CN103792227A - Nano composite oxide sensitive material for formaldehyde and benzene - Google Patents
Nano composite oxide sensitive material for formaldehyde and benzene Download PDFInfo
- Publication number
- CN103792227A CN103792227A CN201410042995.8A CN201410042995A CN103792227A CN 103792227 A CN103792227 A CN 103792227A CN 201410042995 A CN201410042995 A CN 201410042995A CN 103792227 A CN103792227 A CN 103792227A
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- Prior art keywords
- benzene
- formaldehyde
- bismuth
- sensitive material
- titanium
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Abstract
The invention relates to a nano composite oxide sensitive material for monitoring formaldehyde and benzene. The nano composite oxide sensitive material is a nano powder material consisting of the components in percentage by mass: 50-60 percent of Bi2O3, 20-30 percent of TiO2 and 15-25 percent of MnO2. A preparation method comprises the steps of co-dissolving bismuth salt, titanium salt and manganese salt in a citric acid aqueous solution, performing ultrasonic oscillation until the solution is clarified, adding a proper amount of ethylene diamine tetraacetic acid disodium under high-speed stirring to keep the solution clarified, continuing to stir, dropwise adding ammonia water to adjust the pH value of the solution, stewing, aging, filtering and drying the product, performing full grinding, and roasting in a box type resistance furnace to obtain the powder material consisting of the Bi2O3, TiO2 and MnO2. A formaldehyde and benzene catalysis luminous sensor made of the composite oxide sensitive material provided by the invention is wide in linear range, high in selectivity and high in sensitivity, and can monitor the formaldehyde and the benzene in air on line without influence by coexistence substances.
Description
Technical field
The present invention relates to a kind of for monitoring the catalytic luminescence sensitive material of formaldehyde and benzene, especially by Bi
2o
3, TiO
2and MnO
2the nano composite oxide sensitive material of composition, belongs to field of sensing technologies.
Background technology
Formaldehyde is a kind of colourless volatile industrial chemicals, is widely used in the products such as compressive plate, coating, paint, cosmetics and wrappage as adhesive raw materials, sanitizer, antiseptic and finishing agent.People have different reflections to the formaldehyde of various concentration in air, when concentration of formaldehyde reaches 0.06～0.07mg/m in air
3time, will there is slight asthma in children, reach 0.1mg/m
3time just have peculiar smell and sense of discomfort, reach 0.5mg/m
3in time, can stimulate eyes to cause to shed tears, reach 0.6mg/m
3can cause throat discomfort or pain, reach 1mg/m
3in time, can cause in a large number and sheds tears, reach 10mg/m
3in time, is felt to have difficulty in breathing, and reaches 30mg/m
3time can make people suffocate.Long Term Contact low dosage formaldehyde (0.1mg/m
3below) can cause the pathologies such as chronic respiratory disease, women's pregnancy syndrome, the reduction of neonate's physique and chromosome abnormality.
Benzene is a kind of industrial chemicals with aromatic odor, and airborne benzene is mainly derived from building coating, paint for decoration, adhesive solvent and vehicle exhaust etc.Chronic Benzene Poisoning is mainly that skin, eyes and the upper respiratory tract are had to spread effect; Often Contact benzene, skin can be because of degreasing desiccation furfur, some appearance allergic eczemas; The long-term benzene that sucks can cause alpastic anemia.
Benzene and formaldehyde are all confirmed as carcinogen by IARC (IARC), and the two is all the major pollutants in room air.Zoopery shows that formaldehyde and benzene all can increase Micronucleus and rate of teratosperm, cause pregnant mouse abortion ratio to rise and litter size decline, damage mouse spleen and lungs, have synergy when the two synergy.The benzene and the formaldehyde that studies have reported that low concentration can bring out leukaemia, and because benzene and formaldehyde in the environment of our live and work are ubiquitous, the method for therefore studying rapid and accurate determination Minim Benzene in Gas Phase and formaldehyde has very strong realistic meaning.
The method of measuring trace formaldehyde and benzene mainly contains photometry, electrochemical process, chromatography, chemoluminescence method, makings Liquid Chromatography/Mass Spectrometry and the chromatography of ions etc.Could complete mensuration by analytical instrument because these methods all need preconcentration and suitable processing, therefore length consuming time is difficult for on-the-spot realization.Inventor uses nanosized copper ferromanganese (atomic ratio 4: 3: 1) composite oxides 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 " for 2006, can detect online 1～80mg/m
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.In the paper that is entitled as " nano composite oxide catalytic luminescence method is measured airborne formaldehyde " of delivering on " chemical journal " for 2008, use nanoscale molybdenum vanadium titanium (atomic ratio is 2: 3: 5) composite oxides as sensitive material, can detect online 0.07～34mg/m
3formaldehyde, detection limit can reach 0.04mg/m
3but the mensuration of benzene, ammonia, sulphuric dioxide and acetone PARA FORMALDEHYDE PRILLS(91,95) has certain interference, patent of invention 200910223546.2 discloses a kind of nano sensitive material of monitoring benzene homologues, utilize sensor prepared by this material can monitor airborne micro-benzene, but formaldehyde, methyl alcohol, sulfuretted hydrogen and acetic acid etc. also have response signal.
Summary of the invention
The object of the invention is to overcome the deficiency of conventional art, nano catalytic luminescence sensitive material that a kind of PARA FORMALDEHYDE PRILLS(91,95) and benzene has high selectivity more and preparation method thereof is provided.The monitoring formaldehyde of making of this sensitive material and the gas sensor of benzene, can be at the scene fast, the airborne trace formaldehyde of Accurate Determining and benzene and be not subject to the interference of other concurrent.
Nano sensitive material of the present invention is by Bi
2o
3, TiO
2and MnO
2the nano-powder material of composition, its preparation method is: by bismuth salt, it is in 10% aqueous citric acid solution that titanium salt and manganese salt are dissolved in massfraction altogether, sonic oscillation is to clarification, under high-speed stirred, add appropriate disodium ethylene diamine tetraacetate to make solution keep clear state more than 5 hours, continue to stir the speed that is no more than 1mL take per minute and drip the ammoniacal liquor of massfraction 15% to pH value as 6.5-7.3, still aging 2-5 hour, by sedimentation and filtration and be placed in drying box dry 5-10 hour at 95-110 ℃ of temperature, after fully grinding, in chamber type electric resistance furnace, be no more than the speed of 5 ℃ with per minute and be warming up to 290-330 ℃, keep this temperature roasting 2-3 hour, obtain by Bi
2o
3, TiO
2and MnO
2the powder body material of composition.
Wherein, bismuth salt is one or more potpourri of the anhydride of bismuth acetate, bismuth oxalate, bismuth nitrate, bismuth sulfate, bismuth phosphate and bismuth trichloride 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 manganese salt is one or more potpourri of the anhydride of manganese acetate, manganese sulfate, manganese chloride, manganese nitrate and Manganese perchlorate or hydrate.
When the particle diameter of nanometer powder making is no more than 35nm, and each constituent mass mark meets Bi
2o
3(50-60%), TiO
2(20-30%) and MnO
2(15-25%) time, for thering is very high sensitivity and selectivity as the sensitive material of monitoring formaldehyde and benzene.
Embodiment
Embodiment 1
By seven water bismuth oxalates, it is in 10% aqueous citric acid solution that Titanium Nitrate and acetate dihydrate manganese are dissolved in massfraction altogether, sonic oscillation is to clarification, under high-speed stirred, add appropriate disodium ethylene diamine tetraacetate to make solution keep clear state 6 hours, continue to stir the speed that is no more than 1mL take per minute and drip the ammoniacal liquor of massfraction 15% to pH value as 6.6, still aging 3 hours, by sedimentation and filtration and be placed in drying box at 100 ℃ of temperature dry 6 hours, after fully grinding, in chamber type electric resistance furnace, be no more than the speed of 5 ℃ with per minute and be warming up to 300 ℃, keep this temperature roasting 2 hours, obtain by Bi
2o
3, TiO
2and MnO
2the powder body material of composition.
Analyze: with this powder body material of transmissioning electric mirror test, its maximum particle diameter is no more than 35nm, and mean grain size is about 30nm; It is carried out to constituent analysis, and recording mass percent is 52.1%Bi
2o
3, 28.5%TiO
2and 19.4%MnO
2.
Application: measure airborne formaldehyde and benzene using this powder body material as sensitive material, the range of linearity is formaldehyde 0.5-75mg/m
3with benzene 0.7-86mg/m
3, detect and be limited to formaldehyde 0.1mg/m
3with benzene 0.3mg/m
3, concurrent does not disturb.
Embodiment 2
By five water bismuth nitrates, bismuth sulfate, it is in 10% aqueous citric acid solution that phosphate dihydrate titanium and manganese sulfate are dissolved in massfraction altogether, sonic oscillation is to clarification, under high-speed stirred, add appropriate disodium ethylene diamine tetraacetate to make solution keep clear state 7 hours, continue to stir the speed that is no more than 1mL take per minute and drip the ammoniacal liquor of massfraction 15% to pH value as 7.2, still aging 2 hours, by sedimentation and filtration and be placed in drying box at 105 ℃ of temperature dry 7 hours, after fully grinding, in chamber type electric resistance furnace, be no more than the speed of 5 ℃ with per minute and be warming up to 325 ℃, keep this temperature roasting 3 hours, obtain by Bi
2o
3, TiO
2and MnO
2the powder body material of composition.
Analyze: with this powder body material of transmissioning electric mirror test, its maximum particle diameter is no more than 33nm, and mean grain size is about 27nm; It is carried out to constituent analysis, and recording mass percent is 55.7%Bi
2o
3, 24.1%TiO
2and 20.2%MnO
2.
Application: measure airborne formaldehyde and benzene using this powder body material as sensitive material, the range of linearity is formaldehyde 0.3-65mg/m
3with benzene 0.5-70mg/m
3, detect and be limited to formaldehyde 0.08mg/m
3with benzene 0.2mg/m
3, concurrent does not disturb.
Embodiment 3
By bismuth phosphate, acetic acid titanium, it is in 10% aqueous citric acid solution that manganese nitrate and tetrahydrate manganese chloride are dissolved in massfraction altogether, sonic oscillation is to clarification, under high-speed stirred, add appropriate disodium ethylene diamine tetraacetate to make solution keep clear state 8 hours, continue to stir the speed that is no more than 1mL take per minute and drip the ammoniacal liquor of massfraction 15% to pH value as 6.8, still aging 5 hours, by sedimentation and filtration and be placed in drying box at 95 ℃ of temperature dry 9 hours, after fully grinding, in chamber type electric resistance furnace, be no more than the speed of 5 ℃ with per minute and be warming up to 310 ℃, keep this temperature roasting 3 hours, obtain by Bi
2o
3, TiO
2and MnO
2the powder body material of composition.
Analyze: with this powder body material of transmissioning electric mirror test, its maximum particle diameter is no more than 35nm, and mean grain size is about 30nm; It is carried out to constituent analysis, and recording mass percent is 57.4%Bi
2o
3, 26.1%TiO
2and 16.5%MnO
2.
Application: measure airborne formaldehyde and benzene using this powder body material as sensitive material, the range of linearity is formaldehyde 0.8-105mg/m
3with benzene 0.9-96mg/m
3, detect and be limited to formaldehyde 0.3mg/m
3with benzene 0.3mg/m
3, concurrent does not disturb.
Embodiment 4
By bismuth acetate, it is in 10% aqueous citric acid solution that nine water titanium sulfates and perchlorate hexahydrate's manganese are dissolved in massfraction altogether, sonic oscillation is to clarification, under high-speed stirred, add appropriate disodium ethylene diamine tetraacetate to make solution keep clear state 6 hours, continue to stir the speed that is no more than 1mL take per minute and drip the ammoniacal liquor of massfraction 15% to pH value as 6.9, still aging 4 hours, by sedimentation and filtration and be placed in drying box at 98 ℃ of temperature dry 8 hours, after fully grinding, in chamber type electric resistance furnace, be no more than the speed of 5 ℃ with per minute and be warming up to 295 ℃, keep this temperature roasting 2.5 hours, obtain by Bi
2o
3, TiO
2and MnO
2the powder body material of composition.
Analyze: with this powder body material of transmissioning electric mirror test, its maximum particle diameter is no more than 35nm, and mean grain size is about 28nm; It is carried out to constituent analysis, and recording mass percent is 59.2%Bi
2o
3, 22.4%TiO
2and 18.4%MnO
2.
Application: measure airborne formaldehyde and benzene using this powder body material as sensitive material, the range of linearity is formaldehyde 0.2-54mg/m
3with benzene 0.5-71mg/m
3, detect and be limited to formaldehyde 0.06mg/m
3with benzene 0.1mg/m
3, concurrent does not disturb.
Embodiment 5
By bismuth trichloride, it is in 10% aqueous citric acid solution that titanium tetrachloride and six water manganese nitrates are dissolved in massfraction altogether, sonic oscillation is to clarification, under high-speed stirred, add appropriate disodium ethylene diamine tetraacetate to make solution keep clear state 7 hours, continue to stir the speed that is no more than 1mL take per minute and drip the ammoniacal liquor of massfraction 15% to pH value as 7.0, still aging 3 hours, by sedimentation and filtration and be placed in drying box at 108 ℃ of temperature dry 5 hours, after fully grinding, in chamber type electric resistance furnace, be no more than the speed of 5 ℃ with per minute and be warming up to 320 ℃, keep this temperature roasting 2 hours, obtain by Bi
2o
3, TiO
2and MnO
2the powder body material of composition.
Analyze: with this powder body material of transmissioning electric mirror test, its maximum particle diameter is no more than 35nm, and mean grain size is about 30nm; It is carried out to constituent analysis, and recording mass percent is 51.5%Bi
2o
3, 23.7%TiO
2and 24.8%MnO
2.
Application: measure airborne formaldehyde and benzene using this powder body material as sensitive material, the range of linearity is formaldehyde 0.3-65mg/m
3with benzene 0.5-76mg/m
3, detect and be limited to formaldehyde 0.1mg/m
3with benzene 0.3mg/m
3, concurrent does not disturb.
Claims (3)
1. for monitoring a nano composite oxide sensitive material for formaldehyde and benzene, it is characterized in that by Bi
2o
3, TiO
2and MnO
2the nano-powder material of composition, wherein the mass percent scope of each component is Bi
2o
3(50-60%), TiO
2(20-30%) and MnO
2(15-25%), its preparation method is: by bismuth salt, it is in 10% aqueous citric acid solution that titanium salt and manganese salt are dissolved in massfraction altogether, sonic oscillation is to clarification, under high-speed stirred, add gross mass to be no more than the disodium ethylene diamine tetraacetate of citric acid in batches, make solution keep clear state more than 5 hours, continue to stir the speed that is no more than 1mL take per minute and drip the ammoniacal liquor of massfraction 15% to pH value as 6.5-7.3, still aging 2-5 hour, by sedimentation and filtration and be placed in drying box dry 5-10 hour at 95-110 ℃ of temperature, after fully grinding, in chamber type electric resistance furnace, be no more than the speed of 5 ℃ with per minute and be warming up to 290-330 ℃, keep this temperature roasting 2-3 hour, obtain by Bi
2o
3, TiO
2and MnO
2the powder body material of composition.
2. according to claim 1 a kind of for monitoring the nano composite oxide sensitive material of formaldehyde and benzene, it is characterized in that described bismuth salt is one or more potpourri of the anhydride of bismuth acetate, bismuth oxalate, bismuth nitrate, bismuth sulfate, bismuth phosphate and bismuth trichloride 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 manganese salt is one or more potpourri of the anhydride of manganese acetate, manganese sulfate, manganese chloride, manganese nitrate and Manganese perchlorate or hydrate.
3. according to claim 1 a kind of for monitoring the nano composite oxide sensitive material of formaldehyde and benzene, it is characterized in that the particle diameter of described nano-powder is no more than 35nm.
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|---|---|---|---|
| CN201410042995.8A CN103792227B (en) | 2014-01-22 | 2014-01-22 | Nano composite oxide sensitive material for formaldehyde and benzene |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201410042995.8A CN103792227B (en) | 2014-01-22 | 2014-01-22 | Nano composite oxide sensitive material for formaldehyde and benzene |
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|---|---|
| CN103792227A true CN103792227A (en) | 2014-05-14 |
| CN103792227B CN103792227B (en) | 2017-02-15 |
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| CN104267022A (en) * | 2014-09-04 | 2015-01-07 | 北京联合大学 | Cross sensitive material of ammonia and benzene in air and preparation method of cross sensitive material |
| CN104297416A (en) * | 2014-11-03 | 2015-01-21 | 北京联合大学 | Cataluminescence sensitive material for formaldehyde, benzene and ammonia in air |
| CN104297436A (en) * | 2014-11-03 | 2015-01-21 | 北京联合大学 | Material for detecting cross sensitivity of formaldehyde and methanol |
| CN105527276A (en) * | 2015-12-25 | 2016-04-27 | 北京联合大学 | Cataluminescence sensitive material for rapid determination of formaldehyde and sulfur dioxide |
| CN105628856A (en) * | 2015-12-25 | 2016-06-01 | 北京联合大学 | Luminescent sensitive material catalyzed by benzene and sulfur dioxide |
| CN109490375A (en) * | 2018-11-30 | 2019-03-19 | 北京联合大学 | The low-temperature sensitive material of formaldehyde and benzene |
| 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 |
| CN110376196A (en) * | 2019-07-16 | 2019-10-25 | 北京联合大学 | Sensitive material that is a kind of while responding hydrogen sulfide and sulfur dioxide |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104267022A (en) * | 2014-09-04 | 2015-01-07 | 北京联合大学 | Cross sensitive material of ammonia and benzene in air and preparation method of cross sensitive material |
| CN104297416A (en) * | 2014-11-03 | 2015-01-21 | 北京联合大学 | Cataluminescence sensitive material for formaldehyde, benzene and ammonia in air |
| CN104297436A (en) * | 2014-11-03 | 2015-01-21 | 北京联合大学 | Material for detecting cross sensitivity of formaldehyde and methanol |
| CN104297436B (en) * | 2014-11-03 | 2016-04-20 | 北京联合大学 | A kind of cross sensitivity material detecting formaldehyde and methyl alcohol |
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| CN105628856A (en) * | 2015-12-25 | 2016-06-01 | 北京联合大学 | Luminescent sensitive material catalyzed by benzene and sulfur dioxide |
| CN105527276A (en) * | 2015-12-25 | 2016-04-27 | 北京联合大学 | Cataluminescence sensitive material for rapid determination of formaldehyde and sulfur dioxide |
| CN105628856B (en) * | 2015-12-25 | 2017-10-20 | 北京联合大学 | A kind of catalytic luminescence sensitive material of benzene and sulfur dioxide |
| CN109490375A (en) * | 2018-11-30 | 2019-03-19 | 北京联合大学 | The low-temperature sensitive material of formaldehyde and benzene |
| 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 |
| CN110376196A (en) * | 2019-07-16 | 2019-10-25 | 北京联合大学 | Sensitive material that is a kind of while responding hydrogen sulfide and sulfur dioxide |
| CN110376196B (en) * | 2019-07-16 | 2021-12-03 | 北京联合大学 | Sensitive material capable of simultaneously responding to hydrogen sulfide and sulfur dioxide |
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