CN113933449A - Low-temperature catalytic luminescence sensitive material of trimethylamine - Google Patents
Low-temperature catalytic luminescence sensitive material of trimethylamine Download PDFInfo
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- CN113933449A CN113933449A CN202010666470.7A CN202010666470A CN113933449A CN 113933449 A CN113933449 A CN 113933449A CN 202010666470 A CN202010666470 A CN 202010666470A CN 113933449 A CN113933449 A CN 113933449A
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- yttrium
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- dysprosium
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- 239000000463 material Substances 0.000 title claims abstract description 55
- GETQZCLCWQTVFV-UHFFFAOYSA-N trimethylamine Chemical compound CN(C)C GETQZCLCWQTVFV-UHFFFAOYSA-N 0.000 title claims abstract description 48
- 230000003197 catalytic effect Effects 0.000 title claims abstract description 8
- 238000004020 luminiscence type Methods 0.000 title claims abstract description 7
- 239000000843 powder Substances 0.000 claims abstract description 44
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims abstract description 27
- NLQFUUYNQFMIJW-UHFFFAOYSA-N dysprosium(III) oxide Inorganic materials O=[Dy]O[Dy]=O NLQFUUYNQFMIJW-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000002131 composite material Substances 0.000 claims abstract description 26
- 239000000499 gel Substances 0.000 claims abstract description 16
- 229920001817 Agar Polymers 0.000 claims abstract description 8
- 239000002253 acid Substances 0.000 claims abstract description 8
- 239000008272 agar Substances 0.000 claims abstract description 8
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims abstract description 7
- 239000008103 glucose Substances 0.000 claims abstract description 7
- 150000000703 Cerium Chemical class 0.000 claims abstract description 5
- 150000000914 Dysprosium Chemical class 0.000 claims abstract description 5
- 150000003746 yttrium Chemical class 0.000 claims abstract description 5
- 238000002360 preparation method Methods 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims description 41
- 239000000243 solution Substances 0.000 claims description 28
- 238000010438 heat treatment Methods 0.000 claims description 26
- 239000007864 aqueous solution Substances 0.000 claims description 21
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 21
- 238000001816 cooling Methods 0.000 claims description 21
- 239000000203 mixture Substances 0.000 claims description 16
- BJEPYKJPYRNKOW-REOHCLBHSA-N (S)-malic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O BJEPYKJPYRNKOW-REOHCLBHSA-N 0.000 claims description 7
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 7
- 239000001630 malic acid Substances 0.000 claims description 7
- 235000011090 malic acid Nutrition 0.000 claims description 7
- 238000000643 oven drying Methods 0.000 claims description 7
- 238000010992 reflux Methods 0.000 claims description 7
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 6
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims description 4
- OBOSXEWFRARQPU-UHFFFAOYSA-N 2-n,2-n-dimethylpyridine-2,5-diamine Chemical compound CN(C)C1=CC=C(N)C=N1 OBOSXEWFRARQPU-UHFFFAOYSA-N 0.000 claims description 3
- 229910002651 NO3 Inorganic materials 0.000 claims description 3
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 3
- VYLVYHXQOHJDJL-UHFFFAOYSA-K cerium trichloride Chemical compound Cl[Ce](Cl)Cl VYLVYHXQOHJDJL-UHFFFAOYSA-K 0.000 claims description 3
- 239000002245 particle Substances 0.000 claims description 3
- 229910000164 yttrium(III) phosphate Inorganic materials 0.000 claims description 3
- UXBZSSBXGPYSIL-UHFFFAOYSA-K yttrium(iii) phosphate Chemical compound [Y+3].[O-]P([O-])([O-])=O UXBZSSBXGPYSIL-UHFFFAOYSA-K 0.000 claims description 3
- WQXKGOOORHDGFP-UHFFFAOYSA-N 1,2,4,5-tetrafluoro-3,6-dimethoxybenzene Chemical compound COC1=C(F)C(F)=C(OC)C(F)=C1F WQXKGOOORHDGFP-UHFFFAOYSA-N 0.000 claims description 2
- MAYVZUQEFSJDHA-UHFFFAOYSA-N 1,5-bis(methylsulfanyl)naphthalene Chemical compound C1=CC=C2C(SC)=CC=CC2=C1SC MAYVZUQEFSJDHA-UHFFFAOYSA-N 0.000 claims description 2
- NGDQQLAVJWUYSF-UHFFFAOYSA-N 4-methyl-2-phenyl-1,3-thiazole-5-sulfonyl chloride Chemical compound S1C(S(Cl)(=O)=O)=C(C)N=C1C1=CC=CC=C1 NGDQQLAVJWUYSF-UHFFFAOYSA-N 0.000 claims description 2
- QXPQVUQBEBHHQP-UHFFFAOYSA-N 5,6,7,8-tetrahydro-[1]benzothiolo[2,3-d]pyrimidin-4-amine Chemical compound C1CCCC2=C1SC1=C2C(N)=NC=N1 QXPQVUQBEBHHQP-UHFFFAOYSA-N 0.000 claims description 2
- 229960001759 cerium oxalate Drugs 0.000 claims description 2
- ZMZNLKYXLARXFY-UHFFFAOYSA-H cerium(3+);oxalate Chemical compound [Ce+3].[Ce+3].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O ZMZNLKYXLARXFY-UHFFFAOYSA-H 0.000 claims description 2
- VGBWDOLBWVJTRZ-UHFFFAOYSA-K cerium(3+);triacetate Chemical compound [Ce+3].CC([O-])=O.CC([O-])=O.CC([O-])=O VGBWDOLBWVJTRZ-UHFFFAOYSA-K 0.000 claims description 2
- OZECDDHOAMNMQI-UHFFFAOYSA-H cerium(3+);trisulfate Chemical compound [Ce+3].[Ce+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O OZECDDHOAMNMQI-UHFFFAOYSA-H 0.000 claims description 2
- VZDYWEUILIUIDF-UHFFFAOYSA-J cerium(4+);disulfate Chemical compound [Ce+4].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O VZDYWEUILIUIDF-UHFFFAOYSA-J 0.000 claims description 2
- 229910000355 cerium(IV) sulfate Inorganic materials 0.000 claims description 2
- KACTUDRDWYCYMT-UHFFFAOYSA-H dysprosium(3+);oxalate Chemical compound [Dy+3].[Dy+3].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O KACTUDRDWYCYMT-UHFFFAOYSA-H 0.000 claims description 2
- FLWXWKDFOLALOB-UHFFFAOYSA-H dysprosium(3+);trisulfate Chemical compound [Dy+3].[Dy+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O FLWXWKDFOLALOB-UHFFFAOYSA-H 0.000 claims description 2
- NFSAPTWLWWYADB-UHFFFAOYSA-N n,n-dimethyl-1-phenylethane-1,2-diamine Chemical compound CN(C)C(CN)C1=CC=CC=C1 NFSAPTWLWWYADB-UHFFFAOYSA-N 0.000 claims description 2
- IBSDADOZMZEYKD-UHFFFAOYSA-H oxalate;yttrium(3+) Chemical compound [Y+3].[Y+3].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O IBSDADOZMZEYKD-UHFFFAOYSA-H 0.000 claims description 2
- 229910000347 yttrium sulfate Inorganic materials 0.000 claims description 2
- RTAYJOCWVUTQHB-UHFFFAOYSA-H yttrium(3+);trisulfate Chemical compound [Y+3].[Y+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RTAYJOCWVUTQHB-UHFFFAOYSA-H 0.000 claims description 2
- 150000008064 anhydrides Chemical class 0.000 claims 3
- 239000011540 sensing material Substances 0.000 claims 1
- 230000035945 sensitivity Effects 0.000 abstract description 4
- 239000012266 salt solution Substances 0.000 abstract 1
- 238000001514 detection method Methods 0.000 description 8
- 238000004458 analytical method Methods 0.000 description 7
- 238000001035 drying Methods 0.000 description 6
- 230000005540 biological transmission Effects 0.000 description 5
- 230000002452 interceptive effect Effects 0.000 description 5
- 239000000956 alloy Substances 0.000 description 4
- 229910045601 alloy Inorganic materials 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 150000004677 hydrates Chemical class 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 239000011858 nanopowder Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 238000004817 gas chromatography Methods 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- UBOOKRVGOBKDMM-UHFFFAOYSA-N 3h-imidazo[4,5-c]pyridine Chemical compound C1=NC=C2NC=NC2=C1 UBOOKRVGOBKDMM-UHFFFAOYSA-N 0.000 description 1
- 241000251468 Actinopterygii Species 0.000 description 1
- 238000002479 acid--base titration Methods 0.000 description 1
- 238000012271 agricultural production Methods 0.000 description 1
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 1
- BYCKXMUEODWQNZ-UHFFFAOYSA-H cerium(3+);oxalate;decahydrate Chemical compound O.O.O.O.O.O.O.O.O.O.[Ce+3].[Ce+3].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O BYCKXMUEODWQNZ-UHFFFAOYSA-H 0.000 description 1
- YQFSZFSGFIVQDY-UHFFFAOYSA-K cerium(3+);triacetate;pentahydrate Chemical compound O.O.O.O.O.[Ce+3].CC([O-])=O.CC([O-])=O.CC([O-])=O YQFSZFSGFIVQDY-UHFFFAOYSA-K 0.000 description 1
- QQZMWMKOWKGPQY-UHFFFAOYSA-N cerium(3+);trinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O QQZMWMKOWKGPQY-UHFFFAOYSA-N 0.000 description 1
- PQBKXYUMEMUVIH-UHFFFAOYSA-H cerium(3+);trisulfate;octahydrate Chemical compound O.O.O.O.O.O.O.O.[Ce+3].[Ce+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O PQBKXYUMEMUVIH-UHFFFAOYSA-H 0.000 description 1
- MEXSQFDSPVYJOM-UHFFFAOYSA-J cerium(4+);disulfate;tetrahydrate Chemical compound O.O.O.O.[Ce+4].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O MEXSQFDSPVYJOM-UHFFFAOYSA-J 0.000 description 1
- 238000001212 derivatisation Methods 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- -1 dysprosium acetate pentahydrate Chemical compound 0.000 description 1
- ULOOLRKTTNPQEM-UHFFFAOYSA-H dysprosium(3+);oxalate;decahydrate Chemical compound O.O.O.O.O.O.O.O.O.O.[Dy+3].[Dy+3].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O ULOOLRKTTNPQEM-UHFFFAOYSA-H 0.000 description 1
- DCKWZDOAGNMKMX-UHFFFAOYSA-N dysprosium(3+);trinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Dy+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O DCKWZDOAGNMKMX-UHFFFAOYSA-N 0.000 description 1
- NCCPVLRLAAMOQH-UHFFFAOYSA-H dysprosium(3+);trisulfate;octahydrate Chemical compound O.O.O.O.O.O.O.O.[Dy+3].[Dy+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O NCCPVLRLAAMOQH-UHFFFAOYSA-H 0.000 description 1
- 230000002740 effect on eyes Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 235000021323 fish oil Nutrition 0.000 description 1
- 235000013332 fish product Nutrition 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000003988 headspace gas chromatography Methods 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000004255 ion exchange chromatography Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 235000013372 meat Nutrition 0.000 description 1
- 230000002503 metabolic effect Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- CTXJKXXQOORSKU-UHFFFAOYSA-H oxalate;yttrium(3+);nonahydrate Chemical compound O.O.O.O.O.O.O.O.O.[Y+3].[Y+3].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O CTXJKXXQOORSKU-UHFFFAOYSA-H 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 210000002345 respiratory system Anatomy 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 230000000638 stimulation Effects 0.000 description 1
- HFEOHRWLEGXZHW-UHFFFAOYSA-K trichlorodysprosium;hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Cl-].[Dy+3] HFEOHRWLEGXZHW-UHFFFAOYSA-K 0.000 description 1
- AIQRTHPXPDTMBQ-UHFFFAOYSA-K yttrium(3+);triacetate;tetrahydrate Chemical compound O.O.O.O.[Y+3].CC([O-])=O.CC([O-])=O.CC([O-])=O AIQRTHPXPDTMBQ-UHFFFAOYSA-K 0.000 description 1
- QBAZWXKSCUESGU-UHFFFAOYSA-N yttrium(3+);trinitrate;hexahydrate Chemical compound O.O.O.O.O.O.[Y+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O QBAZWXKSCUESGU-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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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- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Analytical Chemistry (AREA)
- Molecular Biology (AREA)
- Physics & Mathematics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Catalysts (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
The invention relates to a low-temperature catalytic luminescence sensitive material of trimethylamine, which is characterized in that Pt is doped with Y2O3、CeO2And Dy2O3To form the composite powder material. The preparation method comprises the following steps: firstly, agar powder is added into yttrium salt, cerium salt and dysprosium salt solution to form gel, and then the gel is calcined by sections to obtain Y2O3、CeO2And Dy2O3The composite powder material is impregnated with chloroplatinic acid reduced by glucose to obtain Pt-doped Y2O3、CeO2And Dy2O3To form the composite powder material. The gas sensor made of the sensitive material provided by the invention can be used for measuring the trace trimethylamine in the air at a low temperature and high sensitivity without being interfered by other common coexisting molecules.
Description
Technical Field
The invention relates to a nano-sensitive material for monitoring trimethylamine, in particular to Y doped with Pt2O3、CeO2And Dy2O3A sensitive material composed of nano-powder belongs to the technical field of sensing.
Background
Trimethylamine belongs to gaseous pollutants, is colorless gas with fish oil odor at normal temperature (the fishy smell of fish products mainly comes from the trimethylamine), is flammable and explosive, has strong stimulation effect on eyes, nose, throat and respiratory tract of people, has large harm after long-term contact, and the existence and concentration of the trimethylamine are important standards for evaluating the food quality of meat and fish, are odor marks for representing certain metabolic defect diseases, are main objects for controlling environmental odor pollution and are key parameters for controlling the quality of certain industrial and agricultural production. Therefore, the accurate determination of the trimethylamine concentration is of great significance. The detection methods of trimethylamine are various, and the detection methods comprise an acid-base titration method and a Kjeldahl nitrogen distillation method which are simpler, but the analysis results of the two methods have large errors and are only used for preliminary determination; spectrophotometry, ion chromatography, high performance liquid chromatography, headspace gas chromatography, pre-column derivatization gas chromatography, direct injection gas chromatography, and the like have high precision and accurate detection, but have the disadvantages of complicated analysis steps, long time consumption and expensive equipment. The patent ZL201210170269.5 discloses a nanometer sensitive material for detecting trimethylamine, however, the temperature of the sensitive material exceeds 300 ℃, the background of heat radiation generated by the temperature can form a strong base line signal, and the strong base line can seriously affect the sensitivity of the catalytic luminescence sensor.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a sensitive material with higher selectivity and catalytic luminescence activity on trimethylamine at lower temperature. The trimethylamine gas sensor made of the sensitive material has small background, greatly improves the sensitivity to the trimethylamine, and can accurately measure the trace trimethylamine in the air without being interfered by common coexisting molecules.
The sensitive material of the invention is Y doped with Pt2O3、CeO2And Dy2O3The preparation method of the nano-powder comprises the following steps: dissolving yttrium salt in 30-35% citric acid aqueous solution by mass percent, stirring at room temperature for 1 hour to form solution A, dissolving cerium salt and dysprosium salt in 40-45% malic acid aqueous solution by mass percent, stirring at 50 ℃ for 1 hour to form solution B, slowly adding the solution A into the solution B, heating to 90-95 ℃, continuing stirring for 2-3 hours, keeping the temperature, adding agar powder, continuing stirring for 3 hours, cooling to room temperature to form gel, drying the gel, heating to 280-300 ℃ in a box-type resistance furnace at a speed of not more than 2 ℃ per minute, keeping the temperature for 3-4 hours, continuing heating to 380-400 ℃ at a speed of not more than 2 ℃ per minute, keeping the temperature for 2-3 hours, and naturally cooling to room temperature to obtain the product Y2O3、CeO2And Dy2O3OfA composite powder material; adding chloroplatinic acid into 30% glucose aqueous solution, heating and refluxing for 2-4 hr, naturally cooling to room temperature, adding the above composite powder material under continuous stirring, stirring for 2 hr, standing overnight, filtering, and oven drying to obtain Pt-doped Y2O3、CeO2And Dy2O3To form the composite powder material.
The yttrium salt is one or a mixture of more of anhydrous substances or hydrates of yttrium acetate, yttrium oxalate, yttrium nitrate, yttrium sulfate, yttrium phosphate and yttrium chloride, the cerium salt is one or a mixture of more of anhydrous substances or hydrates of cerium acetate, cerium oxalate, cerium nitrate, ammonium ceric nitrate, cerium sulfate, ammonium ceric sulfate and cerium chloride, and the dysprosium salt is one or a mixture of more of anhydrous substances or hydrates of dysprosium nitrate, dysprosium sulfate, dysprosium chloride, dysprosium acetate and dysprosium oxalate.
When the grain diameter of the prepared nano powder is not more than 30nm, and each component meets the requirements of Pt (0.2-0.7%) and Y2O3（36-43%）、CeO2(30-35%) and Dy2O3(25-30%) has high sensitivity and selectivity when used as a sensitive material for monitoring trimethylamine.
Detailed Description
Example 1
Dissolving yttrium acetate tetrahydrate in a citric acid aqueous solution with the mass fraction of 30%, stirring at room temperature for 1 hour to form a solution A, dissolving cerium acetate pentahydrate and dysprosium nitrate hexahydrate in a malic acid aqueous solution with the mass fraction of 45%, stirring at 50 ℃ for 1 hour to form a solution B, slowly adding the solution A into the solution B, heating to 90 ℃, continuing stirring for 3 hours, keeping the temperature, adding agar powder, continuing stirring for 3 hours, cooling to room temperature to form gel, drying the gel, heating to 280 ℃ at a speed of not more than 2 ℃ per minute in a box-type resistance furnace, keeping the temperature for 4 hours, continuing heating to 380 ℃ at a speed of not more than 2 ℃ per minute, keeping the temperature for 3 hours, and naturally cooling to room temperature to obtain a product Y2O3、CeO2And Dy2O3Composite powder material; adding chloroplatinic acid into 30 mass percent of glucoseHeating and refluxing for 4 hours in the aqueous solution, naturally cooling to room temperature, adding the composite powder material under the continuous stirring state, continuously stirring for 2 hours, standing overnight, filtering, and drying to obtain Pt-doped Y2O3、CeO2And Dy2O3To form the composite powder material.
And (3) analysis: the maximum grain diameter of the powder material is not more than 28nm and the average grain diameter is about 15nm by a transmission electron microscope test; the composition was analyzed to find that the composition was 0.2% Pt and 41.3% Y2O3、30.4% CeO2And 28.1% Dy2O3。
The application comprises the following steps: the powder material is used as a sensitive material to measure trimethylamine in air, and the linear range is 0.8-140 mg/m3The detection limit can reach 0.3mg/m3The co-presence is not interfering.
Example 2
Dissolving yttrium oxalate nonahydrate in a citric acid aqueous solution with the mass fraction of 31%, stirring at room temperature for 1 hour to form a solution A, dissolving cerium oxalate decahydrate, cerium nitrate hexahydrate and dysprosium sulfate octahydrate in a malic acid aqueous solution with the mass fraction of 44%, stirring at 50 ℃ for 1 hour to form a solution B, slowly adding the solution A into the solution B, heating to 92 ℃, continuing stirring for 3 hours, keeping the temperature, adding agar powder, continuing stirring for 3 hours, cooling to room temperature to form gel, drying the gel, heating to 285 ℃ at the speed of not more than 2 ℃ per minute in a box-type resistance furnace, keeping the temperature for 4 hours, continuing heating to 385 ℃ at the speed of not more than 2 ℃ per minute, keeping the temperature for 3 hours, and naturally cooling to room temperature to obtain a product Y2O3、CeO2And Dy2O3Composite powder material; adding chloroplatinic acid into 30% glucose aqueous solution, heating and refluxing for 3 hr, naturally cooling to room temperature, adding the composite powder material under continuous stirring, stirring for 2 hr, standing overnight, filtering, and oven drying to obtain Pt-doped Y2O3、CeO2And Dy2O3To form the composite powder material.
And (3) analysis: this is measured by transmission electron microscopyA powder material having a maximum particle size of not more than 30nm and an average particle size of about 18 nm; the composition of the alloy was analyzed to find that the alloy had a composition of 0.6% Pt and 38.5% Y2O3、34.3% CeO2And 26.6% Dy2O3。
The application comprises the following steps: the powder material is used as a sensitive material to measure trimethylamine in air, and the linear range is 0.7-120 mg/m3The detection limit can reach 0.1mg/m3The co-presence is not interfering.
Example 3
Dissolving yttrium nitrate hexahydrate in 32 mass percent citric acid aqueous solution, stirring at room temperature for 1 hour to form solution A, dissolving ammonium ceric nitrate, cerium sulfate octahydrate and dysprosium chloride hexahydrate in 43 mass percent malic acid aqueous solution, stirring at 50 ℃ for 1 hour to form solution B, slowly adding solution A into solution B, heating to 93 ℃, continuing stirring for 3 hours, keeping the temperature, adding agar powder, continuing stirring for 3 hours, cooling to room temperature to form gel, drying the gel, heating to 290 ℃ at a speed of not more than 2 ℃ per minute in a box-type resistance furnace, keeping the temperature for 3 hours, continuing heating to 390 ℃ at a speed of not more than 2 ℃ per minute, keeping the temperature for 3 hours, naturally cooling to room temperature to obtain Y2O3、CeO2And Dy2O3Composite powder material; adding chloroplatinic acid into 30% glucose aqueous solution, heating and refluxing for 2 hr, naturally cooling to room temperature, adding the composite powder material under continuous stirring, stirring for 2 hr, standing overnight, filtering, and oven drying to obtain Pt-doped Y2O3、CeO2And Dy2O3To form the composite powder material.
And (3) analysis: the powder material is tested by a transmission electron microscope, the maximum grain diameter is not more than 30nm, and the average grain diameter is about 20 nm; the composition of the alloy was analyzed to find that the alloy had a composition of 0.3% Pt and 36.6% Y2O3、33.5% CeO2And 29.6% Dy2O3。
The application comprises the following steps: the powder material is used as a sensitive material to measure trimethylamine in air, and the linear range is 0.8-117 mg/m3Detection limitCan reach 0.4mg/m3The co-presence is not interfering.
Example 4
Dissolving yttrium sulfate octahydrate in a citric acid aqueous solution with the mass fraction of 33% and stirring at room temperature for 1 hour to form a solution A, dissolving ammonium ceric sulfate tetrahydrate and dysprosium acetate pentahydrate in a malic acid aqueous solution with the mass fraction of 42% and stirring at the temperature of 50 ℃ for 1 hour to form a solution B, slowly adding the solution A into the solution B, heating to 94 ℃ and continuing stirring for 2 hours, keeping the temperature, adding agar powder, continuing stirring for 3 hours, cooling to room temperature to form gel, drying the gel, heating to 295 ℃ at the speed of not more than 2 ℃ per minute in a box-type resistance furnace, keeping the temperature for 3 hours, continuing heating to 395 ℃ at the speed of not more than 2 ℃ per minute, keeping the temperature for 2 hours, and naturally cooling to room temperature to obtain a Y product2O3、CeO2And Dy2O3Composite powder material; adding chloroplatinic acid into 30% glucose aqueous solution, heating and refluxing for 3 hr, naturally cooling to room temperature, adding the composite powder material under continuous stirring, stirring for 2 hr, standing overnight, filtering, and oven drying to obtain Pt-doped Y2O3、CeO2And Dy2O3To form the composite powder material.
And (3) analysis: the maximum grain diameter of the powder material is not more than 29nm and the average grain diameter is about 20nm by a transmission electron microscope test; the composition was analyzed to find that the composition was 0.7% Pt and 39.4% Y2O3、32.7% CeO2And 27.2% Dy2O3。
The application comprises the following steps: the powder material is used as a sensitive material to measure trimethylamine in air, and the linear range is 0.6-102 mg/m3The detection limit can reach 0.2mg/m3The co-presence is not interfering.
Example 5
Dissolving yttrium phosphate and yttrium chloride in 35% citric acid aqueous solution by mass fraction, stirring at room temperature for 1 hour to form solution A, dissolving cerium chloride and dysprosium oxalate decahydrate in 40% malic acid aqueous solution by mass fraction, stirring at 50 ℃ for 1 hour to form solution B, and slowly adding solution A into solution BHeating to 95 deg.C, stirring for 2 hr, maintaining the temperature, adding agar powder, stirring for 3 hr, cooling to room temperature to form gel, oven drying the gel, heating to 300 deg.C in a box-type resistance furnace at a rate of 2 deg.C/min, maintaining the temperature for 3 hr, heating to 400 deg.C at a rate of 2 deg.C/min, maintaining the temperature for 2 hr, and naturally cooling to room temperature to obtain the final product Y2O3、CeO2And Dy2O3Composite powder material; adding chloroplatinic acid into 30% glucose aqueous solution, heating and refluxing for 4 hr, naturally cooling to room temperature, adding the composite powder material under continuous stirring, stirring for 2 hr, standing overnight, filtering, and oven drying to obtain Pt-doped Y2O3、CeO2And Dy2O3To form the composite powder material.
And (3) analysis: the maximum grain diameter of the powder material is not more than 26nm and the average grain diameter is about 15nm by a transmission electron microscope test; the composition was analyzed to find that the composition was 0.5% Pt and 42.7% Y2O3、31.8% CeO2And 25.0% Dy2O3。
The application comprises the following steps: the powder material is used as a sensitive material to measure trimethylamine in air, and the linear range is 0.7-99 mg/m3The detection limit can reach 0.3mg/m3The co-presence is not interfering.
Claims (3)
1. A low-temperature catalytic luminescence sensitive material of trimethylamine is characterized in that: doped with Pt by Y2O3、CeO2And Dy2O3The composite powder material comprises the following components in percentage by mass 0.2-0.7% of Pt and 36-43% of Y2O3、30-35% CeO2And 25-30% Dy2O3The preparation method comprises the following steps: dissolving yttrium salt in 30-35% citric acid aqueous solution, stirring at room temperature for 1 hr to form solution A, dissolving cerium salt and dysprosium salt in 40-45% malic acid aqueous solution, stirring at 50 deg.C for 1 hr to form solution B, slowly adding solution A into solution B, heating to 90-95 deg.C, and stirringStirring for 2-3 hr, maintaining the temperature, adding agar powder, stirring for 3 hr, cooling to room temperature to form gel, stoving the gel, heating to 280-300 deg.c in a box-type resistance furnace at 2 deg.c/min, maintaining the temperature for 3-4 hr, heating to 380-400 deg.c at 2 deg.c/min, maintaining the temperature for 2-3 hr, and naturally cooling to room temperature to obtain the Y-shaped food2O3、CeO2And Dy2O3Composite powder material; adding chloroplatinic acid into 30% glucose aqueous solution, heating and refluxing for 2-4 hr, naturally cooling to room temperature, adding the above composite powder material under continuous stirring, stirring for 2 hr, standing overnight, filtering, and oven drying to obtain Pt-doped Y2O3、CeO2And Dy2O3To form the composite powder material.
2. The trimethylamine low-temperature catalytic luminescent sensitive material as claimed in claim 1, wherein the particle size of the composite powder material is not more than 30 nm.
3. The low-temperature catalytic luminescence sensing material of trimethylamine according to claim 1, wherein the yttrium salt is one or a mixture of more of anhydride or hydrate of yttrium acetate, yttrium oxalate, yttrium nitrate, yttrium sulfate, yttrium phosphate and yttrium chloride, the cerium salt is one or a mixture of more of anhydride or hydrate of cerium acetate, cerium oxalate, cerium nitrate, ammonium ceric nitrate, cerium sulfate, ammonium ceric sulfate and cerium chloride, and the dysprosium salt is one or a mixture of more of anhydride or hydrate of dysprosium nitrate, dysprosium sulfate, dysprosium chloride, dysprosium acetate and dysprosium oxalate.
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| CN103487473A (en) * | 2013-09-26 | 2014-01-01 | 内蒙古科技大学 | Rare earth modified zinc oxide gas sensor and preparation method thereof |
| CN108519459A (en) * | 2018-03-29 | 2018-09-11 | 北京联合大学 | The sensitive material of low temperature formaldehyde, sulfur dioxide and trimethylamine |
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