CN108519459B - The sensitive material of low temperature formaldehyde, sulfur dioxide and trimethylamine - Google Patents
The sensitive material of low temperature formaldehyde, sulfur dioxide and trimethylamine Download PDFInfo
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- CN108519459B CN108519459B CN201810270497.7A CN201810270497A CN108519459B CN 108519459 B CN108519459 B CN 108519459B CN 201810270497 A CN201810270497 A CN 201810270497A CN 108519459 B CN108519459 B CN 108519459B
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- yttrium
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/10—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using catalysis
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G39/00—Compounds of molybdenum
- C01G39/02—Oxides; Hydroxides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
- C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
Abstract
The present invention relates to a kind of low-temperature sensitive materials for measuring formaldehyde in air, sulfur dioxide and trimethylamine simultaneously, it is characterized in that by BaO, MoO3And Y2O3The composite powder material of composition, wherein the mass fraction of each component is 26-34%BaO, 36-45%MoO3And 26-36%Y2O3.Preparation method is: with continuous stirring, the aqueous hydrochloric acid solution of barium salt is added drop-wise in the aqueous solution of malic acid of yttrium salt, agar powder is added after heating and stirs to clarify, this solution & stir is added to being completely dissolved in ammonium molybdate crystal, it is cooled to room temperature to form gel, it will be roasted in chamber type electric resistance furnace after the drying of this gel, cooled to room temperature is obtained by BaO, MoO3And Y2O3The composite powder material of composition.The gas sensor made using sensitive material provided by the present invention can quickly measure trace formaldehyde, sulfur dioxide and the trimethylamine in air without the interference by other common concurrents at the scene.
Description
Technical field
The present invention relates to a kind of low temperature formaldehyde, the sensitive material of sulfur dioxide and trimethylamine, especially by BaO, MoO3With
Y2O3The composite powder material of composition, belongs to field of sensing technologies.
Background technique
Formaldehyde is a kind of colourless volatile industrial chemicals, as adhesive raw materials, disinfectant, preservative and finishing agent quilt
It is widely used in the products such as compression plate, coating, paint, cosmetics and packaging material, and as the use of application product is not by
It is disconnected to be discharged into air.People have different reflections to the formaldehyde of concentration various in air: when the concentration of formaldehyde in air reaches
0.08mg/m3When children will occur slightly to pant, reach 0.1mg/m3When just have peculiar smell sense, reach 0.6mg/m3When can cause
Throat discomfort or pain, reach 1mg/m3When eyes can be caused largely to shed tears, reach 10mg/m3Shi Zehui feels expiratory dyspnea, reaches
To 30mg/m3When can make one to suffocate.Long Term Contact low dosage formaldehyde (0.1mg/m3Can cause below) chronic respiratory disease,
Women pregnancy syndrome, newborn's constitution reduce and the lesions such as chromosome abnormality.Formaldehyde is by International Cancer Research Center
(IARC) it is confirmed as carcinogen.
Sulfur dioxide is one of major pollutants in atmosphere, has many cities that the tight of sulfur dioxide harm occurred in the world
Weight event makes many people's poisonings or dead.Sulfur dioxide has acidity, can generate small with the substance reaction of other in air
Sulphite and sulphate particle.When these particles are inhaled into, they will be gathered in lung, be Respiratory symptoms and disease
One of the main reason for sick.When with eye contact, red and swollen and pain will cause.After sulfur dioxide enters respiratory tract, because its is readily soluble
Yu Shui, therefore major part is arrested in the upper respiratory tract, generating on wet mucous membrane has corrosive sulfurous acid, sulfuric acid and sulfuric acid
Salt enhances stimulation.For the smooth muscle of the upper respiratory tract because there is nerve ending receptor, assassination, which swashs, will generate narrow contracting reaction,
Reduce the lumen of trachea and bronchus, airway resistance increases.The upper respiratory tract acts on this detention of sulfur dioxide, certain
It can reduce stimulation of the sulfur dioxide to lung in degree.Sulfur dioxide can be rapidly absorbed into blood, generate toxic side effect to whole body,
The vigor of its energy destructive enzyme has certain damage to liver to significantly influence the metabolism of carbohydrate and protein.It is dynamic
Object test proves, after sulfur dioxide slow poisoning, the immune of body is obviously inhibited.
Trimethylamine also belongs to vaporous pollutant, is colourless gas (the fishy smell master of fish products for having fish oil stink under room temperature
Will be from trimethylamine), it is inflammable and explosive, and the eye to people, nose, throat and respiratory tract have stronger stimulation, Long Term Contact
Endanger larger, the presence of trimethylamine and its concentration are to assess the major criterion of meat and fish food quality, are characterization certain generations
The odor identification for thanking to deficiency disorders is the main object of environmental malodors contamination control, is that certain industrial and agricultural production quality control
Key parameter.
In many life areas, such as residential kitchen, freezer and market aquatic products sale room, these three molecules are usually simultaneously
In the presence of therefore, establishing has certain show to the rapid analysis method of trace formaldehyde, sulfur dioxide and front three amine concentration in air
Sincere justice.The measuring method of formaldehyde, sulfur dioxide or trimethylamine mainly have gas chromatography, liquid chromatography, spectrophotometry,
Infra-red sepectrometry, flow injection analysis, electrochemical process and chromatography of ions etc., due to these methods require preconcentration and
Proper treatment could be completed to measure by large-sized analytic instrument, therefore time-consuming is not easy live realization.Catalytic reaction is utilized in document
Light method measures the method for formaldehyde, sulfur dioxide or trimethylamine it has been reported that still having catalysis to these three molecules simultaneously respectively
The catalyst for the sensitivity characteristic that shines has not been reported.
Summary of the invention
The purpose of the present invention is overcoming the shortcomings of conventional art, provide it is a kind of no more than 200 DEG C at a temperature of PARA FORMALDEHYDE PRILLS(91,95),
Sulfur dioxide and trimethylamine have catalytic luminescence sensitive material of response and preparation method thereof.The gas made of this sensitive material
Body sensor, can at the scene quickly, the trace formaldehyde in Accurate Determining air, sulfur dioxide and trimethylamine be without by other total
Deposit the interference of molecule.
Sensitive material of the present invention is by BaO, MoO3And Y2O3The composite powder material of composition, preparation method is such as
Under: barium salt is dissolved in the aqueous hydrochloric acid solution that mass fraction is 10-15% and forms solution A, it is 15- that yttrium salt, which is dissolved in mass fraction,
Solution B is formed in 20% aqueous solution of malic acid, with continuous stirring, solution A is slowly dropped in solution B, and it is small to continue stirring 2
When, it is warming up to 95-98 DEG C, keeps temperature that agar powder is added and continues stirring to solution clarification, ammonium molybdate crystal is directly added into
This solution & stir is cooled to room temperature to form gel to being completely dissolved；After the drying of this gel, with every point in chamber type electric resistance furnace
Speed of the clock no more than 3 DEG C is warming up to 220-230 DEG C, keeps this temperature 4-5 hours, continues to be no more than 3 DEG C of speed per minute
Degree is warming up to 380-400 DEG C, keeps this temperature 2-3 hours, cooled to room temperature is obtained by BaO, MoO3And Y2O3Composition is answered
Close powder body material.
Wherein, barium salt is the anhydride of barium chloride and barium nitrate or one or two kinds of mixtures of hydrate, yttrium salt are
One or more of mixing of acetic acid yttrium, yttrium oxalate, yttrium nitrate, yttrium sulfate, the anhydride of yttrium phosphate and yttrium chloride or hydrate
Object.
Composite powder material each component mass fraction obtained meets BaO (26-34%), MoO3(36-45%) and Y2O3
When (26-36%) and partial size are 15-45 nanometers, it is used as the catalytic luminescence of formaldehyde in air, sulfur dioxide and trimethylamine
Sensitive material just has very high catalytic oxidation activity at 200 DEG C or less.
Specific embodiment
Embodiment 1
Barium chloride is dissolved in the aqueous hydrochloric acid solution that mass fraction is 10% and forms solution A, four water acetic acid yttriums are molten
It is to form solution B in 20% aqueous solution of malic acid in mass fraction, with continuous stirring, solution A is slowly dropped to solution B
In, continue stirring 2 hours, be warming up to 95 DEG C, keeps temperature that agar powder is added and continue stirring to solution clarification, by ammonium molybdate crystalline substance
Body is directly added into this solution and is stirred to being completely dissolved, and is cooled to room temperature to form gel；After the drying of this gel, box
225 DEG C are warming up to the speed for being no more than 3 DEG C per minute in resistance furnace, keeps this temperature 4.5 hours, is continued not surpass per minute
It crosses 3 DEG C of speed and is warming up to 382 DEG C, keep this temperature 3 hours, cooled to room temperature is obtained by BaO, MoO3And Y2O3Composition
Composite powder material.
Analysis: carrying out constituent analysis to composite powder material, and measuring mass percent is 26.7%BaO, 43.2%MoO3、
And 30.1%Y2O3；Transmission electron microscope measures average grain diameter about 22nm.
Using: using this powder body material as detection formaldehyde in air, the catalytic luminescence sensitivity material of sulfur dioxide and trimethylamine
Material, operating temperature are 188 DEG C, and the range of linearity is formaldehyde 0.1-75mg/m3, sulfur dioxide 0.2-67mg/m3With trimethylamine 0.4-
125mg/m3, detect and be limited to formaldehyde 0.05mg/m3, sulfur dioxide 0.1mg/m3With trimethylamine 0.2mg/m3, common concurrent do not have
Interference.
Embodiment 2
Barium nitrate is dissolved in the aqueous hydrochloric acid solution that mass fraction is 11% and forms solution A, nine water yttrium oxalates are dissolved in matter
Amount score is to form solution B in 19% aqueous solution of malic acid, and with continuous stirring, solution A is slowly dropped in solution B, after
Continuous stirring 2 hours, is warming up to 96 DEG C, keeps temperature that agar powder is added and continues to stir to solution and clarifies, and ammonium molybdate crystal is straight
It connects and this solution is added and is stirred to being completely dissolved, be cooled to room temperature to form gel；After the drying of this gel, in box resistance
226 DEG C are warming up to the speed for being no more than 3 DEG C per minute in furnace, keeps this temperature 4 hours, is continued to be no more than 3 DEG C per minute
Speed be warming up to 384 DEG C, keep this temperature 2.5 hours, cooled to room temperature is obtained by BaO, MoO3And Y2O3Composition is answered
Close powder body material.
Analysis: carrying out constituent analysis to composite powder material, and measuring mass percent is 33.3%BaO, 39.8%MoO3、
And 26.9%Y2O3；Transmission electron microscope measures average grain diameter about 35nm.
Using: using this powder body material as detection formaldehyde in air, the catalytic luminescence sensitivity material of sulfur dioxide and trimethylamine
Material, operating temperature are 179 DEG C, and the range of linearity is formaldehyde 0.1-68mg/m3, sulfur dioxide 0.2-75mg/m3With trimethylamine 0.4-
135mg/m3, detect and be limited to formaldehyde 0.05mg/m3, sulfur dioxide 0.1mg/m3With trimethylamine 0.2mg/m3。
Embodiment 3
Barium chloride and barium nitrate are dissolved in the aqueous hydrochloric acid solution that mass fraction is 12% and form solution A, by six water nitric acid
It is to form solution B in 18% aqueous solution of malic acid that yttrium and eight water yttrium sulfates, which are dissolved in mass fraction, with continuous stirring, by solution A
It is slowly dropped in solution B, continues stirring 2 hours, be warming up to 97 DEG C, keep temperature that agar powder is added and continue stirring to solution
Clarification, is directly added into this solution for ammonium molybdate crystal and is stirred to being completely dissolved, be cooled to room temperature to form gel；This is coagulated
After glue drying, 228 DEG C are warming up to the speed for being no more than 3 DEG C per minute in chamber type electric resistance furnace, keeps this temperature 4 hours, after
It is continuous to be warming up to 390 DEG C with the speed for being no more than 3 DEG C per minute, keep this temperature 2 hours, cooled to room temperature obtain by BaO,
MoO3And Y2O3The composite powder material of composition.
Analysis: carrying out constituent analysis to composite powder material, and measuring mass percent is 28.5%BaO, 36.1%MoO3、
And 35.4%Y2O3；Transmission electron microscope measures average grain diameter about 42nm.
Using: using this powder body material as detection formaldehyde in air, the catalytic luminescence sensitivity material of sulfur dioxide and trimethylamine
Material, operating temperature are 192 DEG C, and the range of linearity is formaldehyde 0.1-59mg/m3, sulfur dioxide 0.2-70mg/m3With trimethylamine 0.3-
123mg/m3, detect and be limited to formaldehyde 0.05mg/m3, sulfur dioxide 0.1mg/m3With trimethylamine 0.2mg/m3, common concurrent do not have
Interference.
Embodiment 4
Barium chloride and barium nitrate are dissolved in the aqueous hydrochloric acid solution that mass fraction is 14% and form solution A, Jiang Jiushui
It is to form solution B in 17% aqueous solution of malic acid that yttrium oxalate, yttrium phosphate and yttrium chloride, which are dissolved in mass fraction, with continuous stirring,
Solution A is slowly dropped in solution B, stirring 2 hours is continued, is warming up to 98 DEG C, keep temperature that agar powder is added and continues to stir
Mix to solution clarify, ammonium molybdate crystal is directly added into this solution and is stirred to being completely dissolved, be cooled to room temperature to be formed it is solidifying
Glue；After the drying of this gel, 224 DEG C are warming up to the speed for being no more than 3 DEG C per minute in chamber type electric resistance furnace, keeps this temperature
5 hours, continues to be warming up to 395 DEG C with the speed for being no more than 3 DEG C per minute, keep this temperature 2 hours, cooled to room temperature obtains
To by BaO, MoO3And Y2O3The composite powder material of composition.
Analysis: carrying out constituent analysis to composite powder material, and measuring mass percent is 30.9%BaO, 37.2%MoO3、
And 31.9%Y2O3；Transmission electron microscope measures average grain diameter about 31nm.
Using: using this powder body material as detection formaldehyde in air, the catalytic luminescence sensitivity material of sulfur dioxide and trimethylamine
Material, operating temperature are 185 DEG C, and the range of linearity is formaldehyde 0.1-70mg/m3, sulfur dioxide 0.2-62mg/m3With trimethylamine 0.4-
121mg/m3, detect and be limited to formaldehyde 0.05mg/m3, sulfur dioxide 0.1mg/m3With trimethylamine 0.2mg/m3, common concurrent do not have
Interference.
Embodiment 5
Barium nitrate is dissolved in the aqueous hydrochloric acid solution that mass fraction is 15% and forms solution A, by acetic acid yttrium and six water chlorinations
It is to form solution B in 16% aqueous solution of malic acid that yttrium, which is dissolved in mass fraction, with continuous stirring, solution A is slowly dropped to molten
In liquid B, continue stirring 2 hours, be warming up to 97 DEG C, keep temperature that agar powder is added and continues stirring to solution clarification, by molybdic acid
Ammonium crystal is directly added into this solution and is stirred to being completely dissolved, and is cooled to room temperature to form gel；After the drying of this gel,
222 DEG C are warming up to be no more than 3 DEG C of speed per minute in chamber type electric resistance furnace, keeps this temperature 4 hours, is continued with per minute not
Speed more than 3 DEG C is warming up to 398 DEG C, keeps this temperature 2 hours, and cooled to room temperature is obtained by BaO, MoO3And Y2O3Group
At composite powder material.
Analysis: carrying out constituent analysis to composite powder material, and measuring mass percent is 31.6%BaO, 41.7%MoO3、
And 26.7%Y2O3；Transmission electron microscope measures average grain diameter about 27nm.
Using: using this powder body material as detection formaldehyde in air, the catalytic luminescence sensitivity material of sulfur dioxide and trimethylamine
Material, operating temperature are 195 DEG C, and the range of linearity is formaldehyde 0.1-65mg/m3, sulfur dioxide 0.2-49mg/m3With trimethylamine 0.3-
89mg/m3, detect and be limited to formaldehyde 0.05mg/m3, sulfur dioxide 0.1mg/m3With trimethylamine 0.2mg/m3, common concurrent do not have
Interference.
Claims (1)
1. the sensitive material of a kind of low temperature formaldehyde, sulfur dioxide and trimethylamine, it is characterized in that by BaO, MoO3And Y2O3The grain of composition
The composite powder material that diameter is 15-45 nanometers, wherein the mass percent range of each component is 26-34%BaO, 36-45%
MoO3And 26-36%Y2O3, preparation method is: it is molten to be formed in the aqueous hydrochloric acid solution of 10-15% that barium salt is dissolved in mass fraction
Liquid A, it is to form solution B in 15-20% aqueous solution of malic acid that yttrium salt, which is dissolved in mass fraction, and with continuous stirring, solution A is delayed
Slowly it is added drop-wise in solution B, continues stirring 2 hours, be warming up to 95-98 DEG C, keep temperature that agar powder is added and continue to stir to molten
Liquid clarification, is directly added into this solution & stir to being completely dissolved for ammonium molybdate crystal, is cooled to room temperature to form gel；By this gel
After drying, it is warming up to 220-230 DEG C with the speed for being no more than 3 DEG C per minute in chamber type electric resistance furnace, keeps this temperature 4-5 small
When, continue to be warming up to 380-400 DEG C with the speed for being no more than 3 DEG C per minute, keeps this temperature 2-3 hours, naturally cool to room
Temperature is obtained by BaO, MoO3And Y2O3The composite powder material of composition；The barium salt be barium chloride and barium nitrate anhydride or
One or two kinds of mixtures of hydrate, yttrium salt is acetic acid yttrium, yttrium oxalate, yttrium nitrate, yttrium sulfate, yttrium phosphate and yttrium chloride
One or more of mixtures of anhydride or hydrate.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810270497.7A CN108519459B (en) | 2018-03-29 | 2018-03-29 | The sensitive material of low temperature formaldehyde, sulfur dioxide and trimethylamine |
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| CN201810270497.7A CN108519459B (en) | 2018-03-29 | 2018-03-29 | The sensitive material of low temperature formaldehyde, sulfur dioxide and trimethylamine |
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| CN108519459B true CN108519459B (en) | 2019-10-08 |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109490373B (en) * | 2018-11-30 | 2020-11-13 | 北京联合大学 | Catalytic luminous sensitive material of formaldehyde, carbon monoxide and sulfur dioxide |
| CN110045055B (en) * | 2019-05-16 | 2021-07-09 | 北京联合大学 | High-selectivity sensitive material of trimethylamine and hydrogen sulfide |
| CN110672591B (en) * | 2019-10-22 | 2021-10-12 | 北京联合大学 | Low-temperature response sensitive material for formaldehyde and trimethylamine in air |
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| CN103826743A (en) * | 2011-09-30 | 2014-05-28 | 韩国电力公社 | Fluidized bed aqueous gas-converting catalyst |
| CN104039451A (en) * | 2011-11-29 | 2014-09-10 | 希路瑞亚技术公司 | Nanowire catalysts and methods for their use and preparation |
| 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 |
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|---|---|---|---|---|
| CN103826743A (en) * | 2011-09-30 | 2014-05-28 | 韩国电力公社 | Fluidized bed aqueous gas-converting catalyst |
| CN104039451A (en) * | 2011-11-29 | 2014-09-10 | 希路瑞亚技术公司 | Nanowire catalysts and methods for their use and preparation |
| 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 |
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