CN103275709B - Catalysis sensitive material of acetaldehyde - Google Patents

Catalysis sensitive material of acetaldehyde Download PDF

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Publication number
CN103275709B
CN103275709B CN201310122609.1A CN201310122609A CN103275709B CN 103275709 B CN103275709 B CN 103275709B CN 201310122609 A CN201310122609 A CN 201310122609A CN 103275709 B CN103275709 B CN 103275709B
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acetaldehyde
sensitive material
titanium
catalysis sensitive
catalysis
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CN103275709A (en
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周考文
邢正
蔡鑫
高彬隽
张洁
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College of Biochemical Engineering of Beijing Union University
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College of Biochemical Engineering of Beijing Union University
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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

The catalysis sensitive material of acetaldehyde
Technical field
The present invention relates to a kind of for monitoring the catalysis sensitive material of air acetaldehyde, especially by Al 2o 3, TiO 2and Fe 2o 3the composite metal oxide sensitive material of composition.Belong to field of sensing technologies.
Background technology
Acetaldehyde is a kind of volatile, irritant smell, colourless runny liquid, 20.8 DEG C of boiling points, and relative density is less than 1.Water soluble, ethanol, ether, chloroform, acetone and benzene.Its steam and air can form explosive mixture, explosion limits 4.0%～57.0% (volume).
Airborne low concentration acetaldehyde can cause eye, nose and upper respiratory tract irritation and bronchitis, sucks high concentration acetaldehyde and can cause the 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 can there is liver, kidney and cardiac damage.Skin contact acetaldehyde can cause irritant dermatitis.Visible, set up the assay method of acetaldehyde in air and there is certain realistic meaning.
The method of measuring acetaldehyde in 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 HPLC method is measured acetaldehyde in rat plasma " on the 12nd phase in 2012 " Pharmaceutical Analysis magazine ", Yu Tao etc. have delivered the article that is entitled as " trace formaldehyde and acetaldehyde in DNPH pre column Derivatization beer " on the 8th phase " Chinese Journal of Health Laboratory Technology " in 2012, Zou Yue etc. have delivered the article that is entitled as " Ultra Performance Liquid Chromatography method is measured formaldehyde and the acetaldehyde in cigarette wrapping paper " on the 5th phase " Yunnan chemical " in 2012, 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 " on the 29th phase " China Dispensary " in 2012, Zhang Yuanyuans etc. have been delivered the article that is entitled as " headspace GC detects acetaldehyde in beer " on the 9th phase " assay office " in 2011, Lu Wenjuan etc. have delivered the article that is entitled as " acetaldehyde in purge and trap-Water By Gas Chromatography, acryl aldehyde, vinyl cyanide " on the 10th phase in 2011 " physical and chemical inspection (chemical fascicle) ", Lv Guibin etc. have delivered article being entitled as " purge and trap-vapor-phase chromatography is measured the acetaldehyde in water simultaneously, acryl aldehyde and formaldehyde " etc. on the 6th phase " development fields of environmental monitoring in china " in 2011.In addition, Lv little Hu etc. has delivered and has been entitled as " isopropyl alcohol-ClO on the 8th phase " SCI " in 1991 --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 of Determination of Acetaldehyde by Chemiluminescence with Flow Injection " on the 6th phase " assay office " in 2011; although these two sections of articles are taking chemoluminescence method as basis, be also the method for measuring aldehyde in solution.
While measuring airborne micro-acetaldehyde by above these methods, need to use at the scene air sampler Concentration Sampling, and then get back to laboratory dissolving wash-out and be prepared into fluid sample and measure.
Cao little An etc. have delivered the article that is entitled as " a kind of catalytic luminescence aldehydes gas sensor research based on strontium carbonate nano material " on the 12nd phase " analytical chemistry " in 2004, have reported the method for acetaldehyde in a kind of direct mensuration air.They carry out quantitative test using strontium carbonate nano material as sensitive material at wavelength 425nm place, and the range of linearity is 6～6000mg/m 3, detect and be limited to 2mg/m 3.But ethanol and formaldehyde can cause respectively 42.5% and 12.5% interference.
Summary of the invention
The object of the invention is to overcome the deficiency of conventional art, provide a kind of for monitoring catalysis sensitive material of air acetaldehyde and preparation method thereof.The sensor of acetaldehyde in the monitoring air of making of this material, can be at the scene fast, the airborne micro-acetaldehyde of Accurate Determining and be not subject to the impact of other common mutual interference material.
Catalysis sensitive material of the present invention is by Al 2o 3, TiO 2and Fe 2o 3nano-powder composition, concrete preparation method is:
By aluminium salt soluble in water, titanium salt and molysite are dissolved in deionized water altogether, sonic oscillation is to clear, mixed liquor is heated to 45 DEG C, under constantly stirring, slowly drip the ammoniacal liquor of massfraction 10-20%, rate of addition be p.s. 1-2 drip, until generate without precipitation, be cooled to room temperature, continue to stir 1 hour, leave standstill 5-8 hour, by sedimentation and filtration, dry 2 hours in 110 DEG C, after fully grinding, in chamber type electric resistance furnace, be no more than the speed of 5 DEG C with per minute and be warming up to 450-490 DEG C, keep this temperature calcining 4-6 hour, naturally the cooling catalysis sensitive material that obtains acetaldehyde.
Wherein, aluminium salt is one or more potpourri of the anhydride of aluminium nitrate, aluminium sulphate, aluminum perchlorate, aluminum chloride and aluminum acetate or hydrate, titanium salt is one or more potpourri of the anhydride of Titanium Nitrate, titanium phosphate, titanium sulfate, acetic acid titanium and titanium tetrachloride or hydrate, and molysite is one or more potpourri of the anhydride of iron chloride, ferric perchlorate, iron sulfate, ferrous sulphate, ferric nitrate and ferrous nitrate or hydrate.
The sensitive material transmissioning electric mirror test making, when its particle diameter is no more than 50nm, and the mass percent of each component meets Al 2o 3(25-40%), TiO 2(35-50%) and Fe 2o 3(10-25%) time, for thering is very high sensitivity and selectivity as the sensitive material of monitoring air acetaldehyde.
Tool of the present invention has the following advantages:
(1) utilize the alkalescent of weak aqua ammonia to carry out the Acidity of Aikalinity of slow regulator solution, precipitation process is slow, and particle growth is even, and gained powder body material particle diameter is little, narrow distribution range;
(2) prepared sensitive material has very high sensitivity and selectivity to aldehydes gas;
(3) the aldehydes gas sensor made from prepared sensitive material exceedes 130 hours continuous serviceable life.
Embodiment
Embodiment 1
By nine water aluminium nitrates, phosphate dihydrate titanium and Iron trichloride hexahydrate are dissolved in deionized water altogether, sonic oscillation is to clear, mixed liquor is heated to 45 DEG C, under constantly stirring, slowly drip the ammoniacal liquor of massfraction 10%, rate of addition is 1 of p.s., until generate without precipitation, be cooled to room temperature, continue to stir 1 hour, leave standstill 6 hours, by sedimentation and filtration, dry 2 hours in 110 DEG C, after fully grinding, in chamber type electric resistance furnace, be no more than the speed of 5 DEG C with per minute and be warming up to 480 DEG C, keep this temperature calcining 4 hours, naturally the cooling catalysis sensitive material that obtains acetaldehyde.
Analyze: with this powder body material of transmissioning electric mirror test, its particle diameter is no more than 50nm; It is carried out to constituent analysis, and the mass percent that records each composition is 25.8%Al 2o 3, 49.5%TiO 2and 24.7%Fe 2o 3.
Application: measure airborne acetaldehyde using this powder as catalytic luminescence sensitive material, the range of linearity 2～200mg/m 3, detection limit can reach 1.5mg/m 3, concurrent does not disturb.
Embodiment 2
By 18 water aluminium sulphate, acetic anhydride titanium and nine water ferric perchlorates are dissolved in deionized water altogether, sonic oscillation is to clear, mixed liquor is heated to 45 DEG C, under constantly stirring, slowly drip the ammoniacal liquor of massfraction 12%, rate of addition is 2 of p.s.s, until generate without precipitation, be cooled to room temperature, continue to stir 1 hour, leave standstill 7 hours, by sedimentation and filtration, dry 2 hours in 110 DEG C, after fully grinding, in chamber type electric resistance furnace, be no more than the speed of 5 DEG C with per minute and be warming up to 470 DEG C, keep this temperature calcining 6 hours, naturally the cooling catalysis sensitive material that obtains acetaldehyde.
Analyze: with this powder body material of transmissioning electric mirror test, its particle diameter is no more than 45nm; It is carried out to constituent analysis, and the mass percent that records each composition is 40.0%Al 2o 3, 35.9%TiO 2and 24.1%Fe 2o 3.
Application: measure airborne acetaldehyde using this powder as catalytic luminescence sensitive material, the range of linearity 2～150mg/m 3, detection limit can reach 1.5mg/m 3, concurrent does not disturb.
Embodiment 3
By nine water aluminum perchlorates, Aluminum Chloride Hexahydrate, nitrate trihydrate titanium, phosphate dihydrate titanium, anhydrous ironic sulfate and nine water ferric nitrates are dissolved in deionized water altogether, sonic oscillation is to clear, mixed liquor is heated to 45 DEG C, under constantly stirring, slowly drip the ammoniacal liquor of massfraction 20%, rate of addition is 2 of p.s.s, until generate without precipitation, be cooled to room temperature, continue to stir 1 hour, leave standstill 8 hours, by sedimentation and filtration, dry 2 hours in 110 DEG C, after fully grinding, in chamber type electric resistance furnace, be no more than the speed of 5 DEG C with per minute and be warming up to 460 DEG C, keep this temperature calcining 5 hours, naturally the cooling catalysis sensitive material that obtains acetaldehyde.
Analyze: with this powder body material of transmissioning electric mirror test, its particle diameter is no more than 40nm; It is carried out to constituent analysis, and the mass percent that records each composition is 39.1%Al 2o 3, 49.6%TiO 2and 11.3%Fe 2o 3.
Application: measure airborne acetaldehyde using this powder as catalytic luminescence sensitive material, the range of linearity 2～300mg/m 3, detection limit can reach 1.2mg/m 3, concurrent does not disturb.
Embodiment 4
By acetate dihydrate aluminium, anhydrous titanium tetrachloride and six water ferrous nitrates are dissolved in deionized water altogether, sonic oscillation is to clear, mixed liquor is heated to 45 DEG C, under constantly stirring, slowly drip the ammoniacal liquor of massfraction 15%, rate of addition is 1 of p.s., until generate without precipitation, be cooled to room temperature, continue to stir 1 hour, leave standstill 5 hours, by sedimentation and filtration, dry 2 hours in 110 DEG C, after fully grinding, in chamber type electric resistance furnace, be no more than the speed of 5 DEG C with per minute and be warming up to 490 DEG C, keep this temperature calcining 5 hours, naturally the cooling catalysis sensitive material that obtains acetaldehyde.
Analyze: with this powder body material of transmissioning electric mirror test, its particle diameter is no more than 50nm; It is carried out to constituent analysis, and the mass percent that records each composition is 33.7%Al 2o 3, 42.1%TiO 2and 24.2%Fe 2o 3.
Application: measure airborne acetaldehyde using this powder as catalytic luminescence sensitive material, the range of linearity 2～200mg/m 3, detection limit can reach 1.5mg/m 3, concurrent does not disturb.
Embodiment 5
By nine water aluminum perchlorates, nine water titanium sulfates, anhydrous titanium tetrachloride, anhydrous slufuric acid ferrous iron and nine water ferric nitrates are dissolved in deionized water altogether, sonic oscillation is to clear, mixed liquor is heated to 45 DEG C, under constantly stirring, slowly drip the ammoniacal liquor of massfraction 18%, rate of addition is 2 of p.s.s, until generate without precipitation, be cooled to room temperature, continue to stir 1 hour, leave standstill 7 hours, by sedimentation and filtration, dry 2 hours in 110 DEG C, after fully grinding, in chamber type electric resistance furnace, be no more than the speed of 5 DEG C with per minute and be warming up to 450 DEG C, keep this temperature calcining 6 hours, naturally the cooling catalysis sensitive material that obtains acetaldehyde.
Analyze: with this powder body material of transmissioning electric mirror test, its particle diameter is no more than 45nm; It is carried out to constituent analysis, and the mass percent that records each composition is 36.9%Al 2o 3, 48.1%TiO 2and 15.0%Fe 2o 3.
Application: measure airborne acetaldehyde using this powder as catalytic luminescence sensitive material, the range of linearity 1.5～170mg/m 3, detection limit can reach 1.0mg/m 3, concurrent does not disturb.

Claims (3)

1. for monitoring a catalysis sensitive material for acetaldehyde, it is characterized in that by Al 2o 3, TiO 2and Fe 2o 3nano-powder composition, wherein the mass percent scope of each component is 25.8-40%Al 2o 3, 42.1-50%TiO 2and 10-24.7%Fe 2o 3, its preparation method is: by aluminium salt soluble in water, titanium salt and molysite are dissolved in deionized water altogether, sonic oscillation is to clear, mixed liquor is heated to 45 DEG C, under constantly stirring, slowly drip the ammoniacal liquor of massfraction 10-20%, rate of addition be p.s. 1-2 drip, until generate without precipitation, be cooled to room temperature, continue to stir 1 hour, leave standstill 5-8 hour, by sedimentation and filtration, dry 2 hours in 110 DEG C, after fully grinding, in chamber type electric resistance furnace, be no more than the speed of 5 DEG C with per minute and be warming up to 450-490 DEG C, keep this temperature calcining 4-6 hour, naturally the cooling catalysis sensitive material that obtains acetaldehyde.
2. according to claim 1 a kind of for monitoring the catalysis sensitive material of acetaldehyde, it is characterized in that described aluminium salt is one or more potpourri of the anhydride of aluminium nitrate, aluminium sulphate, aluminum perchlorate, aluminum chloride and aluminum acetate or hydrate, titanium salt is one or more potpourri of the anhydride of Titanium Nitrate, titanium phosphate, titanium sulfate, acetic acid titanium and titanium tetrachloride or hydrate, and molysite is one or more potpourri of the anhydride of iron chloride, ferric perchlorate, iron sulfate, ferrous sulphate, ferric nitrate and ferrous nitrate or hydrate.
3. according to claim 1 a kind of for monitoring the catalysis sensitive material of acetaldehyde, it is characterized in that the particle diameter of described nano-powder is no more than 50nm.
CN201310122609.1A 2013-03-29 2013-03-29 Catalysis sensitive material of acetaldehyde Expired - Fee Related CN103275709B (en)

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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
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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