CN110376196B - Sensitive material capable of simultaneously responding to hydrogen sulfide and sulfur dioxide - Google Patents
Sensitive material capable of simultaneously responding to hydrogen sulfide and sulfur dioxide Download PDFInfo
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- CN110376196B CN110376196B CN201910638922.8A CN201910638922A CN110376196B CN 110376196 B CN110376196 B CN 110376196B CN 201910638922 A CN201910638922 A CN 201910638922A CN 110376196 B CN110376196 B CN 110376196B
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- neodymium
- dysprosium
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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
- G01N21/84—Systems specially adapted for particular applications
Abstract
The invention relates to a sensitive material simultaneously responding to hydrogen sulfide and sulfur dioxide, which is characterized in that Al is used2O3、Dy2O3And Nd2O3To form the nanometer powder material. The preparation method comprises the following steps: co-dissolving aluminum salt, dysprosium salt and neodymium salt in acetic acid aqueous solution, dripping citric acid aqueous solution and isopropanol aqueous solution, ultrasonically oscillating to clarify, heating and refluxing, volatilizing 1/4 moisture, cooling to obtain gel, infrared drying the gel, grinding, two-stage roasting, and naturally cooling to obtain the final product2O3、Dy2O3And Nd2O3To form the composite powder material. The gas sensor made of the sensitive material provided by the invention can simultaneously measure trace hydrogen sulfide and sulfur dioxide in the air on site without being interfered by other common coexisting molecules.
Description
Technical Field
The invention relates to a sensitive material simultaneously responding to hydrogen sulfide and sulfur dioxide, in particular to a sensitive material prepared from Al2O3、Dy2O3And Nd2O3A sensitive material composed of nano-powder belongs to the technical field of sensing.
Background
Hydrogen sulfide is a combustible colorless gas with a typical odor of eggs, generally a product of certain chemical reactions and natural protein decomposition processes. The industries with more hydrogen sulfide contact mainly comprise sewage treatment, paper making, petroleum processing, fertilizer manufacturing, chemical fiber manufacturing, certain chemical raw material manufacturing and the like. Inhalation of hydrogen sulfide by humans can cause acute poisoning and chronic damage. Acute hydrogen sulfide poisoning can be classified into three-level poisoning, mild poisoning, moderate poisoning and severe poisoning, and poisoning with different degrees has obvious difference in clinical manifestations. Mild poisoning manifested by photophobia, lacrimation, eye sting, foreign body sensation, nasal discharge, and burning sensation in nose and throat, and can be detected as conjunctival congestion, dry lung, and dim voice, and also has mild dizziness, headache, and asthenia symptoms; moderate poisoning is characterized by immediate occurrence of symptoms such as dizziness, headache, hypodynamia, nausea, vomiting, ataxia and the like, transient disturbance of consciousness, respiratory mucosa stimulation symptoms and eye stimulation symptoms can be caused, and dry or wet rales of lungs, conjunctival congestion, edema and the like can be detected; severe poisoning is manifested as symptoms of the central nervous system, including dizziness, palpitation, dyspnea, and bradykinesia, followed by dysphoria, confusion, vomiting, diarrhea, abdominal pain, and convulsion, which rapidly enter into coma and finally die due to respiratory paralysis. When exposed to very high concentrations of hydrogen sulfide, "shock-like" poisoning can occur, with the contacter falling down suddenly within seconds, stopping breathing. Repeated inhalation of low concentrations of hydrogen sulfide over a long period of time can cause hyposmia, as well as the appearance of neurasthenia and vegetative nerve dysfunction.
Sulfur dioxide is one of the main pollutants in the atmosphere and is an important indicator for determining whether the atmosphere is polluted or not. In many cities in the world, serious sulfur dioxide hazards occur, and many people are poisoned or die. Sulfur dioxide is acidic and can react with other substances in the air to form tiny sulfite and sulfate particles. When these particles are inhaled, they will accumulate in the lungs, which is one of the major causes of respiratory symptoms and disease. If mixed with water and then contacted with the skin, frostbite may occur. When in contact with the eye, redness and swelling and pain can result. After sulfur dioxide enters the respiratory tract, most of it is blocked in the upper respiratory tract because it is easily dissolved in water, and forms corrosive sulfurous acid, sulfuric acid and sulfate on the wet mucosa, thus enhancing the irritation. Smooth muscle of upper respiratory tract has peripheral nerve receptor, and when stimulated, it will produce constriction reaction to reduce the lumen of trachea and bronchus and increase the resistance of airway. The retention effect of the upper respiratory tract on sulfur dioxide can reduce the stimulation of sulfur dioxide to the lung to a certain extent. Sulfur dioxide can be absorbed into blood to produce toxic and side effects on the whole body, and the sulfur dioxide can destroy the activity of enzyme, thereby obviously influencing the metabolism of carbohydrate and protein and having certain damage to liver. Animal experiments prove that the immunity of the organism is obviously inhibited after sulfur dioxide chronic poisoning.
The accurate detection method of hydrogen sulfide and sulfur dioxide in the air mainly comprises the following steps: spectrophotometry, fluorescence photometry, flow injection chemiluminescence, gas chromatography, liquid chromatography, and other instrumental analysis methods. These methods are relatively sensitive, but the operation is complex, and the methods must be completed in a laboratory and cannot be realized on site.
Disclosure of Invention
The invention aims to provide a sensitive material simultaneously responding to hydrogen sulfide and sulfur dioxide and a preparation method thereof. The gas sensor made of the sensitive material can quickly and accurately measure trace hydrogen sulfide and sulfur dioxide on site without interference of other coexisting substances.
The sensitive material of the invention is made of Al2O3、Dy2O3And Nd2O3The preparation method of the nano-powder comprises the following steps:
dissolving aluminum salt, dysprosium salt and neodymium salt which are easy to dissolve in acidic aqueous solution into acetic acid aqueous solution with the mass fraction of 40-45%, respectively dropwise adding citric acid aqueous solution with the mass fraction of 70% and isopropanol aqueous solution with the mass fraction of 50%, ultrasonically oscillating to be clear, heating and refluxing for 2-4 hours in an oil bath with the temperature of 100-2O3、Dy2O3And Nd2O3The composite oxide powder material is formed.
Wherein, the aluminum salt is one or a mixture of more of anhydride or hydrate of aluminum nitrate, aluminum sulfate, aluminum perchlorate, aluminum chloride and aluminum acetate, 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, and the neodymium salt is one or a mixture of more of anhydride or hydrate of neodymium nitrate, neodymium oxalate, neodymium sulfate, neodymium chloride, neodymium acetate and neodymium perchlorate.
When the particle size of the prepared nano powder is in the range of 15-30nm, and all the components meet the requirement of Al2O3(40-49％)、Dy2O3(25-34%) and Nd2O3(24-30%) for detecting hydrogen sulfide and dioxideThe sulfur sensitive material has high sensitivity and selectivity.
Detailed Description
Example 1
Dissolving aluminum nitrate nonahydrate, dysprosium sulfate octahydrate, dysprosium chloride and neodymium nitrate hexahydrate in an acetic acid aqueous solution with the mass fraction of 40%, respectively dropwise adding a citric acid aqueous solution with the mass fraction of 70% and an isopropanol aqueous solution with the mass fraction of 50%, ultrasonically oscillating until the mixture is clear, heating and refluxing for 4 hours in a 100 ℃ oil bath, removing a reflux pipe, heating to volatilize 1/4 moisture, cooling to obtain gel, drying the gel for 2 hours in infrared mode, fully grinding, heating to 250 ℃ in a box-type resistance furnace at the speed of not more than 3 ℃ per minute, keeping the temperature for 5 hours, heating to 350 ℃ at the speed of not more than 4 ℃ per minute, keeping the temperature for 5 hours, and naturally cooling to obtain the aluminum nitrate hexahydrate2O3、Dy2O3And Nd2O3The composite oxide powder material is formed.
And (3) analysis: testing the powder material by a transmission electron microscope, wherein the particle size range of the powder material is 15-25 nm; the composition of the product is Al by energy spectrum analysis2O3(42.8％)、Dy2O3(33.1%) and Nd2O3(24.1％)。
The application comprises the following steps: the powder is used as a catalytic luminescent sensitive material for measuring hydrogen sulfide and sulfur dioxide, and the linear range is 0.4-23mg/m of hydrogen sulfide3And 0.2-44mg/m of sulfur dioxide3The detection limit is 0.2mg/m of hydrogen sulfide3And sulfur dioxide 0.1mg/m3Common co-occurrences do not interfere.
Example 2
Dissolving aluminum sulfate octadecahydrate, aluminum perchlorate, dysprosium nitrate hexahydrate and neodymium oxalate decahydrate in 41% acetic acid aqueous solution by mass fraction, respectively dropwise adding 70% citric acid aqueous solution and 50% isopropanol aqueous solution, ultrasonically oscillating to clarify, heating and refluxing for 4 hours in 101 ℃ oil bath, removing reflux pipe, heating to volatilize 1/4 moisture, cooling to obtain gel, infrared drying for 3 hours, fully grinding, and heating at a speed of not more than 3 ℃ per minute in a box-type resistance furnaceHeating to 253 deg.C, maintaining the temperature for 5 hr, heating to 348 deg.C at a rate of 4 deg.C/min, maintaining the temperature for 5 hr, and naturally cooling to obtain Al2O3、Dy2O3And Nd2O3The composite oxide powder material is formed.
And (3) analysis: the powder material is tested by a transmission electron microscope, and the particle size range of the powder material is 20-30 nm; the composition of the product is Al by energy spectrum analysis2O3(46.5％)、Dy2O3(25.3%) and Nd2O3(28.2％)。
The application comprises the following steps: the powder is used as a catalytic luminescent sensitive material for measuring hydrogen sulfide and sulfur dioxide, and the linear range is 0.6-25mg/m of hydrogen sulfide3And 0.2-45mg/m of sulfur dioxide3The detection limit is 0.2mg/m of hydrogen sulfide3And sulfur dioxide 0.1mg/m3Common co-occurrences do not interfere.
Example 3
Dissolving aluminum perchlorate nonahydrate, aluminum chloride, dysprosium chloride hexahydrate and neodymium sulfate octahydrate in an acetic acid aqueous solution with the mass fraction of 42%, respectively dropwise adding a citric acid aqueous solution with the mass fraction of 70% and an isopropanol aqueous solution with the mass fraction of 50%, ultrasonically oscillating to be clear, heating and refluxing for 3 hours in an oil bath at 102 ℃, removing a reflux pipe, heating to volatilize 1/4 moisture, cooling to obtain gel, drying the gel for 2 hours in infrared mode, fully grinding, heating to 256 ℃ at the speed of not more than 3 ℃ per minute in a box-type resistance furnace, keeping the temperature for 4 hours, heating to 346 ℃ at the speed of not more than 4 ℃ per minute, keeping the temperature for 5.5 hours, and naturally cooling to obtain the aluminum perchlorate-aluminum alloy2O3、Dy2O3And Nd2O3The composite oxide powder material is formed.
And (3) analysis: testing the powder material by a transmission electron microscope, wherein the particle size range of the powder material is 15-25 nm; the composition of the product is Al by energy spectrum analysis2O3(48.2％)、Dy2O3(26.3%) and Nd2O3(25.5％)。
The application comprises the following steps: the powder is used as the catalyst for measuring hydrogen sulfide and sulfur dioxideThe linear range of the luminescent sensitive material is 0.5-25mg/m of hydrogen sulfide3And 0.3-54mg/m of sulfur dioxide3The detection limit is 0.2mg/m of hydrogen sulfide3And sulfur dioxide 0.1mg/m3Common co-occurrences do not interfere.
Example 4
Dissolving aluminum chloride hexahydrate, dysprosium acetate pentahydrate, neodymium chloride hexahydrate and neodymium perchlorate in 43% aqueous solution of acetic acid by mass fraction, respectively dropwise adding 70% aqueous solution of citric acid and 50% aqueous solution of isopropanol, ultrasonically oscillating until the mixture is clear, heating and refluxing for 3 hours in a 103 ℃ oil bath, removing a reflux pipe, heating to volatilize 1/4 moisture, cooling to obtain gel, infrared drying for 3 hours, fully grinding, heating to 259 ℃ at a speed of no more than 3 ℃ per minute in a box-type resistance furnace, keeping the temperature for 4 hours, heating to 344 ℃ at a speed of no more than 4 ℃ per minute, keeping the temperature for 5.5 hours, and naturally cooling to obtain the Al-doped aluminum oxide2O3、Dy2O3And Nd2O3The composite oxide powder material is formed.
And (3) analysis: testing the powder material by a transmission electron microscope, wherein the particle size range of the powder material is 15-25 nm; the composition of the product is Al by energy spectrum analysis2O3(41.7％)、Dy2O3(32.0%) and Nd2O3(26.3％)。
The application comprises the following steps: the powder is used as a catalytic luminescent sensitive material for measuring hydrogen sulfide and sulfur dioxide, and the linear range is 0.6-28mg/m of hydrogen sulfide3And 0.2-45mg/m of sulfur dioxide3The detection limit is 0.2mg/m of hydrogen sulfide3And sulfur dioxide 0.1mg/m3Common co-occurrences do not interfere.
Example 5
Dissolving aluminum acetate dihydrate, dysprosium chloride hexahydrate, dysprosium oxalate decahydrate and neodymium acetate tetrahydrate in 44% acetic acid aqueous solution by mass fraction, respectively dropwise adding 70% citric acid aqueous solution and 50% isopropanol aqueous solution by mass fraction, ultrasonically oscillating to clarify, heating and refluxing for 2 hours in 104 ℃ oil bath, removing reflux pipe, heating to volatilize 1/4 water, cooling to obtain condensateDrying the gel with infrared for 2 hr, grinding, heating to 262 deg.C in a box-type resistance furnace at a speed of 3 deg.C/min, maintaining the temperature for 3 hr, heating to 342 deg.C at a speed of 4 deg.C/min, maintaining the temperature for 6 hr, and naturally cooling to obtain the final product2O3、Dy2O3And Nd2O3The composite oxide powder material is formed.
And (3) analysis: the powder material is tested by a transmission electron microscope, and the particle size range of the powder material is 20-30 nm; the composition of the product is Al by energy spectrum analysis2O3(44.0％)、Dy2O3(31.2%) and Nd2O3(24.8％)。
The application comprises the following steps: the powder is used as a catalytic luminescent sensitive material for measuring hydrogen sulfide and sulfur dioxide, and the linear range is 0.4-25mg/m of hydrogen sulfide3And 0.2-47mg/m of sulfur dioxide3The detection limit is 0.2mg/m of hydrogen sulfide3And sulfur dioxide 0.1mg/m3Common co-occurrences do not interfere.
Example 6
Co-dissolving aluminum perchlorate nonahydrate, aluminum acetate dihydrate, dysprosium oxalate decahydrate and neodymium perchlorate into an acetic acid aqueous solution with the mass fraction of 45%, respectively dropwise adding a citric acid aqueous solution with the mass fraction of 70% and an isopropanol aqueous solution with the mass fraction of 50%, ultrasonically oscillating until the mixture is clear, heating and refluxing for 2 hours in an oil bath at 105 ℃, removing a reflux pipe, heating and volatilizing 1/4 moisture, cooling to obtain gel, carrying out infrared drying for 3 hours, fully grinding, heating to 265 ℃ at the speed of not more than 3 ℃ per minute in a box-type resistance furnace, keeping the temperature for 3 hours, heating to 340 ℃ at the speed of not more than 4 ℃ per minute, keeping the temperature for 6 hours, and naturally cooling to obtain the Al-doped aluminum perchlorate2O3、Dy2O3And Nd2O3The composite oxide powder material is formed.
And (3) analysis: testing the powder material by a transmission electron microscope, wherein the particle size range of the powder material is 15-25 nm; the composition of the product is Al by energy spectrum analysis2O3(47.4％)、Dy2O3(25.0%) and Nd2O3(27.6％)。
The application comprises the following steps: the powder is used as a catalytic luminescent sensitive material for measuring hydrogen sulfide and sulfur dioxide, and the linear range is 0.5-24mg/m of hydrogen sulfide3And 0.2-42mg/m of sulfur dioxide3The detection limit is 0.2mg/m of hydrogen sulfide3And sulfur dioxide 0.1mg/m3Common co-occurrences do not interfere.
Claims (2)
1. A sensitive material for simultaneously responding to hydrogen sulfide and sulfur dioxide is prepared from Al2O3、Dy2O3And Nd2O3The composite powder material with the grain diameter range of 15-30nm comprises 40-49 mass percent of Al2O3、25-34％Dy2O3And 24-30% Nd2O3The preparation method comprises the following steps: dissolving aluminum salt, dysprosium salt and neodymium salt which are easy to dissolve in acidic aqueous solution into acetic acid aqueous solution with the mass fraction of 40-45%, respectively dropwise adding citric acid aqueous solution with the mass fraction of 70% and isopropanol aqueous solution with the mass fraction of 50%, ultrasonically oscillating to be clear, heating and refluxing for 2-4 hours in an oil bath with the temperature of 100-2O3、Dy2O3And Nd2O3The composite oxide powder material is formed.
2. A sensing material responsive to both hydrogen sulfide and sulfur dioxide as claimed in claim 1 wherein said aluminum salt is one or a mixture of one or more of the anhydrates or hydrates of aluminum nitrate, aluminum sulfate, aluminum perchlorate, aluminum chloride and aluminum acetate, dysprosium salt is one or a mixture of one or more of the anhydrates or hydrates of dysprosium nitrate, dysprosium sulfate, dysprosium chloride, dysprosium acetate and dysprosium oxalate, and neodymium salt is one or a mixture of one or more of the anhydrates or hydrates of neodymium nitrate, neodymium oxalate, neodymium sulfate, neodymium chloride, neodymium acetate and neodymium perchlorate.
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