CN110095559B - Catalytic luminous sensitive material of low-temperature formaldehyde, benzene and ammonia - Google Patents
Catalytic luminous sensitive material of low-temperature formaldehyde, benzene and ammonia Download PDFInfo
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- CN110095559B CN110095559B CN201910265321.7A CN201910265321A CN110095559B CN 110095559 B CN110095559 B CN 110095559B CN 201910265321 A CN201910265321 A CN 201910265321A CN 110095559 B CN110095559 B CN 110095559B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- 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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G15/00—Compounds of gallium, indium or thallium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G21/00—Compounds of lead
- C01G21/02—Oxides
- C01G21/06—Lead monoxide (PbO)
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- 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
- G01—MEASURING; TESTING
- 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
- 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
Abstract
The invention relates to a catalytic luminescent sensitive material of low-temperature formaldehyde, benzene and ammonia, which is characterized in that gold atoms are doped with Dy2O3、In2O3And PbO. The preparation method comprises the following steps: sequentially adding a malic acid aqueous solution of dysprosium salt, a citric acid aqueous solution of indium salt and a tartaric acid aqueous solution of lead salt into a chloroauric acid aqueous solution, heating and stirring, adding agar powder, stirring to clarify, cooling to form gel, drying, roasting for two sections and naturally cooling to obtain Au atom-doped Dy2O3、In2O3And PbO. The gas sensor made of the sensitive material provided by the invention can be used for measuring trace formaldehyde, benzene and ammonia in the air at high sensitivity on site without being interfered by other common coexisting molecules.
Description
Technical Field
The invention relates to a low-temperature formaldehyde, benzene and ammonia catalytic luminescence sensitive material, in particular to a gold atom doped Dy2O3、In2O3And PbO, belonging to the sensing technical field.
Background
Because indoor decoration and various modern living goods are widely used to cause indoor air pollution to become more serious, formaldehyde (HCHO) is widely applied to products such as compression plates, coatings, paints, cosmetics, packaging materials and the like as an adhesive raw material, a disinfectant, a preservative and a finishing agent, and is continuously released into the air along with the use of the applied products. Benzene (C)6H6) Is a chemical raw material with aromatic odor, and is often used as a thinner of decorative coatings. Ammonia (NH)3) Is an alkaline gas having a strong pungent odor and is slowly released from the wall to which the construction antifreeze is applied, and thus formaldehyde, benzene and ammonia are main pollutants of indoor air. The methods for measuring formaldehyde, benzene and ammonia mainly include spectrophotometry, electrochemistry, chromatography, chemiluminescence, gas or liquid chromatography, ion chromatography and the like. These methods require prior enrichment and appropriate handling to complete the assay by the analytical instrument, and are therefore time consuming and not easily implemented on site.
The patent ZL201410605596.8 discloses a catalytic luminescence sensitive material for formaldehyde, benzene and ammonia in air, but the use temperature of the sensitive material exceeds 350 ℃, and the background of heat radiation generated by the temperature can form a strong base line signal, thereby seriously influencing the sensitivity of the 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 formaldehyde, benzene and ammonia at lower temperature. The gas sensor made of the sensitive material has small background signal, greatly improves the sensitivity to formaldehyde, benzene and ammonia, and can simultaneously measure the trace formaldehyde, benzene and ammonia in the air without being interfered by common coexisting molecules.
The sensitive material is Dy doped with gold atoms2O3、In2O3The preparation method of the composite powder material consisting of the PbO comprises the following steps:
dissolving dysprosium salt in a malic acid aqueous solution with the mass fraction of 10-15% to form a solution A, dissolving indium salt in a citric acid aqueous solution with the mass fraction of 15-20% to form a solution B, and dissolving lead salt in a tartaric acid aqueous solution with the mass fraction of 12-18% to form a solution C; dissolving chloroauric acid crystals in water, heating to 92 ℃, keeping the temperature under continuous stirring, slowly and dropwise adding the solution A, B and C into the solution in sequence, keeping the temperature under continuous stirring for 2 hours, adding agar powder, continuously stirring until the solution is clear, and cooling to room temperature to form gel; drying the gel, heating to 220-250 deg.C in a box-type resistance furnace at a speed of not more than 2 deg.C per minute, and maintaining the temperatureHeating to 400-450 deg.C at a rate not exceeding 2 deg.C per minute for 3-4 hr, maintaining the temperature for 2-3 hr, and naturally cooling to room temperature to obtain Au atom doped Dy2O3、In2O3And PbO.
The dysprosium salt is one or a mixture of a plurality of anhydrous substances or hydrates of dysprosium nitrate, dysprosium sulfate, dysprosium chloride, dysprosium acetate and dysprosium oxalate, the indium salt is one or a mixture of a plurality of anhydrous substances or hydrates of indium chloride, indium nitrate, indium sulfate, indium acetate and indium phosphate, and the lead salt is one or a mixture of a plurality of anhydrous substances or hydrates of lead nitrate, lead acetate and lead thiocyanate.
When the mass fractions of all the components of the prepared composite sensitive material meet the requirements of Au (0.5-2 percent) and Dy2O3(5-8％)、In2O3(35-47%) and PbO (50-60%), has high sensitivity and selectivity when used as catalytic luminescent sensitive material for trace formaldehyde, benzene and ammonia in air.
Detailed Description
Example 1
Dissolving dysprosium nitrate hexahydrate in a malic acid aqueous solution with the mass fraction of 10% to form a solution A, dissolving indium chloride in a citric acid aqueous solution with the mass fraction of 20% to form a solution B, and dissolving lead nitrate in a tartaric acid aqueous solution with the mass fraction of 12% to form a solution C; dissolving chloroauric acid crystals in water, heating to 92 ℃, keeping the temperature under continuous stirring, slowly and dropwise adding the solution A, B and C into the solution in sequence, keeping the temperature under continuous stirring for 2 hours, adding agar powder, continuously stirring until the solution is clear, and cooling to room temperature to form gel; drying the gel, heating to 225 deg.C in a box-type resistance furnace at a speed of not more than 2 deg.C per minute, maintaining the temperature for 3 hr, heating to 400 deg.C at a speed of not more than 2 deg.C per minute, maintaining the temperature for 3 hr, and naturally cooling to room temperature to obtain Au atom doped Dy2O3、In2O3And PbO.
And (3) analysis: the composite powder material is subjected to component analysis, and the mass percentage of the components is 0.7 percent of Au and 6.3 percent of Dy2O3、41.5％In2O3And 51.5% PbO.
The application comprises the following steps: the powder material is used as a sensitive material for detecting formaldehyde, benzene and ammonia, and the linear range of the powder material is 0.05-37mg/m of formaldehyde30.5-56mg/m of benzene3And ammonia 0.5-47mg/m3The detection limit is 0.02mg/m of formaldehyde30.2mg/m benzene3And ammonia 0.2mg/m3Common co-occurrences do not interfere.
Example 2
Dissolving dysprosium sulfate octahydrate in a malic acid aqueous solution with the mass fraction of 11% to form a solution A, dissolving indium nitrate trihydrate in a citric acid aqueous solution with the mass fraction of 19% to form a solution B, and dissolving lead acetate trihydrate in a tartaric acid aqueous solution with the mass fraction of 13% to form a solution C; dissolving chloroauric acid crystals in water, heating to 92 ℃, keeping the temperature under continuous stirring, slowly and dropwise adding the solution A, B and C into the solution in sequence, keeping the temperature under continuous stirring for 2 hours, adding agar powder, continuously stirring until the solution is clear, and cooling to room temperature to form gel; drying the gel, heating to 230 deg.C in a box-type resistance furnace at a speed of not more than 2 deg.C per minute, maintaining the temperature for 4 hr, heating to 450 deg.C at a speed of not more than 2 deg.C per minute, maintaining the temperature for 2 hr, and naturally cooling to room temperature to obtain Au atom doped Dy2O3、In2O3And PbO.
And (3) analysis: the composite powder material is subjected to component analysis, and the mass percentage of the components is 1.5 percent of Au and 7.2 percent of Dy2O3、35.3％In2O3And 56.0% PbO.
The application comprises the following steps: the powder material is used as a sensitive material for detecting formaldehyde, benzene and ammonia, and the linear range of the powder material is 0.05-35mg/m of formaldehyde30.5-58mg/m of benzene3And ammonia 0.5-51mg/m3The detection limit is 0.02mg/m of formaldehyde30.2mg/m benzene3And ammonia 0.2mg/m3Common co-occurrences do not interfere.
Example 3
Dissolving dysprosium chloride hexahydrate in a malic acid aqueous solution with the mass fraction of 12% to form a solution A, and dissolving dysprosium chloride hexahydrate in a malic acid aqueous solutionDissolving indium sulfate pentahydrate and indium acetate hexahydrate in a citric acid aqueous solution with the mass fraction of 18% to form a solution B, and dissolving lead thiocyanate in a tartaric acid aqueous solution with the mass fraction of 15% to form a solution C; dissolving chloroauric acid crystals in water, heating to 92 ℃, keeping the temperature under continuous stirring, slowly and dropwise adding the solution A, B and C into the solution in sequence, keeping the temperature under continuous stirring for 2 hours, adding agar powder, continuously stirring until the solution is clear, and cooling to room temperature to form gel; drying the gel, heating to 235 deg.C in a box-type resistance furnace at a speed of not more than 2 deg.C per minute, maintaining the temperature for 4 hr, heating to 420 deg.C at a speed of not more than 2 deg.C per minute, maintaining the temperature for 2.5 hr, and naturally cooling to room temperature to obtain Au atom-doped Dy2O3、In2O3And PbO.
And (3) analysis: the composite powder material is subjected to component analysis, and the mass percentage of the components is 1.6 percent of Au and 5.5 percent of Dy2O3、39.7％In2O3And 53.2% PbO.
The application comprises the following steps: the powder material is used as a sensitive material for detecting formaldehyde, benzene and ammonia, and the linear range of the powder material is 0.06-39mg/m of formaldehyde30.5-55mg/m of benzene3And ammonia 0.6-48mg/m3The detection limit is 0.03mg/m of formaldehyde30.2mg/m benzene3And ammonia 0.3mg/m3Common co-occurrences do not interfere.
Example 4
Dissolving dysprosium sulfate octahydrate and dysprosium chloride hexahydrate in a malic acid aqueous solution with the mass fraction of 13% to form a solution A, dissolving indium sulfate pentahydrate in a citric acid aqueous solution with the mass fraction of 17% to form a solution B, and dissolving lead acetate trihydrate and lead thiocyanate in a tartaric acid aqueous solution with the mass fraction of 16% to form a solution C; dissolving chloroauric acid crystals in water, heating to 92 ℃, keeping the temperature under continuous stirring, slowly and dropwise adding the solution A, B and C into the solution in sequence, keeping the temperature under continuous stirring for 2 hours, adding agar powder, continuously stirring until the solution is clear, and cooling to room temperature to form gel; drying the gel, heating to 240 deg.C in a box-type resistance furnace at a speed of not more than 2 deg.C per minute, and maintaining the temperature for 3.5 hrContinuously heating to 430 ℃ at the speed of not more than 2 ℃ per minute, keeping the temperature for 2.5 hours, and naturally cooling to room temperature to obtain the Au atom-doped Dy2O3、In2O3And PbO.
And (3) analysis: the composite powder material is subjected to component analysis, and the mass percentage of the components is 1.0 percent of Au and 6.7 percent of Dy2O3、42.2％In2O3And 50.1% PbO.
The application comprises the following steps: the powder material is used as a sensitive material for detecting formaldehyde, benzene and ammonia, and the linear range of the powder material is 0.05-32mg/m of formaldehyde30.5-51mg/m of benzene3And ammonia 0.5-46mg/m3The detection limit is 0.02mg/m of formaldehyde30.2mg/m benzene3And ammonia 0.2mg/m3Common co-occurrences do not interfere.
Example 5
Dissolving dysprosium pentahydrate acetate in a malic acid aqueous solution with the mass fraction of 14% to form a solution A, dissolving indium hexahydrate acetate in a citric acid aqueous solution with the mass fraction of 16% to form a solution B, and dissolving lead nitrate and lead thiocyanate in a tartaric acid aqueous solution with the mass fraction of 17% to form a solution C; dissolving chloroauric acid crystals in water, heating to 92 ℃, keeping the temperature under continuous stirring, slowly and dropwise adding the solution A, B and C into the solution in sequence, keeping the temperature under continuous stirring for 2 hours, adding agar powder, continuously stirring until the solution is clear, and cooling to room temperature to form gel; drying the gel, heating to 245 deg.C at a speed of not more than 2 deg.C per minute in a box-type resistance furnace, maintaining the temperature for 3 hr, heating to 410 deg.C at a speed of not more than 2 deg.C per minute, maintaining the temperature for 3 hr, and naturally cooling to room temperature to obtain Au atom doped Dy2O3、In2O3And PbO.
And (3) analysis: the composite powder material is subjected to component analysis, and the mass percentage of the components is 0.8 percent of Au and 7.5 percent of Dy2O3、38.4％In2O3And 53.3% PbO.
The application comprises the following steps: the powder material is used as a sensitive material for detecting formaldehyde, benzene and ammonia, and the linear range of the powder material is 0.0 percent of formaldehyde5-40mg/m30.5-52mg/m of benzene3And ammonia 0.5-49mg/m3The detection limit is 0.02mg/m of formaldehyde30.2mg/m benzene3And ammonia 0.2mg/m3Common co-occurrences do not interfere.
Example 6
Dissolving dysprosium oxalate decahydrate in a malic acid aqueous solution with the mass fraction of 15% to form a solution A, dissolving indium phosphate in a citric acid aqueous solution with the mass fraction of 15% to form a solution B, and dissolving lead acetate trihydrate in a tartaric acid aqueous solution with the mass fraction of 18% to form a solution C; dissolving chloroauric acid crystals in water, heating to 92 ℃, keeping the temperature under continuous stirring, slowly and dropwise adding the solution A, B and C into the solution in sequence, keeping the temperature under continuous stirring for 2 hours, adding agar powder, continuously stirring until the solution is clear, and cooling to room temperature to form gel; drying the gel, heating to 250 deg.C in a box-type resistance furnace at a speed of not more than 2 deg.C per minute, maintaining the temperature for 4 hr, heating to 425 deg.C at a speed of not more than 2 deg.C per minute, maintaining the temperature for 2.5 hr, and naturally cooling to room temperature to obtain Au atom-doped Dy2O3、In2O3And PbO.
And (3) analysis: the composite powder material is subjected to component analysis, and the mass percentage of the components is 0.6 percent of Au and 5.1 percent of Dy2O3、36.1％In2O3And 58.2% PbO.
The application comprises the following steps: the powder material is used as a sensitive material for detecting formaldehyde, benzene and ammonia, and the linear range of the powder material is 0.04-33mg/m of formaldehyde30.4-50mg/m of benzene3And ammonia 0.5-51mg/m3The detection limit is 0.02mg/m of formaldehyde30.2mg/m benzene3And ammonia 0.2mg/m3Common co-occurrences do not interfere.
Claims (2)
1. The low-temperature formaldehyde, benzene and ammonia catalyzing and luminous sensitive material is characterized in that gold atoms are doped with Dy2O3、In2O3And PbO, wherein the mass percentage ranges of the components are 0.5-2% of Au and 5-8% of Dy2O3、35-42.2％In2O3And 50-58.2% of PbO, and the preparation method comprises the following steps: dissolving dysprosium salt in a malic acid aqueous solution with the mass fraction of 10-15% to form a solution A, dissolving indium salt in a citric acid aqueous solution with the mass fraction of 15-20% to form a solution B, and dissolving lead salt in a tartaric acid aqueous solution with the mass fraction of 12-18% to form a solution C; dissolving chloroauric acid crystals in water, heating to 92 ℃, keeping the temperature under continuous stirring, slowly and dropwise adding the solution A, B and C into the solution in sequence, keeping the temperature under continuous stirring for 2 hours, adding agar powder, continuously stirring until the solution is clear, and cooling to room temperature to form gel; drying the gel, heating to 220-250 ℃ at a speed of not more than 2 ℃ per minute in a box-type resistance furnace, keeping the temperature for 3-4 hours, continuing heating to 400-450 ℃ 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 Au atom doped Dy with the Au atoms2O3、In2O3And PbO.
2. The low-temperature formaldehyde, benzene and ammonia catalytic luminescent sensing material as claimed in claim 1, wherein 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, the indium salt is one or a mixture of more of anhydride or hydrate of indium chloride, indium nitrate, indium sulfate, indium acetate and indium phosphate, and the lead salt is one or a mixture of anhydride or hydrate of lead nitrate, lead acetate and lead thiocyanate.
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