CN110095559A - The catalytic luminescence sensitive material of low temperature formaldehyde, benzene and ammonia - Google Patents
The catalytic luminescence sensitive material of low temperature formaldehyde, benzene and ammonia Download PDFInfo
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- CN110095559A CN110095559A CN201910265321.7A CN201910265321A CN110095559A CN 110095559 A CN110095559 A CN 110095559A CN 201910265321 A CN201910265321 A CN 201910265321A CN 110095559 A CN110095559 A CN 110095559A
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/56—Platinum group metals
- B01J23/63—Platinum group metals with rare earths or actinides
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/206—Compounds containing only rare earth metals as the metal element oxide or hydroxide being the only anion
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- C01G15/00—Compounds of gallium, indium or thallium
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- C—CHEMISTRY; METALLURGY
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
- C09K11/7701—Chalogenides
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/76—Chemiluminescence; Bioluminescence
- G01N21/766—Chemiluminescence; Bioluminescence of gases
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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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- C—CHEMISTRY; METALLURGY
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- 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
Abstract
The present invention relates to the catalytic luminescence sensitive material of a kind of low temperature formaldehyde, benzene and ammonia, it is characterized in that gold atom doping by Dy2O3、In2O3With the composite powder material of PbO composition.Preparation method is: the aqueous tartaric acid solution of the aqueous solution of malic acid of dysprosium salt, the aqueous citric acid solution of indium salts and lead salt is sequentially added in aqueous solution of chloraurate, under heating stirring, agar powder is added and stirs to clarify, it is cooled into gel, it is atom doped by Dy then to obtain Au by drying, two-stage roasting and natural cooling2O3、In2O3With the composite powder material of PbO composition.The gas sensor made using sensitive material provided by the present invention, can at the scene trace formaldehyde, benzene and the ammonia in Sensitive Determination air without by other common interference that molecule coexists.
Description
Technical field
The present invention relates to the catalytic luminescence sensitive material of a kind of low temperature formaldehyde, benzene and ammonia, especially gold atom doping by
Dy2O3、In2O3With the composite powder material of PbO composition, belong to field of sensing technologies.
Background technique
Since interior decoration and all kinds of being widely used for Modern Live articles make room air pollution be on the rise, formaldehyde
(HCHO) it is widely used in compression plate, coating, paint, cosmetics as adhesive raw materials, disinfectant, preservative and finishing agent
In the products such as packaging material, and as the use of application product is constantly discharged into air.Benzene (C6H6) it is a kind of with virtue
The industrial chemicals of fragrance taste is often used as the solvent or diluent of decorations coating.Ammonia (NH3) it is a kind of with intense irritation smell
Alkaline gas, can from used construction antifreezing agent wall in slow release, therefore, formaldehyde, benzene and ammonia are the masters of room air
Want pollutant.The method of measurement formaldehyde, benzene and ammonia mainly has spectrophotometry, electrochemical process, chromatography, chemoluminescence method, gas
Matter or Liquid Chromatography/Mass Spectrometry and the chromatography of ions etc..These methods, which require preconcentration and proper treatment, could pass through analysis instrument
Measurement is completed, therefore time-consuming is not easy live realization.
Patent of invention ZL201410605596.8 discloses the catalytic luminescence sensitivity material of a kind of formaldehyde in air, benzene and ammonia
Material, but the use temperature of this sensitive material is more than 350 DEG C, the heat radiation background that such temperature generates can form stronger
Background signal has seriously affected the sensitivity of sensor.
Summary of the invention
The purpose of the present invention is overcoming the shortcomings of conventional art, a kind of PARA FORMALDEHYDE PRILLS(91,95), benzene and ammonia at a lower temperature are provided all
There is the more highly selective and active sensitive material of catalytic luminescence.With this sensitive material make gas sensor background signal very
Small, the sensitivity of PARA FORMALDEHYDE PRILLS(91,95), benzene and ammonia is all improved a lot, can measure simultaneously trace formaldehyde, benzene and ammonia in air without
By the common interference that molecule coexists.
Sensitive material of the present invention is gold atom doping by Dy2O3、In2O3With the composite granule material of PbO composition
Material, preparation method are as follows:
Dysprosium salt is dissolved in the aqueous solution of malic acid that mass fraction is 10-15% and forms solution A, indium salts are dissolved in quality point
Solution B is formed in the aqueous citric acid solution that number is 15-20%, it is water-soluble that lead salt is dissolved in the tartaric acid that mass fraction is 12-18%
Solution C is formed in liquid；Gold chloride crystal is soluble in water, be warming up to 92 DEG C, temperature kept to continuously stir down, successively by solution A,
B and C is slowly dropped in this solution, and temperature is kept to continue stirring 2 hours, and agar powder is added and continues stirring to solution and clarifies,
It is cooled to room temperature to form gel；After the drying of this gel, it is warming up in chamber type electric resistance furnace with the speed for being no more than 2 DEG C per minute
It 220-250 DEG C, keeps this temperature 3-4 hours, continues to be warming up to 400-450 DEG C with the speed for being no more than 2 DEG C per minute, keep this
Temperature 2-3 hours, it is atom doped by Dy that cooled to room temperature obtains Au2O3、In2O3With the composite granule material of PbO composition
Material.
Wherein, dysprosium salt is the anhydride of dysprosium nitrate, dysprosium sulfate, dysprosium chloride, acetic acid dysprosium and oxalic acid dysprosium or one kind of hydrate
Or several mixtures, indium salts be inidum chloride, indium nitrate, indium sulfate, indium acetate and indium phosphate anhydride or hydrate one
Kind or several mixtures, lead salt are the anhydride of plumbi nitras, lead acetate and plumbous rhodanate or the one or more of hydrate
Mixture.
When composite sensitive material each component mass fraction obtained meets Au (0.5-2%), Dy2O3(5-8%), In2O3
When (35-47%) and PbO (50-60%), for having as the catalytic luminescence sensitive material of trace formaldehyde, benzene and ammonia in air
Very high sensitivity and selectivity.
Specific embodiment
Embodiment 1
Six water dysprosium nitrates are dissolved in the aqueous solution of malic acid that mass fraction is 10% and form solution A, inidum chloride is dissolved in
Solution B is formed in the aqueous citric acid solution that mass fraction is 20%, plumbi nitras is dissolved in the winestone sour water that mass fraction is 12%
Solution C is formed in solution；Gold chloride crystal is soluble in water, 92 DEG C are warming up to, keeps temperature to continuously stir down, successively by solution
A, B and C is slowly dropped in this solution, and temperature is kept to continue stirring 2 hours, and agar powder is added and continues to stir clear to solution
Clearly, it is cooled to room temperature to form gel；After the drying of this gel, it is no more than 2 DEG C of speed liter per minute in chamber type electric resistance furnace
Temperature keeps this temperature 3 hours to 225 DEG C, continues to be warming up to 400 DEG C with the speed for being no more than 2 DEG C per minute, keeps this temperature 3
Hour, it is atom doped by Dy that cooled to room temperature obtains Au2O3、In2O3With the composite powder material of PbO composition.
Analysis: carrying out constituent analysis to composite powder material, and measuring mass percent is 0.7%Au, 6.3%Dy2O3、
41.5%In2O3And 51.5%PbO.
Using: using this powder body material as detection formaldehyde, the sensitive material of benzene and ammonia, the range of linearity is formaldehyde 0.05-
37mg/m3, benzene 0.5-56mg/m3With ammonia 0.5-47mg/m3, detect and be limited to formaldehyde 0.02mg/m3, benzene 0.2mg/m3With ammonia 0.2mg/
m3, common concurrent do not interfere with.
Embodiment 2
Eight water dysprosium sulfates are dissolved in the aqueous solution of malic acid that mass fraction is 11% and form solution A, by nitrate trihydrate indium
It is dissolved in the aqueous citric acid solution that mass fraction is 19% and forms solution B, it is 13% that acetate trihydrate lead, which is dissolved in mass fraction,
Solution C is formed in aqueous tartaric acid solution；Gold chloride crystal is soluble in water, 92 DEG C are warming up to, temperature is kept to continuously stir down, according to
It is secondary that solution A, B and C are slowly dropped in this solution, it keeps temperature to continue stirring 2 hours, agar powder is added and continues stirring extremely
Solution clarification, is cooled to room temperature to form gel；After the drying of this gel, to be no more than 2 DEG C per minute in chamber type electric resistance furnace
Speed is warming up to 230 DEG C, keeps this temperature 4 hours, continues to be warming up to 450 DEG C with the speed for being no more than 2 DEG C per minute, keeps this
Temperature 2 hours, it is atom doped by Dy that cooled to room temperature obtains Au2O3、In2O3With the composite powder material of PbO composition.
Analysis: carrying out constituent analysis to composite powder material, and measuring mass percent is 1.5%Au, 7.2%Dy2O3、
35.3%In2O3And 56.0%PbO.
Using: using this powder body material as detection formaldehyde, the sensitive material of benzene and ammonia, the range of linearity is formaldehyde 0.05-
35mg/m3, benzene 0.5-58mg/m3With ammonia 0.5-51mg/m3, detect and be limited to formaldehyde 0.02mg/m3, benzene 0.2mg/m3With ammonia 0.2mg/
m3, common concurrent do not interfere with.
Embodiment 3
Six water dysprosium chlorides are dissolved in the aqueous solution of malic acid that mass fraction is 12% and form solution A, by five water indium sulfates
It is dissolved in the aqueous citric acid solution that mass fraction is 18% with six water acetic acid indiums and forms solution B, plumbous rhodanate is dissolved in quality point
Solution C is formed in the aqueous tartaric acid solution that number is 15%；Gold chloride crystal is soluble in water, 92 DEG C are warming up to, temperature is kept to connect
Under continuous stirring, successively solution A, B and C are slowly dropped in this solution, temperature is kept to continue stirring 2 hours, agar powder is added
And continue stirring to solution and clarify, it is cooled to room temperature to form gel；After the drying of this gel, with per minute in chamber type electric resistance furnace
Speed no more than 2 DEG C is warming up to 235 DEG C, keeps this temperature 4 hours, continues to be warming up to the speed for being no more than 2 DEG C per minute
420 DEG C, keep this temperature 2.5 hours, it is atom doped by Dy that cooled to room temperature obtains Au2O3、In2O3With PbO composition
Composite powder material.
Analysis: carrying out constituent analysis to composite powder material, and measuring mass percent is 1.6%Au, 5.5%Dy2O3、
39.7%In2O3And 53.2%PbO.
Using: using this powder body material as detection formaldehyde, the sensitive material of benzene and ammonia, the range of linearity is formaldehyde 0.06-
39mg/m3, benzene 0.5-55mg/m3With ammonia 0.6-48mg/m3, detect and be limited to formaldehyde 0.03mg/m3, benzene 0.2mg/m3With ammonia 0.3mg/
m3, common concurrent do not interfere with.
Embodiment 4
Eight water dysprosium sulfates and six water dysprosium chlorides are dissolved in the aqueous solution of malic acid that mass fraction is 13% and form solution A,
Five water indium sulfates are dissolved in the aqueous citric acid solution that mass fraction is 17% and form solution B, by acetate trihydrate lead and thiocyanic acid
Lead, which is dissolved in the aqueous tartaric acid solution that mass fraction is 16%, forms solution C；Gold chloride crystal is soluble in water, it is warming up to 92
DEG C, it keeps temperature to continuously stir down, successively solution A, B and C is slowly dropped in this solution, keep temperature to continue stirring 2 small
When, agar powder is added and continues stirring to solution and clarifies, is cooled to room temperature to form gel；After the drying of this gel, in box electricity
240 DEG C are warming up to the speed for being no more than 2 DEG C per minute in resistance furnace, keeps this temperature 3.5 hours, is continued to be no more than per minute
2 DEG C of speed is warming up to 430 DEG C, keeps this temperature 2.5 hours, and it is atom doped by Dy that cooled to room temperature obtains Au2O3、
In2O3With the composite powder material of PbO composition.
Analysis: carrying out constituent analysis to composite powder material, and measuring mass percent is 1.0%Au, 6.7%Dy2O3、
42.2%In2O3And 50.1%PbO.
Using: using this powder body material as detection formaldehyde, the sensitive material of benzene and ammonia, the range of linearity is formaldehyde 0.05-
32mg/m3, benzene 0.5-51mg/m3With ammonia 0.5-46mg/m3, detect and be limited to formaldehyde 0.02mg/m3, benzene 0.2mg/m3With ammonia 0.2mg/
m3, common concurrent do not interfere with.
Embodiment 5
Five water acetic acid dysprosiums are dissolved in the aqueous solution of malic acid that mass fraction is 14% and form solution A, by six water acetic acid indiums
It is dissolved in the aqueous citric acid solution that mass fraction is 16% and forms solution B, plumbi nitras and plumbous rhodanate, which are dissolved in mass fraction, is
Solution C is formed in 17% aqueous tartaric acid solution；Gold chloride crystal is soluble in water, 92 DEG C are warming up to, temperature is kept continuously to stir
Mix down, successively solution A, B and C be slowly dropped in this solution, keep temperature continue stirring 2 hours, be added agar powder and after
Continuous stirring to solution is clarified, and is cooled to room temperature to form gel；After the drying of this gel, not surpass per minute in chamber type electric resistance furnace
It crosses 2 DEG C of speed and is warming up to 245 DEG C, keep this temperature 3 hours, continue to be warming up to 410 with the speed for being no more than 2 DEG C per minute
DEG C, keep this temperature 3 hours, it is atom doped by Dy that cooled to room temperature obtains Au2O3、In2O3It is formed with PbO compound
Powder body material.
Analysis: carrying out constituent analysis to composite powder material, and measuring mass percent is 0.8%Au, 7.5%Dy2O3、
38.4%In2O3And 53.3%PbO.
Using: using this powder body material as detection formaldehyde, the sensitive material of benzene and ammonia, the range of linearity is formaldehyde 0.05-
40mg/m3, benzene 0.5-52mg/m3With ammonia 0.5-49mg/m3, detect and be limited to formaldehyde 0.02mg/m3, benzene 0.2mg/m3With ammonia 0.2mg/
m3, common concurrent do not interfere with.
Embodiment 6
Ten water plant acid dysprosiums are dissolved in the aqueous solution of malic acid that mass fraction is 15% and form solution A, indium phosphate is dissolved in
Solution B is formed in the aqueous citric acid solution that mass fraction is 15%, acetate trihydrate lead is dissolved in the winestone that mass fraction is 18%
Solution C is formed in aqueous acid；Gold chloride crystal is soluble in water, 92 DEG C are warming up to, temperature is kept to continuously stir down, successively will
Solution A, B and C are slowly dropped in this solution, and temperature is kept to continue stirring 2 hours, and agar powder is added and continues stirring to solution
Clarification, is cooled to room temperature to form gel；After the drying of this gel, it is no more than 2 DEG C of speed per minute in chamber type electric resistance furnace
250 DEG C are warming up to, keeps this temperature 4 hours, continues to be warming up to 425 DEG C with the speed for being no more than 2 DEG C per minute, keeps this temperature
2.5 hours, it is atom doped by Dy that cooled to room temperature obtains Au2O3、In2O3With the composite powder material of PbO composition.
Analysis: carrying out constituent analysis to composite powder material, and measuring mass percent is 0.6%Au, 5.1%Dy2O3、
36.1%In2O3And 58.2%PbO.
Using: using this powder body material as detection formaldehyde, the sensitive material of benzene and ammonia, the range of linearity is formaldehyde 0.04-
33mg/m3, benzene 0.4-50mg/m3With ammonia 0.5-51mg/m3, detect and be limited to formaldehyde 0.02mg/m3, benzene 0.2mg/m3With ammonia 0.2mg/
m3, common concurrent do not interfere with.
Claims (2)
1. the catalytic luminescence sensitive material of low temperature formaldehyde, benzene and ammonia, it is characterized in that gold atom doping by Dy2O3、In2O3And PbO
The composite powder material of composition, wherein the mass percent range of each component is 0.5-2%Au, 5-8%Dy2O3, 35-47%
In2O3And 50-60%PbO, preparation method are: dysprosium salt being dissolved in the aqueous solution of malic acid that mass fraction is 10-15% and is formed
Indium salts are dissolved in the aqueous citric acid solution that mass fraction is 15-20% and form solution B, lead salt is dissolved in mass fraction by solution A
To form solution C in the aqueous tartaric acid solution of 12-18%；Gold chloride crystal is soluble in water, 92 DEG C are warming up to, temperature is kept to connect
Under continuous stirring, successively solution A, B and C are slowly dropped in this solution, temperature is kept to continue stirring 2 hours, agar powder is added
And continue stirring to solution and clarify, it is cooled to room temperature to form gel；After the drying of this gel, with per minute in chamber type electric resistance furnace
Speed no more than 2 DEG C is warming up to 220-250 DEG C, keeps this temperature 3-4 hours, continues to be no more than 2 DEG C of speed per minute
It is warming up to 400-450 DEG C, keeps this temperature 2-3 hours, it is atom doped by Dy that cooled to room temperature obtains Au2O3、In2O3
With the composite powder material of PbO composition.
2. the catalytic luminescence sensitive material of low temperature formaldehyde according to claim 1, benzene and ammonia, it is characterized in that the dysprosium salt
It is the anhydride of dysprosium nitrate, dysprosium sulfate, dysprosium chloride, acetic acid dysprosium and oxalic acid dysprosium or one or more of mixtures of hydrate, indium
Salt is the mixtures of the anhydride of inidum chloride, indium nitrate, indium sulfate, indium acetate and indium phosphate or the one or more of hydrate,
Lead salt is the anhydride of plumbi nitras, lead acetate and plumbous rhodanate or one or more of mixtures of hydrate.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910265321.7A CN110095559B (en) | 2019-04-03 | 2019-04-03 | Catalytic luminous sensitive material of low-temperature formaldehyde, benzene and ammonia |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910265321.7A CN110095559B (en) | 2019-04-03 | 2019-04-03 | Catalytic luminous sensitive material of low-temperature formaldehyde, benzene and ammonia |
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| CN110095559B CN110095559B (en) | 2021-09-14 |
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| CN110095559B (en) | 2021-09-14 |
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