CN109490374B - Cross sensitive material for formaldehyde, benzene, ammonia and carbon monoxide in air - Google Patents
Cross sensitive material for formaldehyde, benzene, ammonia and carbon monoxide in air Download PDFInfo
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
- G01N27/125—Composition of the body, e.g. the composition of its sensitive layer
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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
Abstract
The invention relates to a cross-sensitive material of formaldehyde, benzene, ammonia and carbon monoxide in air, which is characterized in that Cr loaded by graphene2O3CuO and Nd2O3The preparation method of the catalytic luminescent sensitive material comprises the following steps: converting natural graphite into graphene oxide; dissolving chromium salt in citric acid aqueous solution, dissolving copper salt and neodymium salt in hydrochloric acid aqueous solution, mixing the two solutions under continuous stirring, heating, adding agar powder, cooling to room temperature to form gel, drying the gel, grinding and firing to obtain a powder material; under the condition of continuous stirring, adding graphene oxide and powder materials into a hydrazine hydrate aqueous solution, heating, stirring, naturally cooling, filtering, washing and drying to obtain the graphene-loaded Cr2O3CuO and Nd2O3To form the composite powder material. The gas sensor made of the sensitive material provided by the invention can rapidly measure the trace formaldehyde, benzene, ammonia and carbon monoxide in the air on site.
Description
Technical Field
The invention relates to a cross-sensitive material of formaldehyde, benzene, ammonia and carbon monoxide in air, in particular to a graphene-loaded Cr2O3CuO and Nd2O3The formed catalytic luminescence sensitive material belongs to the technical field of sensing.
Background
Formaldehyde is a colorless and volatile chemical raw material, 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. People have different responses to various concentrations of formaldehyde in air: when the concentration of formaldehyde in the air reaches 0.08mg/m3When children suffer slight asthma, it reaches 0.1mg/m3The taste is abnormal and reaches 0.6mg/m3It can cause discomfort or pain in throat, up to 1mg/m3It can cause a large amount of lacrimation to reach 10mg/m3The patients can feel dyspnea when the pressure reaches 30mg/m3Can suffocate people. Long-term exposure to low formaldehyde doses (0.1 mg/m)3The following) can cause chronic respiratory disease, female pregnancy syndrome, newborn physique reduction and chromosome abnormalityAnd (6) pathological changes. Formaldehyde has been identified as a carcinogen by the international research center for cancer (IARC). Benzene is a chemical raw material with aromatic odor, and chronic benzene poisoning mainly has stimulation effect on 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 is an alkaline, colorless gas with strong pungent odor, and ammonia gas in air is easily dissolved in water and is often adsorbed on human skin mucosa, conjunctiva of eyes and respiratory tract and throat mucosa. When the concentration of ammonia in the air is 0.5mg/m3Can make people feel pungent smell; when the concentration of ammonia in the 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 carbon monoxide is colorless, odorless and nonirritating gas, and the explosion limit of the carbon monoxide mixed with air is 12.5-74%. Carbon monoxide is the most widespread and abundant pollutant in the atmosphere and is also one of the important pollutants generated in the combustion process. When the combustion of the carbonaceous material is incomplete, CO gas can be generated. There are many operations for contacting CO in industrial processes, such as coking, ironmaking, forging, casting and heat treatment in the metallurgical industry; the production of synthetic ammonia, acetone, phosgene and methanol in chemical industry; blasting in a mine and gas explosion accidents in a coal mine; manufacturing a carbon graphite electrode; testing the internal combustion engine; and the production of metal carbonyls such as nickel carbonyl, iron carbonyl and the like, or the production and use of combustible gas containing CO (such as water gas containing 40% of CO, 30% of blast furnace and producer gas and 5% -15% of coal gas) can contact CO. The gas after the explosive or gunpowder explosion contains about 30 to 60 percent of CO. The exhaust gas of internal combustion engines using diesel oil and gasoline also contains about 1% to 8% of CO. After entering human body, CO will combine with hemoglobin in blood, and the combination of CO and hemoglobin is much stronger than that of oxygen and oxygenThe binding capacity of hemoglobin, and thus the amount of hemoglobin capable of binding oxygen, is drastically reduced, thereby causing hypoxia to the tissues of the body, resulting in asphyxia death of the body.
In recent years, indoor air pollution is becoming more serious due to the use of indoor decoration and various modern living goods. Formaldehyde, benzene, ammonia and carbon monoxide are the main pollutants of indoor air. In recent years, relevant departments of the country randomly inspect a newly-built high-grade office building and a family residential district in Beijing, detect the indoor air quality of the residential district, and find that the formaldehyde, benzene, ammonia and carbon monoxide in the indoor air exceed the standard by more than 50 percent, and the air quality seriously threatens the human health.
The methods for respectively measuring formaldehyde, benzene, ammonia and carbon monoxide mainly comprise spectrophotometry, electrochemistry, chromatography, chemiluminescence, gas-liquid-mass-chromatography, ion chromatography and the like. These methods all require prior enrichment and appropriate processing to complete the assay separately by the analytical instrument, and are therefore time consuming and not easily implemented on site. The method for simultaneously measuring the four molecules is not reported.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a catalytic luminescent sensitive material with high selectivity on formaldehyde, benzene, ammonia and carbon monoxide. The gas sensor made of the sensitive material can simultaneously measure the trace formaldehyde, benzene, ammonia and carbon monoxide in the air without being interfered by common coexisting substances.
The sensitive material is loaded by graphene and made of Cr2O3CuO and Nd2O3The preparation method of the composite sensitive material comprises the following steps: slowly adding natural graphite into concentrated sulfuric acid under continuous stirring, slowly adding potassium permanganate with the weight 1.5 times that of the natural graphite after stirring for 3-4 hours, heating to 40-45 ℃, continuously stirring for 3-5 hours, naturally cooling to room temperature, performing suction filtration, and washing a filtrate to be neutral to obtain A; dissolving chromium salt in 20-30 wt% citric acid aqueous solution, dissolving copper salt and neodymium salt in 15-20 wt% hydrochloric acid aqueous solution, mixing the two solutions under continuous stirring for 2 hr, heating to room temperatureAdding agar powder after 90-95 ℃, stirring until the agar powder is completely dissolved, cooling to room temperature to form gel, drying the gel, heating to 250 ℃ at a speed of not more than 3 ℃ per minute in a box-type resistance furnace, keeping the temperature for 4 hours, continuously heating to 450 ℃ at a speed of not more than 3 ℃ per minute, keeping the temperature for 3 hours, and naturally cooling to room temperature to obtain B; under the condition of continuous stirring, adding the A into a hydrazine hydrate aqueous solution with the mass fraction of 15-20%, heating to 45 ℃, stirring at constant temperature for 4-5 hours, adding the B into the hydrazine hydrate aqueous solution, continuously stirring at constant temperature for 2-3 hours, naturally cooling, filtering, washing with deionized water for 3 times, and drying in a vacuum oven at 65 ℃ to obtain the graphene-loaded Cr2O3CuO and Nd2O3To 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 copper salt is one or a mixture of more of anhydrous substances or hydrates of copper chloride, copper sulfate, copper phosphate and copper nitrate, and the neodymium salt is one or a mixture of more of anhydrous substances or hydrates of neodymium nitrate, neodymium oxalate, neodymium sulfate, neodymium chloride, neodymium acetate and neodymium perchlorate.
When the mass fractions of all the components of the prepared composite sensitive material meet the requirement of Cr2O3(15-20％)、CuO(10-16％)、Nd2O3(12-20%) and C (50-60%), and has high sensitivity and selectivity when used as the catalytic luminescent sensitive material for formaldehyde, benzene, ammonia and carbon monoxide in the air.
Detailed Description
Example 1
Slowly adding natural graphite into concentrated sulfuric acid under continuous stirring, slowly adding potassium permanganate with the weight 1.5 times that of the natural graphite after stirring for 3 hours, heating to 42 ℃, continuously stirring for 5 hours, naturally cooling to room temperature, performing suction filtration, and washing a filtrate to be neutral to obtain A; dissolving chromium chloride 6 hydrate in 30% citric acid aqueous solution, dissolving copper chloride 2 hydrate, neodymium nitrate 6 hydrate and neodymium perchlorate in 15% hydrochloric acid aqueous solution, and continuously stirringMixing the two solutions, stirring for 2 hours, heating to 95 ℃, adding agar powder, stirring until the agar powder is completely dissolved, cooling to room temperature to form gel, drying the gel, heating to 205 ℃ in a box-type resistance furnace at a speed of not more than 3 ℃ per minute, keeping the temperature for 4 hours, continuing heating to 450 ℃ at a speed of not more than 3 ℃ per minute, keeping the temperature for 3 hours, and naturally cooling to room temperature to obtain B; under the condition of continuous stirring, adding the A into a hydrazine hydrate aqueous solution with the mass fraction of 15%, heating to 45 ℃, stirring at constant temperature for 4.5 hours, adding the B into the hydrazine hydrate aqueous solution, continuously stirring at constant temperature for 2.3 hours, naturally cooling, filtering, washing with deionized water for 3 times, and drying in a vacuum oven at 65 ℃ to obtain the graphene-loaded Cr2O3CuO and Nd2O3To form the composite powder material.
And (3) analysis: the composite sensitive material is subjected to component analysis, and the measured mass percentage is 16.2% of Cr2O3、12.5％CuO、17.8％Nd2O3And 53.5% C.
The application comprises the following steps: the sensitive material is used for detecting formaldehyde, benzene, ammonia and carbon monoxide, and the linear range of the sensitive material is 0.1-66mg/m of formaldehyde30.6-68mg/m of benzene30.7-80mg/m of ammonia3And carbon monoxide 1-100mg/m3The detection limit is 0.05mg/m of formaldehyde30.2mg/m benzene30.3mg/m of ammonia3And carbon monoxide 0.8mg/m3Common co-occurrences do not interfere.
Example 2
Slowly adding natural graphite into concentrated sulfuric acid under continuous stirring, slowly adding potassium permanganate with the weight 1.5 times that of the natural graphite after stirring for 4 hours, heating to 45 ℃, continuously stirring for 3 hours, naturally cooling to room temperature, performing suction filtration, and washing a filtrate to be neutral to obtain A; dissolving 6 parts of chromium perchlorate in 20% of citric acid aqueous solution, dissolving 5 parts of copper sulfate hydrate and 6 parts of neodymium chloride hydrate in 18% of hydrochloric acid aqueous solution, mixing and stirring the two solutions for 2 hours under continuous stirring, heating to 94 ℃, adding agar powder, stirring until the agar powder is completely dissolved, cooling to room temperature to form gel, drying the gel, and placing the gel in a box-type resistance furnace at a speed of not more than one minuteHeating to 220 deg.C at a speed of 3 deg.C, maintaining the temperature for 4 hr, heating to 430 deg.C at a speed of no more than 3 deg.C per minute, maintaining the temperature for 3 hr, and naturally cooling to room temperature to obtain B; adding the A into a hydrazine hydrate aqueous solution with the mass fraction of 16% under continuous stirring, heating to 45 ℃, stirring at constant temperature for 4.5 hours, adding the B into the hydrazine hydrate aqueous solution, continuously stirring at constant temperature for 3 hours, naturally cooling, filtering, washing with deionized water for 3 times, and drying in a vacuum oven at 65 ℃ to obtain the graphene-loaded Cr2O3CuO and Nd2O3To form the composite powder material.
And (3) analysis: the composite sensitive material is subjected to component analysis, and the measured mass percentage is 19.5% of Cr2O3、15.3％CuO、12.4％Nd2O3And 52.8% C.
The application comprises the following steps: the sensitive material is used for detecting formaldehyde, benzene, ammonia and carbon monoxide, and the linear range of the sensitive material is 0.08-60mg/m of formaldehyde30.8-70mg/m of benzene31-80mg/m of ammonia3And carbon monoxide 1-100mg/m3The detection limit is 0.05mg/m of formaldehyde30.4mg/m benzene30.5mg/m of ammonia3And carbon monoxide 0.8mg/m3Common co-occurrences do not interfere.
Example 3
Slowly adding natural graphite into concentrated sulfuric acid under continuous stirring, slowly adding potassium permanganate with the weight 1.5 times that of the natural graphite after stirring for 3.5 hours, heating to 40 ℃, continuously stirring for 5 hours, naturally cooling to room temperature, performing suction filtration, and washing a filtrate to be neutral to obtain A; dissolving 6 parts of chromium acetate hydrate and chromium sulfate hydrate in 28% of citric acid aqueous solution, dissolving copper phosphate and 8 parts of neodymium sulfate hydrate in 16% of hydrochloric acid aqueous solution, mixing and stirring the two solutions for 2 hours under continuous stirring, heating to 93 ℃, adding agar powder, stirring until the agar powder is completely dissolved, cooling to room temperature to form gel, drying the gel, heating to 230 ℃ in a box-type resistance furnace at a speed of not more than 3 ℃ per minute, keeping the temperature for 4 hours, continuously heating to 420 ℃ at a speed of not more than 3 ℃ per minute, keeping the temperature for 3 hours, and naturally cooling to room temperature to obtain B; in successionAdding the A into a hydrazine hydrate aqueous solution with the mass fraction of 18% while stirring, heating to 45 ℃, stirring at constant temperature for 4 hours, adding the B into the hydrazine hydrate aqueous solution, continuously stirring at constant temperature for 2.5 hours, naturally cooling, filtering, washing with deionized water for 3 times, and drying in a vacuum oven at 65 ℃ to obtain the graphene-loaded Cr2O3CuO and Nd2O3To form the composite powder material.
And (3) analysis: the composite sensitive material is subjected to component analysis, and the measured mass percentage is 18.1% of Cr2O3、14.7％CuO、15.0％Nd2O3And 52.2% C.
The application comprises the following steps: the sensitive material is used for detecting formaldehyde, benzene, ammonia and carbon monoxide, and the linear range of the sensitive material is 0.1-69mg/m of formaldehyde30.7-75mg/m of benzene30.8-80mg/m of benzene3And carbon monoxide 2-100mg/m3The detection limit is 0.05mg/m of formaldehyde30.3mg/m benzene30.4mg/m of ammonia3And carbon monoxide 1mg/m3Common co-occurrences do not interfere.
Example 4
Slowly adding natural graphite into concentrated sulfuric acid under continuous stirring, slowly adding potassium permanganate with the weight 1.5 times that of the natural graphite after stirring for 3 hours, heating to 44 ℃, continuously stirring for 3.5 hours, naturally cooling to room temperature, performing suction filtration, and washing a filtrate to be neutral to obtain A; dissolving chromium oxalate and chromium sulfate in a citric acid aqueous solution with the mass fraction of 22%, dissolving 5 parts of copper sulfate hydrate, copper phosphate, 10 parts of neodymium oxalate hydrate and neodymium perchlorate in a hydrochloric acid aqueous solution with the mass fraction of 20%, mixing and stirring the two solutions for 2 hours under continuous stirring, adding agar powder after heating to 94 ℃, stirring until the two solutions are completely dissolved, cooling to room temperature to form gel, drying the gel, heating to 240 ℃ in a box-type resistance furnace at the speed of not more than 3 ℃ per minute, keeping the temperature for 4 hours, continuously heating to 410 ℃ at the speed of not more than 3 ℃ per minute, keeping the temperature for 3 hours, and naturally cooling to the room temperature to obtain B; adding A into 20% hydrazine hydrate water solution under continuous stirring, heating to 45 deg.C, stirring at constant temperature for 5 hr, adding B, and stirring at constant temperatureNaturally cooling for 2 hours, filtering, washing with deionized water for 3 times, and drying in a vacuum oven at 65 ℃ to obtain the graphene-loaded Cr2O3CuO and Nd2O3To form the composite powder material.
And (3) analysis: the composite sensitive material is subjected to component analysis, and the measured mass percentage is 15.8% of Cr2O3、11.6％CuO、14.3％Nd2O3And 58.3% C.
The application comprises the following steps: the sensitive material is used for detecting formaldehyde, benzene, ammonia and carbon monoxide, and the linear range of the sensitive material is 0.1-70mg/m of formaldehyde30.8-80mg/m of benzene30.8-80mg/m of ammonia3And carbon monoxide 1-100mg/m3The detection limit is 0.05mg/m of formaldehyde30.5mg/m benzene30.5mg/m of ammonia3And carbon monoxide 0.8mg/m3Common co-occurrences do not interfere.
Example 5
Slowly adding natural graphite into concentrated sulfuric acid under continuous stirring, slowly adding potassium permanganate with the weight 1.5 times that of the natural graphite after stirring for 4 hours, heating to 42 ℃, continuously stirring for 4 hours, naturally cooling to room temperature, performing suction filtration, and washing a filtrate to be neutral to obtain A; dissolving 9 parts of chromium nitrate hydrate in 25% of citric acid aqueous solution, dissolving 3 parts of copper nitrate hydrate and 4 parts of neodymium acetate hydrate in 15% of hydrochloric acid aqueous solution, mixing and stirring the two solutions for 2 hours under continuous stirring, heating to 95 ℃, adding agar powder, stirring until the agar powder is completely dissolved, cooling to room temperature to form gel, drying the gel, heating to 250 ℃ in a box-type resistance furnace at a speed of not more than 3 ℃ per minute, keeping the temperature for 4 hours, continuously heating to 400 ℃ at a speed of not more than 3 ℃ per minute, keeping the temperature for 3 hours, and naturally cooling to room temperature to obtain B; under the condition of continuous stirring, adding the A into a hydrazine hydrate aqueous solution with the mass fraction of 19%, heating to 45 ℃, stirring at constant temperature for 4 hours, adding the B into the hydrazine hydrate aqueous solution, continuously stirring at constant temperature for 3 hours, naturally cooling, filtering, washing with deionized water for 3 times, and then placing the mixture into a vacuum oven at 65 ℃ for drying to obtain the graphene-loaded Cr2O3CuO and Nd2O3To form the composite powder material.
And (3) analysis: the composite sensitive material is subjected to component analysis, and the mass percent of the Cr is measured to be 17.7 percent2O3、13.3％CuO、18.6％Nd2O3And 50.4% C.
The application comprises the following steps: the sensitive material is used for detecting formaldehyde, benzene, ammonia and carbon monoxide, and the linear range of the sensitive material is 0.09-50mg/m of formaldehyde30.6-60mg/m of benzene30.7-80mg/m of ammonia3And carbon monoxide 1-100mg/m3The detection limit is 0.05mg/m of formaldehyde30.2mg/m benzene30.3mg/m of ammonia3And carbon monoxide 0.8mg/m3Common co-occurrences do not interfere.
Claims (1)
1. A cross-sensitive material for formaldehyde, benzene, ammonia and CO in air features that the graphene carried Cr2O3CuO and Nd2O3The catalytic luminescent sensitive material comprises the following components in percentage by mass of 15-20% of Cr2O3、10-16％CuO、12-20％Nd2O3And 50-60% of C, and the preparation method comprises the following steps: slowly adding natural graphite into concentrated sulfuric acid under continuous stirring, slowly adding potassium permanganate with the weight 1.5 times that of the natural graphite after stirring for 3-4 hours, heating to 40-45 ℃, continuously stirring for 3-5 hours, naturally cooling to room temperature, performing suction filtration, and washing a filtrate to be neutral to obtain A; dissolving chromium salt in a citric acid aqueous solution with the mass fraction of 20-30%, dissolving copper salt and neodymium salt in a hydrochloric acid aqueous solution with the mass fraction of 15-20%, mixing and stirring the two solutions for 2 hours under continuous stirring, heating to 90-95 ℃, adding agar powder, stirring until the two solutions are completely dissolved, cooling to room temperature to form gel, drying the gel, heating to 250 ℃ at the speed of not more than 3 ℃ per minute in a box-type resistance furnace, keeping the temperature for 4 hours, continuously heating to 450 ℃ at the speed of not more than 3 ℃ per minute, keeping the temperature for 3 hours, and naturally cooling to room temperature to obtain B; adding A into 15-20 wt% hydrazine hydrate water solution under continuous stirring, heating to 45 deg.C, stirring at constant temperature for 4-5 hr, adding B, and continuing to addStirring for 2-3 hours at constant temperature, naturally cooling, filtering, washing with deionized water for 3 times, and drying in a vacuum oven at 65 ℃ to obtain the graphene-loaded Cr2O3CuO and Nd2O3Composite powder material; 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 copper salt is one or a mixture of more of anhydrous substances or hydrates of copper chloride, copper sulfate, copper phosphate and copper nitrate, and the neodymium salt is one or a mixture of more of anhydrous substances or hydrates of neodymium nitrate, neodymium oxalate, neodymium sulfate, neodymium chloride, neodymium acetate and neodymium perchlorate.
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| CN110095559B (en) * | 2019-04-03 | 2021-09-14 | 北京联合大学 | Catalytic luminous sensitive material of low-temperature formaldehyde, benzene and ammonia |
| CN110095560B (en) * | 2019-04-18 | 2021-10-08 | 北京联合大学 | Low-temperature high-selectivity carbon monoxide sensitive material |
| CN110455978B (en) * | 2019-06-30 | 2021-09-14 | 北京联合大学 | Benzene and ammonia low-temperature catalytic luminescence cross-sensitive material |
| CN110658186B (en) * | 2019-10-22 | 2021-08-13 | 北京联合大学 | Sensitive material for simultaneously measuring formaldehyde, benzene and carbon monoxide |
| CN111638207B (en) * | 2020-05-13 | 2023-04-21 | 北京联合大学 | Sensitive material for low temperature formaldehyde, ammonia and carbon monoxide |
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