Fe2O3. A preparation method of the catalysis sensitive material comprises the following steps of co-dissolving Al, Ti and Fe salts having high water solubility in deionized water, slowly and dropwisely adding ammonia water into the mixture with stirring until precipitates disappear, and carrying out standing, aging, washing, drying, grinding and calcination to obtain the catalysis sensitive material for monitoring acetaldehyde. An acetaldehyde cataluminescence sensor prepared from the catalysis sensitive material has a wide linear range, good selectivity and high sensitivity, can monitor acetaldehyde content of air and is not influenced by concomitant materials.
Description
Technical field
The present invention relates to a kind of catalysis sensitive material for monitoring air acetaldehyde, especially by Al
2O
3, TiO
2And Fe
2O
3The complex metal oxides sensitive material of forming.Belong to field of sensing technologies.
Background technology
Acetaldehyde be a kind of volatile, irritating smell, colourless runny liquid are arranged, 20.8 ℃ of boiling points, relative density is less than 1.Water soluble, ethanol, ether, chloroform, acetone and benzene.Its steam and air can form explosive mixture, limits of explosion 4.0%～57.0% (volume).
Airborne lower concentration acetaldehyde can cause eye, nose and upper respiratory tract irritation and bronchitis, sucks high density acetaldehyde and can cause symptoms such as headache, drowsiness, clouded in mind, pulmonary edema and diarrhoea.Wrongly take that acetaldehyde can cause nausea, vomits, diarrhoea, the disturbance of consciousness, and liver, kidney and cardiac damage can appear.Skin contact acetaldehyde can cause irritant dermatitis.As seen, set up that the measuring method of acetaldehyde has certain realistic meaning in the air.
The method of measuring acetaldehyde in the document is a lot, but the method for measuring aldehyde in solution with chromatographic technique is in the majority, as: Wang Mengmeng etc. have delivered the article that is entitled as " content that the HPLC method is measured acetaldehyde in the rat plasma " at the 12nd phase in 2012 " pharmaceutical analysis magazine ", Yu Tao etc. have delivered the article that is entitled as " trace formaldehyde and acetaldehyde in the DNPH column front derivation high effective liquid chromatography for measuring beer " in the 8th phase in 2012 " Chinese sanitary inspection magazine ", Zou Yue etc. have delivered the article that is entitled as " the Ultra Performance Liquid Chromatography method is measured formaldehyde and the acetaldehyde in the cigarette wrapping paper " in the 5th phase in 2012 " Yunnan chemical ", Li Ruisheng etc. have delivered the article that is entitled as " acetaldehyde residual quantity in the medicinal polyester bottles of Headspace Gas Chromatography liquid oral " in the 29th phase in 2012 " China Dispensary ", Zhang Yuanyuans etc. have been delivered the article that is entitled as " the headspace sampling vapor-phase chromatography detects acetaldehyde in the beer " in the 9th phase in 2011 " assay office ", Lu Wenjuan etc. have delivered the article that is entitled as " acetaldehyde in purge and trap-gas chromatography determination water; propenal; vinyl cyanide " in the 10th phase in 2011 " physical and chemical inspection (chemical fascicle) ", and Lv Guibin etc. have delivered article that is entitled as " purge and trap-vapor-phase chromatography is measured the acetaldehyde in the water simultaneously; propenal and formaldehyde " etc. in the 6th phase in 2011 " Chinese environmental monitoring ".In addition, Lv Xiaohu etc. has delivered in the 8th phase in 1991 " SCI " and has been entitled as " Virahol-ClO
--H
2O
2Chemical luminous system is measured the research of trace acetaldehyde " article; Yao Gongan etc. have delivered the article that is entitled as " research that portable injection chemiluminescence is measured acetaldehyde " in the 6th phase in 2011 " assay office "; though these two pieces of articles are based on chemoluminescence method, also are the methods of mensuration aldehyde in solution.
When measuring airborne micro-acetaldehyde with above these methods, need at the scene with air sampler enrichment sampling, and then get back to laboratory dissolving wash-out and be prepared into liquid sample and measure.
Cao Xiaoan etc. have delivered the article that is entitled as " a kind of catalytic luminescence aldehydes gas sensor research based on the Strontium carbonate powder nano material " in the 12nd phase in 2004 " analytical chemistry ", have reported the method for acetaldehyde in a kind of direct mensuration air.They as sensitive material, carry out quantitative analysis at wavelength 425nm place with the Strontium carbonate powder nano material, and linearity range is 6～6000mg/m
3, detect and be limited to 2mg/m
3But ethanol and formaldehyde can cause 42.5% and 12.5% interference respectively.
Summary of the invention
The objective of the invention is to overcome the deficiency of conventional art, provide a kind of for catalysis sensitive material of monitoring air acetaldehyde and preparation method thereof.The sensor of acetaldehyde in the monitoring air of making of this material can fast, accurately be measured airborne micro-acetaldehyde at the scene and not be subjected to the influence of other common coexistence interfering substance.
Catalysis sensitive material of the present invention is by Al
2O
3, TiO
2And Fe
2O
3Nano-powder is formed, and concrete preparation method is:
With aluminium salt soluble in water, titanium salt and molysite are dissolved in the deionized water altogether, sonic oscillation is to clear, mixed solution is heated to 45 ℃, under constantly stirring, slowly drip the ammoniacal liquor of massfraction 10-20%, rate of addition for p.s. 1-2 drip, do not generate until there being precipitation, be cooled to room temperature, continue to stir 1 hour, left standstill 5-8 hour, with sedimentation and filtration, in 110 ℃ of oven dry 2 hours, after fully grinding, in chamber type electric resistance furnace, be no more than 5 ℃ speed with per minute and be warming up to 450-490 ℃, keep this temperature calcining 4-6 hour, naturally cooling namely obtains the catalysis sensitive material of acetaldehyde.
Wherein, aluminium salt is one or more mixture of the anhydride of aluminum nitrate, Tai-Ace S 150, aluminum perchlorate, aluminum chloride and Burow Solution or hydrate, titanium salt is one or more mixture of the anhydride of Titanium Nitrate, titanium phosphate, titanium sulfate, acetic acid titanium and titanium tetrachloride or hydrate, and molysite is one or more mixture of the anhydride of iron(ic) chloride, Iron triperchlorate, ferric sulfate, ferrous sulfate, iron nitrate and Iron nitrate or hydrate.
The sensitive material transmissioning electric mirror test that makes, when its particle diameter is no more than 50nm, and the mass percent of each component satisfies Al
2O
3(25-40%), TiO
2(35-50%) and Fe
2O
3In the time of (10-25%), be used for having very high sensitivity and selectivity as the sensitive material of monitoring air acetaldehyde.
The present invention has following advantage:
(1) utilize the weakly alkaline of weak ammonia to come the acid-basicity of slow regulator solution, precipitation process is slow, and particle growth is even, little, the narrow distribution range of gained powder body material particle diameter;
(2) prepared sensitive material has very high susceptibility and selectivity to aldehydes gas;
Aldehydes gas sensor continuous work-ing life of (3) making with prepared sensitive material was above 130 hours.
Embodiment
Embodiment 1
With nine water aluminum nitrates, phosphate dihydrate titanium and Iron trichloride hexahydrate are dissolved in the deionized water altogether, sonic oscillation is to clear, mixed solution is heated to 45 ℃, under constantly stirring, slowly drip the ammoniacal liquor of massfraction 10%, rate of addition is 1 of p.s., do not generate until there being precipitation, be cooled to room temperature, continue to stir 1 hour, left standstill 6 hours, with sedimentation and filtration, in 110 ℃ of oven dry 2 hours, after fully grinding, in chamber type electric resistance furnace, be no more than 5 ℃ speed with per minute and be warming up to 480 ℃, keep this temperature calcining 4 hours, naturally cooling namely obtains the catalysis sensitive material of acetaldehyde.
Analyze: with this powder body material of transmissioning electric mirror test, its particle diameter is no more than 50nm; It is carried out composition analysis, and recording each mass percent of forming is 25.8%Al
2O
3, 49.5%TiO
2And 24.7%Fe
2O
3
Use: measure airborne acetaldehyde with this powder as the catalytic luminescence sensitive material, linearity range 2～200mg/m
3, detection limit can reach 1.5mg/m
3, concurrent does not disturb.
Embodiment 2
With 18 water Tai-Ace S 150, Glacial acetic acid titanium and nine water Iron triperchlorates are dissolved in the deionized water altogether, sonic oscillation is to clear, mixed solution is heated to 45 ℃, under constantly stirring, slowly drip the ammoniacal liquor of massfraction 12%, rate of addition is 2 of p.s.s, do not generate until there being precipitation, be cooled to room temperature, continue to stir 1 hour, left standstill 7 hours, with sedimentation and filtration, in 110 ℃ of oven dry 2 hours, after fully grinding, in chamber type electric resistance furnace, be no more than 5 ℃ speed with per minute and be warming up to 470 ℃, keep this temperature calcining 6 hours, naturally cooling namely obtains the catalysis sensitive material of acetaldehyde.
Analyze: with this powder body material of transmissioning electric mirror test, its particle diameter is no more than 45nm; It is carried out composition analysis, and recording each mass percent of forming is 40.0%Al
2O
3, 35.9%TiO
2And 24.1%Fe
2O
3
Use: measure airborne acetaldehyde with this powder as the catalytic luminescence sensitive material, linearity range 2～150mg/m
3, detection limit can reach 1.5mg/m
3, concurrent does not disturb.
Embodiment 3
With nine water aluminum perchlorates, Aluminum Chloride Hexahydrate, the nitrate trihydrate titanium, the phosphate dihydrate titanium, anhydrous slufuric acid iron and nine water iron nitrates are dissolved in the deionized water altogether, sonic oscillation is to clear, mixed solution is heated to 45 ℃, under constantly stirring, slowly drip the ammoniacal liquor of massfraction 20%, rate of addition is 2 of p.s.s, do not generate until there being precipitation, be cooled to room temperature, continue to stir 1 hour, left standstill 8 hours, with sedimentation and filtration, in 110 ℃ of oven dry 2 hours, after fully grinding, in chamber type electric resistance furnace, be no more than 5 ℃ speed with per minute and be warming up to 460 ℃, keep this temperature calcining 5 hours, naturally cooling namely obtains the catalysis sensitive material of acetaldehyde.
Analyze: with this powder body material of transmissioning electric mirror test, its particle diameter is no more than 40nm; It is carried out composition analysis, and recording each mass percent of forming is 39.1%Al
2O
3, 49.6%TiO
2And 11.3%Fe
2O
3
Use: measure airborne acetaldehyde with this powder as the catalytic luminescence sensitive material, linearity range 2～300mg/m
3, detection limit can reach 1.2mg/m
3, concurrent does not disturb.
Embodiment 4
With acetate dihydrate aluminium, anhydrous titanium tetrachloride and six water Iron nitrates are dissolved in the deionized water altogether, sonic oscillation is to clear, mixed solution is heated to 45 ℃, under constantly stirring, slowly drip the ammoniacal liquor of massfraction 15%, rate of addition is 1 of p.s., do not generate until there being precipitation, be cooled to room temperature, continue to stir 1 hour, left standstill 5 hours, with sedimentation and filtration, in 110 ℃ of oven dry 2 hours, after fully grinding, in chamber type electric resistance furnace, be no more than 5 ℃ speed with per minute and be warming up to 490 ℃, keep this temperature calcining 5 hours, naturally cooling namely obtains the catalysis sensitive material of acetaldehyde.
Analyze: with this powder body material of transmissioning electric mirror test, its particle diameter is no more than 50nm; It is carried out composition analysis, and recording each mass percent of forming is 33.7%Al
2O
3, 42.1%TiO
2And 24.2%Fe
2O
3
Use: measure airborne acetaldehyde with this powder as the catalytic luminescence sensitive material, linearity range 2～200mg/m
3, detection limit can reach 1.5mg/m
3, concurrent does not disturb.
Embodiment 5
With nine water aluminum perchlorates, nine water titanium sulfates, anhydrous titanium tetrachloride, ferrous and the nine water iron nitrates of anhydrous slufuric acid are dissolved in the deionized water altogether, sonic oscillation is to clear, mixed solution is heated to 45 ℃, under constantly stirring, slowly drip the ammoniacal liquor of massfraction 18%, rate of addition is 2 of p.s.s, do not generate until there being precipitation, be cooled to room temperature, continue to stir 1 hour, left standstill 7 hours, with sedimentation and filtration, in 110 ℃ of oven dry 2 hours, after fully grinding, in chamber type electric resistance furnace, be no more than 5 ℃ speed with per minute and be warming up to 450 ℃, keep this temperature calcining 6 hours, naturally cooling namely obtains the catalysis sensitive material of acetaldehyde.
Analyze: with this powder body material of transmissioning electric mirror test, its particle diameter is no more than 45nm; It is carried out composition analysis, and recording each mass percent of forming is 36.9%Al
2O
3, 48.1%TiO
2And 15.0%Fe
2O
3
Use: measure airborne acetaldehyde with this powder as the catalytic luminescence sensitive material, linearity range 1.5～170mg/m
3, detection limit can reach 1.0mg/m
3, concurrent does not disturb.
Claims (3)
1. a catalysis sensitive material that is used for monitoring acetaldehyde is characterized in that by Al
2O
3, TiO
2And Fe
2O
3Nano-powder is formed, and wherein the mass percent scope of each component is Al
2O
3(25-40%), TiO
2(35-50%) and Fe
2O
3(10-25%), its preparation method is: with aluminium salt soluble in water, titanium salt and molysite are dissolved in the deionized water altogether, sonic oscillation is to clear, mixed solution is heated to 45 ℃, under constantly stirring, slowly drip the ammoniacal liquor of massfraction 10-20%, rate of addition for p.s. 1-2 drip, do not generate until there being precipitation, be cooled to room temperature, continue to stir 1 hour, left standstill 5-8 hour, with sedimentation and filtration, in 110 ℃ of oven dry 2 hours, after fully grinding, be no more than 5 ℃ speed with per minute and be warming up to 450-490 ℃ in chamber type electric resistance furnace, keep this temperature calcining 4-6 hour, naturally cooling namely obtains the catalysis sensitive material of acetaldehyde.
2. according to claim 1 a kind of for the catalysis sensitive material of monitoring acetaldehyde, one or more the mixture that it is characterized in that anhydride that described aluminium salt is aluminum nitrate, Tai-Ace S 150, aluminum perchlorate, aluminum chloride and Burow Solution or hydrate, titanium salt is one or more mixture of the anhydride of Titanium Nitrate, titanium phosphate, titanium sulfate, acetic acid titanium and titanium tetrachloride or hydrate, and molysite is one or more mixture of the anhydride of iron(ic) chloride, Iron triperchlorate, ferric sulfate, ferrous sulfate, iron nitrate and Iron nitrate or hydrate.
3. a kind of catalysis sensitive material for monitoring acetaldehyde according to claim 1 is characterized in that the particle diameter of described nano-powder is no more than 50nm.
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|---|---|---|---|
| CN201310122609.1A CN103275709B (en) | 2013-03-29 | 2013-03-29 | Catalysis sensitive material of acetaldehyde |
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|---|---|---|---|
| CN201310122609.1A CN103275709B (en) | 2013-03-29 | 2013-03-29 | Catalysis sensitive material of acetaldehyde |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110095559A (en) * | 2019-04-03 | 2019-08-06 | 北京联合大学 | The catalytic luminescence sensitive material of low temperature formaldehyde, benzene and ammonia |
| CN114249342A (en) * | 2021-12-21 | 2022-03-29 | 广东药科大学 | Nano gamma-alumina, preparation method thereof and application thereof in detecting 2-methylacrolein |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101382492A (en) * | 2008-10-09 | 2009-03-11 | 北京联合大学生物化学工程学院 | Catalytic luminescent and gas sensitive material of ethanol |
| US20090090626A1 (en) * | 2006-10-12 | 2009-04-09 | Holt Christopher T | Hydrogen sensitive composite material, hydrogen gas sensor, and sensor for detecting hydrogen and other gases with improved baseline resistance |
| US20090148347A1 (en) * | 2007-12-10 | 2009-06-11 | Electronics And Telecommunications Research Institute | Nano-crystalline composite-oxide thin film, environmental gas sensor using the thin film, and method of manufacturing the environmental gas sensor |
| CN101706485A (en) * | 2009-11-23 | 2010-05-12 | 北京联合大学生物化学工程学院 | Doped nano sensitive material for monitoring benzene |
| US20100147684A1 (en) * | 2008-12-12 | 2010-06-17 | Electronics And Telecommunications Research Institute | Ultra-sensitive gas sensor using oxide semiconductor nanofiber and method of fabricating the same |
-
2013
- 2013-03-29 CN CN201310122609.1A patent/CN103275709B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090090626A1 (en) * | 2006-10-12 | 2009-04-09 | Holt Christopher T | Hydrogen sensitive composite material, hydrogen gas sensor, and sensor for detecting hydrogen and other gases with improved baseline resistance |
| US20090148347A1 (en) * | 2007-12-10 | 2009-06-11 | Electronics And Telecommunications Research Institute | Nano-crystalline composite-oxide thin film, environmental gas sensor using the thin film, and method of manufacturing the environmental gas sensor |
| CN101382492A (en) * | 2008-10-09 | 2009-03-11 | 北京联合大学生物化学工程学院 | Catalytic luminescent and gas sensitive material of ethanol |
| US20100147684A1 (en) * | 2008-12-12 | 2010-06-17 | Electronics And Telecommunications Research Institute | Ultra-sensitive gas sensor using oxide semiconductor nanofiber and method of fabricating the same |
| CN101706485A (en) * | 2009-11-23 | 2010-05-12 | 北京联合大学生物化学工程学院 | Doped nano sensitive material for monitoring benzene |
Non-Patent Citations (1)
| Title |
|---|
| 张立春，等: "基于催化发光的挥发性有机物气体传感器研究进展", 《中国科技论文在线》, vol. 5, no. 9, 15 September 2010 (2010-09-15), pages 736 - 741 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110095559A (en) * | 2019-04-03 | 2019-08-06 | 北京联合大学 | The catalytic luminescence sensitive material of low temperature formaldehyde, benzene and ammonia |
| CN110095559B (en) * | 2019-04-03 | 2021-09-14 | 北京联合大学 | Catalytic luminous sensitive material of low-temperature formaldehyde, benzene and ammonia |
| CN114249342A (en) * | 2021-12-21 | 2022-03-29 | 广东药科大学 | Nano gamma-alumina, preparation method thereof and application thereof in detecting 2-methylacrolein |
| CN114249342B (en) * | 2021-12-21 | 2024-02-06 | 广东药科大学 | Nanometer gamma-alumina, preparation method thereof and application thereof in detection of 2-methylacrolein |
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| CN103275709B (en) | 2014-10-22 |
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