CN110455978B - Benzene and ammonia low-temperature catalytic luminescence cross-sensitive material - Google Patents
Benzene and ammonia low-temperature catalytic luminescence cross-sensitive material Download PDFInfo
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Abstract
The invention relates to a low-temperature catalytic luminous cross-sensitive material of benzene and ammonia, which is characterized in that Pt atoms are doped with Cr2O3、In2O3And MnO2To form the composite powder material. The preparation method comprises the following steps: dissolving chromium salt, indium salt and manganese salt in acetic acid water solution, adding glucose and citric acid, stirring until the solution is clear, adding chloroplatinic acid, heating and refluxing, rotationally evaporating to remove one fourth of water, keeping a certain temperature, adding agar powder, continuously stirring until the solution is clear, and naturally cooling to room temperature to form gel. Drying the gel, two-stage roasting and natural cooling to obtain Pt atom doped Cr2O3、In2O3And MnO2To form the composite powder material. The gas sensor made of the sensitive material provided by the invention can work at a lower temperature and can detect trace benzene and ammonia in the air at high sensitivity without being interfered by other common coexisting molecules.
Description
Technical Field
The invention relates to a low-temperature catalytic luminescence cross-sensitive material of benzene and ammonia, in particular to a Pt atom doped Cr2O3、In2O3And MnO2The composite powder material belongs to the field of sensing technology.
Background
Benzene (C)6H6) Is a chemical raw material with aromatic odor, and is determined as a carcinogen by the world health organization. Benzene in the air is mainly derived from building coatings, decorative paints, adhesive solutions, automobile exhaust and the like. Benzene is one of the main pollutants in indoor air and has great threat to human health. Chronic benzene poisoning is mainly a stimulus to the skin, eyes and upper respiratory tract; the skin can be dried and desquamated due to degreasing when being frequently contacted with benzene, and allergic eczema is generated in some cases; long-term benzene inhalation can lead to aplastic anemia.
Ammonia gas (NH)3) Is an alkaline, colorless and strongly pungent gas, and is easily dissolved in water and often adsorbed on human skin mucosa, eye conjunctiva and respiratory tract and throat mucosa. The ammonia gas in the indoor air can be slowly released from the wall using the construction antifreeze, and when the concentration of the ammonia gas in the air is 0.5mg/m3Can make people feel pungent smell when the ammonia concentration in air exceeds 80mg/m3In short time, people can have lacrimation, pharyngalgia, cough, chest distress, dyspnea, dizziness, headache, nausea, emesis, debilitation and other symptoms, and can also have pulmonary edema and respiratory tract pathological changes. People living in low-concentration ammonia environment for a long time can gradually paralyze respiratory tract cilia and damage mucosal epithelial tissues, so that pathogenic microorganisms are easy to invade, and the resistance of the body to diseases is weakened.
The method for measuring benzene mainly comprises a photometric method, an electrochemical method, a chromatographic method, a chemiluminescence method, a chromatography-mass spectrometry method, an ion chromatography method and the like. The conventional detection means of ammonia gas mainly comprises spectrophotometry, gas chromatography, liquid chromatography, electrochemical method and the like. These methods are relatively sensitive and must be carried out in a laboratory, but are complex in operation, require prior enrichment and appropriate treatment to complete the measurement by an analytical instrument, and cannot be carried out on site. The on-site determination method of benzene and ammonia gas mainly comprises a detection tube colorimetric method, and the method has insufficient stability and sensitivity and cannot complete accurate determination of trace components.
The invention patent ZL200910223546.2 discloses a doped nano sensitive material for monitoring benzene series, the invention patent ZL200710306935.2 discloses a nano composite oxide sensitive material of ammonia, the invention patent ZL201410460628.X discloses a cross sensitive material of ammonia and benzene in air and a preparation method thereof, and the invention patent ZL201410605596.8 discloses a catalytic luminescence sensitive material of formaldehyde, benzene and ammonia in air, but the use temperature of the sensitive materials exceeds 350 ℃, the thermal radiation background generated by the use temperature can form a strong base line signal, and the base line signal can seriously influence the sensitivity of the sensor.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a cross-sensitive material which has higher selectivity and catalytic luminescence activity to benzene and ammonia at lower temperature. The gas sensor made of the sensitive material has small background signal, greatly improves the sensitivity of benzene and ammonia measurement, and can simultaneously measure trace benzene and ammonia in the air without being interfered by common coexisting molecules.
The sensitive material is Pt atom doped Cr2O3、In2O3And MnO2The preparation method of the composite powder material comprises the following steps:
dissolving chromium salt, indium salt and manganese salt which are easily dissolved in an acidic aqueous solution into an acetic acid aqueous solution with the mass fraction of 10-15%, adding glucose and citric acid with the mass ratio of 1: 1, stirring at the constant temperature of 30-40 ℃ for 2-3 hours until the solution is clear, then adding chloroplatinic acid, heating and refluxing for 3-4 hours, rotationally evaporating to remove one fourth of moisture, cooling to room temperature, transferring to a beaker, heating in a water bath to 90-95 ℃, keeping the temperature for continuous stirring, adding agar powder, continuously stirring until the solution is clear, and naturally cooling to room temperature to form gel; drying the gel, heating to 200-220 deg.C in a box-type resistance furnace at a speed of not more than 2 deg.C per minute, maintaining the temperature for 3-4 hr, heating to 350-380 deg.C at a speed of not more than 2 deg.C per minute, maintaining the temperature for 2-3 hr, and naturally cooling to room temperature to obtain Pt-doped Cr2O3、In2O3And MnO2To form the composite powder material.
Wherein, the chromium salt is one or a mixture of more of anhydrous substances or hydrates of chromium chloride, chromium perchlorate, chromium acetate, chromium oxalate, chromium nitrate and chromium sulfate, the indium salt is one or a mixture of more of anhydrous substances or hydrates of indium chloride, indium nitrate, indium sulfate, indium acetate and indium phosphate, and the manganese salt is one or a mixture of more of anhydrous substances or hydrates of manganese acetate, manganese sulfate, manganese chloride, manganese nitrate and manganese perchlorate.
When the mass fraction of each component of the prepared composite sensitive material meets 0.6-1.3 percent of Pt,Cr2O3(25-35％)、In2O3(35-40%) and MnO2(30-35%) and has high sensitivity and selectivity when used as a low-temperature catalytic luminescent cross-sensitive material for trace benzene and ammonia in air.
Detailed Description
Example 1
Dissolving chromium chloride hexahydrate, indium nitrate trihydrate and manganese acetate dihydrate into an acetic acid aqueous solution with the mass fraction of 10%, adding glucose and citric acid with the mass ratio of 1: 1, stirring at the constant temperature of 30 ℃ for 3 hours until the solution is clear, then adding chloroplatinic acid, heating and refluxing for 3 hours, rotationally evaporating to remove one fourth of water, cooling to room temperature, transferring to a beaker, heating in a water bath to 90 ℃, keeping the temperature for continuous stirring, adding agar powder, continuously stirring until the solution is clear, and naturally cooling to the room temperature to form gel; drying the gel, heating to 200 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 355 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 Pt-doped Cr2O3、In2O3And MnO2To form the composite powder material.
And (3) analysis: the composite powder material is subjected to component analysis, and the mass percent of the components is 0.7 percent of Pt and 29.5 percent of Cr2O3、37.6％In2O3And 32.2% MnO2。
The application comprises the following steps: the powder material is used as a sensitive material for detecting benzene and ammonia, and the linear range of the powder material is 0.4-58mg/m of benzene3And ammonia 0.5-49mg/m3The detection limit is 0.2mg/m of benzene3And ammonia 0.2mg/m3And the working temperature is 195 ℃.
Example 2
Dissolving chromium perchlorate hexahydrate, indium chloride, indium phosphate and manganese sulfate into 11% acetic acid aqueous solution, adding glucose and citric acid in a mass ratio of 1: 1, stirring at a constant temperature of 32 ℃ for 2 hours until the mixture is clear, adding chloroplatinic acid, heating and refluxing for 4 hours, rotationally evaporating to remove one fourth of moisture, cooling to room temperature, transferring to a burning furnaceHeating in a cup in water bath to 91 ℃, keeping the temperature and continuously stirring, adding agar powder and continuously stirring until the solution is clear, and naturally cooling to room temperature to form gel; drying the gel, heating to 202 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 360 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 Pt-doped Cr2O3、In2O3And MnO2To form the composite powder material.
And (3) analysis: the composite powder material is subjected to component analysis, and the mass percent of the components is 0.9 percent of Pt and 33.3 percent of Cr2O3、35.4％In2O3And 30.4% MnO2。
The application comprises the following steps: the powder material is used as a sensitive material for detecting benzene and ammonia, and the linear range of the powder material is 0.5-61mg/m of benzene3And ammonia 0.5-55mg/m3The detection limit is 0.2mg/m of benzene3And ammonia 0.2mg/m3And the working temperature is 185 ℃.
Example 3
Dissolving chromium acetate hexahydrate, indium sulfate pentahydrate and manganese chloride tetrahydrate in an acetic acid aqueous solution with the mass fraction of 12%, adding glucose and citric acid with the mass ratio of 1: 1, stirring at the constant temperature of 34 ℃ for 3 hours until the solution is clear, then adding chloroplatinic acid, heating and refluxing for 3 hours, rotationally evaporating to remove one fourth of water, cooling to room temperature, transferring to a beaker, heating in a water bath to 93 ℃, keeping the temperature for continuous stirring, adding agar powder, continuously stirring until the solution is clear, and naturally cooling to the room temperature to form gel; drying the gel, heating to 208 deg.C in a box-type resistance furnace at a speed of 2 deg.C/min, maintaining the temperature for 3 hr, heating to 365 deg.C at a speed of 2 deg.C/min, maintaining the temperature for 2 hr, and naturally cooling to room temperature to obtain Pt-doped Cr2O3、In2O3And MnO2To form the composite powder material.
And (3) analysis: the composite powder material is subjected to component analysis, and the mass percent of the components is 1.3 percent of Pt and 26.7 percent of Cr2O3、38.5％In2O3And 33.5% MnO2。
The application comprises the following steps: the powder material is used as a sensitive material for detecting benzene and ammonia, and the linear range of the powder material is 0.5-58mg/m of benzene3And ammonia 0.6-78mg/m3The detection limit is 0.2mg/m of benzene3And ammonia 0.3mg/m3And the working temperature is 215 ℃.
Example 4
Dissolving chromium oxalate, indium acetate hexahydrate and manganese nitrate hexahydrate in 13% acetic acid aqueous solution, adding glucose and citric acid in a mass ratio of 1: 1, stirring at a constant temperature of 36 ℃ for 2 hours until the solution is clear, then adding chloroplatinic acid, heating and refluxing for 4 hours, rotationally evaporating to remove one fourth of water, cooling to room temperature, transferring to a beaker, heating in a water bath to 92 ℃, keeping the temperature for continuous stirring, adding agar powder, continuously stirring until the solution is clear, and naturally cooling to room temperature to form gel; drying the gel, heating to 210 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 370 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 Pt-doped Cr2O3、In2O3And MnO2To form the composite powder material.
And (3) analysis: the composite powder material is subjected to component analysis, and the mass percent of the components is 1.0 percent of Pt and 31.1 percent of Cr2O3、36.2％In2O3And 31.7% MnO2。
The application comprises the following steps: the powder material is used as a sensitive material for detecting benzene and ammonia, and the linear range of the powder material is 0.5-55mg/m of benzene3And ammonia 0.5-45mg/m3The detection limit is 0.2mg/m of benzene3And ammonia 0.2mg/m3And the working temperature is 200 ℃.
Example 5
Dissolving chromium nitrate nonahydrate, indium sulfate pentahydrate, indium phosphate and manganese perchlorate hexahydrate in an acetic acid aqueous solution with the mass fraction of 14%, adding glucose and citric acid in the mass ratio of 1: 1, stirring at the constant temperature of 38 ℃ for 3 hours until the mixture is clear, then adding chloroplatinic acid, heating and refluxing for 3 hours, and rotationally evaporating quarter of the chloroplatinic acidCooling to room temperature, transferring to a beaker, heating to 94 ℃ in a water bath, continuously stirring while keeping the temperature, adding agar powder, continuously stirring until the solution is clear, and naturally cooling to room temperature to form gel; drying the gel, heating to 215 deg.C at a speed of 2 deg.C/min in a box-type resistance furnace, maintaining the temperature for 3 hr, heating to 375 deg.C at a speed of 2 deg.C/min, maintaining the temperature for 2 hr, and naturally cooling to room temperature to obtain Pt-doped Cr2O3、In2O3And MnO2To form the composite powder material.
And (3) analysis: the composite powder material is subjected to component analysis, and the mass percent of the components is 0.6 percent of Pt and 26.3 percent of Cr2O3、39.0％In2O3And 34.1% MnO2。
The application comprises the following steps: the powder material is used as a sensitive material for detecting benzene and ammonia, and the linear range of the powder material is 0.5-59mg/m of benzene3And ammonia 0.5-64mg/m3The detection limit is 0.2mg/m of benzene3And ammonia 0.2mg/m3The working temperature was 205 ℃.
Example 6
Dissolving chromium sulfate, indium nitrate trihydrate, manganese chloride tetrahydrate and manganese perchlorate into an acetic acid aqueous solution with the mass fraction of 15%, adding glucose and citric acid with the mass ratio of 1: 1, stirring at the constant temperature of 40 ℃ for 2 hours until the solution is clear, then adding chloroplatinic acid, heating and refluxing for 4 hours, rotationally evaporating to remove one fourth of moisture, cooling to room temperature, transferring to a beaker, heating in a water bath to 95 ℃, keeping the temperature for continuous stirring, adding agar powder, continuously stirring until the solution is clear, and naturally cooling to the room temperature to form gel; drying the gel, heating to 220 deg.C in a box-type resistance furnace at a speed of 2 deg.C/min, maintaining the temperature for 4 hr, heating to 380 deg.C at a speed of 2 deg.C/min, maintaining the temperature for 3 hr, and naturally cooling to room temperature to obtain Pt-doped Cr2O3、In2O3And MnO2To form the composite powder material.
And (3) analysis: the composite powder material is subjected to component analysis, and the measured mass percentage is 0.8 percent of Pt,27.5％Cr2O3、39.7％In2O3And 32.0% MnO2。
The application comprises the following steps: the powder material is used as a sensitive material for detecting benzene and ammonia, and the linear range of the powder material is 0.4-52mg/m of benzene3And ammonia 0.5-58mg/m3The detection limit is 0.2mg/m of benzene3And ammonia 0.2mg/m3And the working temperature is 210 ℃.
Claims (2)
1. A low-temp catalytic luminous cross-sensitive material of benzene and ammonia is prepared from Pt atom doped with Cr2O3、In2O3And MnO2The composite powder material comprises 0.6-1.3% of Pt and 25-33.3% of Cr in percentage by mass2O3、35-40％In2O3And 30-35% MnO2The preparation method comprises the following steps: dissolving chromium salt, indium salt and manganese salt which are easily dissolved in acidic aqueous solution into acetic acid aqueous solution with the mass fraction of 10-15%, and adding into the acetic acid aqueous solution with the mass ratio of 1∶1, stirring glucose and citric acid at a constant temperature of 30-40 ℃ for 2-3 hours until the glucose and the citric acid are clear, then adding chloroplatinic acid, heating and refluxing for 3-4 hours, rotationally evaporating one fourth of water, cooling to room temperature, transferring to a beaker, heating in a water bath to 90-95 ℃, keeping the temperature under continuous stirring, adding agar powder, continuously stirring until the solution is clear, and naturally cooling to room temperature to form gel; drying the gel, heating to 200-220 deg.C in a box-type resistance furnace at a speed of not more than 2 deg.C per minute, maintaining the temperature for 3-4 hr, heating to 350-380 deg.C at a speed of not more than 2 deg.C per minute, maintaining the temperature for 2-3 hr, and naturally cooling to room temperature to obtain Pt-doped Cr2O3、In2O3And MnO2To form the composite powder material.
2. The low-temperature catalytic luminescent cross-sensitive material of benzene and ammonia as claimed in claim 1, wherein the chromium salt is one or more of chromium chloride, chromium perchlorate, chromium acetate, chromium oxalate, chromium nitrate and chromium sulfate anhydride or hydrate, the indium salt is one or more of indium chloride, indium nitrate, indium sulfate, indium acetate and indium phosphate anhydride or hydrate, and the manganese salt is one or more of manganese acetate, manganese sulfate, manganese chloride, manganese nitrate and manganese perchlorate anhydride or hydrate.
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