CN111638208A - Low temperature carbon monoxide and formaldehyde cross-sensitive material - Google Patents
Low temperature carbon monoxide and formaldehyde cross-sensitive material Download PDFInfo
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- CN111638208A CN111638208A CN202010409735.5A CN202010409735A CN111638208A CN 111638208 A CN111638208 A CN 111638208A CN 202010409735 A CN202010409735 A CN 202010409735A CN 111638208 A CN111638208 A CN 111638208A
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- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 title claims abstract description 99
- 239000000463 material Substances 0.000 title claims abstract description 47
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 229910002091 carbon monoxide Inorganic materials 0.000 title claims abstract description 33
- 229910021382 natural graphite Inorganic materials 0.000 claims abstract description 29
- 239000000843 powder Substances 0.000 claims abstract description 27
- 239000002131 composite material Substances 0.000 claims abstract description 21
- 239000007864 aqueous solution Substances 0.000 claims abstract description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 15
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 15
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 13
- 239000010955 niobium Substances 0.000 claims abstract description 10
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims abstract description 10
- 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 8
- 239000002253 acid Substances 0.000 claims abstract description 8
- XFHGGMBZPXFEOU-UHFFFAOYSA-I azanium;niobium(5+);oxalate Chemical compound [NH4+].[Nb+5].[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O.[O-]C(=O)C([O-])=O XFHGGMBZPXFEOU-UHFFFAOYSA-I 0.000 claims abstract description 8
- 239000008103 glucose Substances 0.000 claims abstract description 8
- 238000005406 washing Methods 0.000 claims abstract description 8
- 150000001868 cobalt Chemical class 0.000 claims abstract description 5
- 239000000203 mixture Substances 0.000 claims description 45
- 238000003756 stirring Methods 0.000 claims description 32
- 238000010438 heat treatment Methods 0.000 claims description 31
- 238000001816 cooling Methods 0.000 claims description 28
- 239000000243 solution Substances 0.000 claims description 20
- BEFDCLMNVWHSGT-UHFFFAOYSA-N ethenylcyclopentane Chemical compound C=CC1CCCC1 BEFDCLMNVWHSGT-UHFFFAOYSA-N 0.000 claims description 15
- 239000004334 sorbic acid Substances 0.000 claims description 15
- 229940075582 sorbic acid Drugs 0.000 claims description 15
- 235000010199 sorbic acid Nutrition 0.000 claims description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 14
- 238000009775 high-speed stirring Methods 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 230000032683 aging Effects 0.000 claims description 8
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 7
- 229910052799 carbon Inorganic materials 0.000 claims description 7
- 239000008367 deionised water Substances 0.000 claims description 7
- 229910021641 deionized water Inorganic materials 0.000 claims description 7
- 238000001704 evaporation Methods 0.000 claims description 7
- 239000012065 filter cake Substances 0.000 claims description 7
- 239000000706 filtrate Substances 0.000 claims description 7
- 238000000227 grinding Methods 0.000 claims description 7
- 230000007935 neutral effect Effects 0.000 claims description 7
- 239000012286 potassium permanganate Substances 0.000 claims description 7
- 238000000967 suction filtration Methods 0.000 claims description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 7
- 229940011182 cobalt acetate Drugs 0.000 claims description 2
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 2
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 2
- 229940044175 cobalt sulfate Drugs 0.000 claims description 2
- 229910000361 cobalt sulfate Inorganic materials 0.000 claims description 2
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 claims description 2
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 claims description 2
- -1 cobalt chloride anhydride Chemical class 0.000 claims 1
- 230000035945 sensitivity Effects 0.000 abstract description 5
- 238000002360 preparation method Methods 0.000 abstract description 2
- QVQLCTNNEUAWMS-UHFFFAOYSA-N barium oxide Chemical compound [Ba]=O QVQLCTNNEUAWMS-UHFFFAOYSA-N 0.000 abstract 2
- 229910000428 cobalt oxide Inorganic materials 0.000 abstract 1
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 abstract 1
- 238000001914 filtration Methods 0.000 abstract 1
- 229910000476 molybdenum oxide Inorganic materials 0.000 abstract 1
- 229910000484 niobium oxide Inorganic materials 0.000 abstract 1
- URLJKFSTXLNXLG-UHFFFAOYSA-N niobium(5+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Nb+5].[Nb+5] URLJKFSTXLNXLG-UHFFFAOYSA-N 0.000 abstract 1
- PQQKPALAQIIWST-UHFFFAOYSA-N oxomolybdenum Chemical compound [Mo]=O PQQKPALAQIIWST-UHFFFAOYSA-N 0.000 abstract 1
- 238000006722 reduction reaction Methods 0.000 abstract 1
- 238000004458 analytical method Methods 0.000 description 10
- 239000007789 gas Substances 0.000 description 9
- 238000001514 detection method Methods 0.000 description 8
- 238000002485 combustion reaction Methods 0.000 description 5
- 238000004519 manufacturing process Methods 0.000 description 5
- 102000001554 Hemoglobins Human genes 0.000 description 4
- 108010054147 Hemoglobins Proteins 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 230000003197 catalytic effect Effects 0.000 description 3
- 239000003344 environmental pollutant Substances 0.000 description 3
- 238000004880 explosion Methods 0.000 description 3
- 231100000719 pollutant Toxicity 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- MEYVLGVRTYSQHI-UHFFFAOYSA-L cobalt(2+) sulfate heptahydrate Chemical compound O.O.O.O.O.O.O.[Co+2].[O-]S([O-])(=O)=O MEYVLGVRTYSQHI-UHFFFAOYSA-L 0.000 description 2
- ZBYYWKJVSFHYJL-UHFFFAOYSA-L cobalt(2+);diacetate;tetrahydrate Chemical compound O.O.O.O.[Co+2].CC([O-])=O.CC([O-])=O ZBYYWKJVSFHYJL-UHFFFAOYSA-L 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 208000031404 Chromosome Aberrations Diseases 0.000 description 1
- 208000014085 Chronic respiratory disease Diseases 0.000 description 1
- 206010067477 Cytogenetic abnormality Diseases 0.000 description 1
- 208000000059 Dyspnea Diseases 0.000 description 1
- 206010013975 Dyspnoeas Diseases 0.000 description 1
- 206010021143 Hypoxia Diseases 0.000 description 1
- 206010023644 Lacrimation increased Diseases 0.000 description 1
- YGYAWVDWMABLBF-UHFFFAOYSA-N Phosgene Chemical compound ClC(Cl)=O YGYAWVDWMABLBF-UHFFFAOYSA-N 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 208000006673 asthma Diseases 0.000 description 1
- 238000005422 blasting Methods 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 239000013064 chemical raw material Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
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- 238000000576 coating method Methods 0.000 description 1
- GFHNAMRJFCEERV-UHFFFAOYSA-L cobalt chloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Co+2] GFHNAMRJFCEERV-UHFFFAOYSA-L 0.000 description 1
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 description 1
- QGUAJWGNOXCYJF-UHFFFAOYSA-N cobalt dinitrate hexahydrate Chemical compound O.O.O.O.O.O.[Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O QGUAJWGNOXCYJF-UHFFFAOYSA-N 0.000 description 1
- 238000004939 coking Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000000645 desinfectant Substances 0.000 description 1
- 239000002283 diesel fuel Substances 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 239000002360 explosive Substances 0.000 description 1
- 230000032686 female pregnancy Effects 0.000 description 1
- 238000005242 forging Methods 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 238000004817 gas chromatography Methods 0.000 description 1
- 239000003502 gasoline Substances 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000003721 gunpowder Substances 0.000 description 1
- 238000003905 indoor air pollution Methods 0.000 description 1
- 229940087654 iron carbonyl Drugs 0.000 description 1
- 230000004317 lacrimation Effects 0.000 description 1
- 238000004811 liquid chromatography Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000002796 luminescence method Methods 0.000 description 1
- 238000004020 luminiscence type Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- DLCOPLYGCSRNAY-UHFFFAOYSA-N molybdenum titanium vanadium Chemical compound [Ti][Mo][V] DLCOPLYGCSRNAY-UHFFFAOYSA-N 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 1
- 231100000344 non-irritating Toxicity 0.000 description 1
- 230000009965 odorless effect Effects 0.000 description 1
- 239000005022 packaging material Substances 0.000 description 1
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- 239000002994 raw material Substances 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
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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
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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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- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
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- Pathology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
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- Carbon And Carbon Compounds (AREA)
- Investigating Or Analyzing Materials By The Use Of Fluid Adsorption Or Reactions (AREA)
Abstract
The invention relates to a low-temperature carbon monoxide and formaldehyde cross-sensitive material which is characterized in that graphene-loaded Pt atoms are doped with CoO and Nb2O5To form the composite powder material. The preparation method comprises the following steps: firstly, preparing graphene oxide from natural graphite; then, preparing cobalt oxide and niobium oxide from cobalt salt and ammonium niobium oxalate; finally, chloroplatinic acid is added into the glucose aqueous solution, graphene oxide, barium oxide and molybdenum oxide are added into the aqueous solution, and reduction, filtration, washing and drying are carried out to obtain the Pt atom-doped CoO and Nb loaded with graphene2O5To form the composite powder material. The gas sensor made of the sensitive material provided by the invention can be used for measuring trace carbon monoxide and formaldehyde in the air at a low temperature with high sensitivity without being interfered by other common coexisting molecules.
Description
Technical Field
The invention relates to a low-temperature carbon monoxide and formaldehyde cross-sensitive material, in particular to a graphene-loaded Pt atom-doped CoO and Nb composite material2O5The composite powder material belongs to the field of sensing technology.
Background
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. The main source of atmospheric CO is engine exhaust, followed by the combustion of fossil fuels in boilers. 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. Carbon monoxide can be combined with hemoglobin in blood after entering a human body, and the combination capability of CO and hemoglobin is far stronger than that of oxygen and hemoglobin, so that the quantity of hemoglobin capable of being combined with oxygen is reduced sharply, and the oxygen deficiency of organism tissues is caused, and the human body is suffocated to die.
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)3Below) can cause diseases such as chronic respiratory disease, female pregnancy syndrome, newborn physique reduction and chromosome abnormality.
The accurate detection means of carbon monoxide and formaldehyde mainly comprise: spectrophotometry, electrochemistry, gas chromatography, liquid chromatography, chemiluminescence, and the like, which all have relatively high sensitivity, but require pre-enrichment with an atmospheric sampler and appropriate processing of the collected sample to complete the measurement with an analytical instrument, and therefore must be done in a laboratory and cannot be done on site. In recent years, indoor air pollution is becoming more serious due to the use of indoor decoration and various modern living goods. Formaldehyde and carbon monoxide are the main pollutants of indoor air. Therefore, the technology and the method for rapidly and accurately measuring the trace carbon monoxide and formaldehyde in the air have very strong practical significance.
The patent ZL201210014164.0 discloses a nano sensitive material for monitoring carbon monoxide. In a paper published in the journal of chemistry and entitled 'measuring formaldehyde in air by a nanometer composite oxide catalytic luminescence method', an improved nanometer-level molybdenum-vanadium-titanium (atomic ratio is 2: 3: 5) composite oxide is used as a sensitive material, and 0.07-34 mg/m of online detection can be realized3The detection limit of the formaldehyde can reach 0.04mg/m3. However, these sensitive materials are used at temperatures in excess of 300 ℃, and the background of the thermal radiation generated by such temperatures can form a strong baseline signal, which can seriously affect 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 carbon monoxide and formaldehyde at lower temperature. The gas sensor made of the sensitive material has small background signal, greatly improves the sensitivity to carbon monoxide and formaldehyde, and can simultaneously measure trace carbon monoxide and formaldehyde in the air without being interfered by common coexisting molecules.
The sensitive material is prepared by doping Pt atoms loaded by graphene and is formed by CoO and Nb2O5The preparation method of the composite powder material comprises the following steps:
slowly adding natural graphite into aqueous hydrogen peroxide solution with the mass fraction of 15% of 1/2 natural graphite under continuous stirring, adding 2/3 parts of potassium permanganate with the weight of the natural graphite and concentrated sulfuric acid with the weight equal to that of the natural graphite under continuous stirring, heating to 55-60 ℃, continuously stirring for 5 hours, naturally cooling to room temperature, carrying out suction filtration, and washing a filtrate to be neutral to obtain A; co-dissolving cobalt salt and ammonium niobium oxalate which are easy to dissolve in waterHeating to 50 ℃ in a 10 mass percent hydrochloric acid aqueous solution, adding sorbic acid under the high-speed stirring state to keep the solution clear, cooling to room temperature, standing and aging for 6-8 hours, heating to 60 ℃, continuing to add sorbic acid under the high-speed stirring state to keep the solution clear, rotationally evaporating the solution at 85-90 ℃ to remove 1/2 moisture, cooling to room temperature to obtain gel, drying the gel for 2 hours, fully grinding, heating to 250 ℃ at a speed of not more than 3 ℃ per minute in a box-type resistance furnace, keeping the temperature for 5 hours, continuing to heat to 350 ℃ 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, chloroplatinic acid is added into a glucose aqueous solution with the mass fraction of 20-25%, the mixture is stirred at the constant temperature of 30-35 ℃ until the mixture is clear, then A is added, the mixture is heated to 50 ℃, the mixture is stirred at the constant temperature for 3-4 hours, B is added, the mixture is stirred at the constant temperature for 4-5 hours, the mixture is naturally cooled to the room temperature, filtered, a filter cake is washed for 3 times by deionized water and then placed in a vacuum oven at the temperature of 60 ℃ for drying, and the graphene-loaded Pt atom-doped CoO and Nb are obtained2O5To form the composite powder material.
Wherein the cobalt salt is one or more of anhydrous substances or hydrate of cobalt nitrate, cobalt sulfate, cobalt acetate and cobalt chloride.
When the mass fractions of all the components of the prepared composite sensitive material meet the requirements of Pt (0.6-1.2%), CoO (15-20%) and Nb2O5(15-20%) and C (61-69%), and has high sensitivity and selectivity when used as a catalytic luminescent sensitive material for trace formaldehyde and carbon monoxide in air.
Detailed Description
Example 1
Slowly adding natural graphite into aqueous hydrogen peroxide solution with the mass fraction of 15% of 1/2 natural graphite under continuous stirring, adding 2/3 parts of potassium permanganate with the weight of the natural graphite and concentrated sulfuric acid with the weight equal to that of the natural graphite under continuous stirring, heating to 55 ℃, continuously stirring for 5 hours, naturally cooling to room temperature, carrying out suction filtration, and washing a filtrate to be neutral to obtain A; dissolving cobalt nitrate hexahydrate and ammonium niobium oxalate which are easy to dissolve in water into mass componentsAdding sorbic acid into 10% hydrochloric acid aqueous solution, heating to 50 ℃, adding sorbic acid under a high-speed stirring state to keep the solution clear, cooling to room temperature, standing and aging for 8 hours, heating to 60 ℃, continuing to add sorbic acid under the high-speed stirring state to keep the solution clear, rotationally evaporating 1/2 moisture at 85 ℃, cooling to room temperature to obtain gel, drying the gel for 2 hours, fully grinding, heating to 250 ℃ in a box-type resistance furnace at a speed of not more than 3 ℃ per minute, keeping the temperature for 5 hours, continuing to heat to 300 ℃ 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, chloroplatinic acid is added into a glucose aqueous solution with the mass fraction of 25%, the mixture is stirred at the constant temperature of 35 ℃ until the mixture is clear, then A is added, the mixture is heated to 50 ℃, the mixture is stirred at the constant temperature for 4 hours, B is added, the mixture is stirred at the constant temperature for 4 hours, the mixture is naturally cooled to the room temperature, filtered, filter cakes are washed for 3 times by deionized water and then placed in a vacuum oven at the temperature of 60 ℃ for drying, and the graphene-loaded Pt atom-doped CoO and Nb are obtained2O5To 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, 15.8 percent of CoO and 18.2 percent of Nb2O5And 65.1% C.
The application comprises the following steps: the powder material is used as a sensitive material for detecting formaldehyde and carbon monoxide, and the linear range of the powder material is 0.06-54mg/m of formaldehyde3And carbon monoxide 0.5-65mg/m3The detection limit is 0.02mg/m of formaldehyde3And carbon monoxide 0.2mg/m3And the working temperature is 200 ℃.
Example 2
Slowly adding natural graphite into aqueous hydrogen peroxide solution with the mass fraction of 15% of 1/2 natural graphite under continuous stirring, adding 2/3 parts of potassium permanganate with the weight of the natural graphite and concentrated sulfuric acid with the weight equal to that of the natural graphite under continuous stirring, heating to 56 ℃, continuously stirring for 5 hours, naturally cooling to room temperature, carrying out suction filtration, and washing a filtrate to be neutral to obtain A; dissolving water-soluble cobalt sulfate heptahydrate and ammonium niobium oxalate in 10 wt% hydrochloric acid aqueous solution, heating to 50 deg.C, and stirring at high speedAdding sorbic acid under the state of keeping the solution clear, cooling to room temperature, standing and aging for 6 hours, heating to 60 ℃, continuously adding sorbic acid under the state of high-speed stirring and keeping the solution clear, rotationally evaporating the solution at 86 ℃ to remove 1/2 moisture, cooling to room temperature to obtain gel, drying the gel for 2 hours, fully grinding, heating to 240 ℃ in a box-type resistance furnace at the speed of not more than 3 ℃ per minute, keeping the temperature for 5 hours, continuously heating to 310 ℃ 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; under the condition of continuous stirring, chloroplatinic acid is added into a glucose aqueous solution with the mass fraction of 23%, the mixture is stirred at the constant temperature of 33 ℃ until the mixture is clear, then A is added, the mixture is heated to 50 ℃, the mixture is stirred at the constant temperature for 3 hours, B is added, the mixture is stirred at the constant temperature for 4 hours, the mixture is naturally cooled to the room temperature, filtered, filter cakes are washed for 3 times by deionized water and then placed in a vacuum oven at the temperature of 60 ℃ for drying, and the graphene-loaded Pt atom-doped CoO and Nb are obtained2O5To 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, 19.0 percent of CoO and 16.1 percent of Nb2O5And 64.2% C.
The application comprises the following steps: the powder material is used as a sensitive material for detecting formaldehyde and carbon monoxide, and the linear range of the powder material is 0.07-66mg/m of formaldehyde3And carbon monoxide 0.5-57mg/m3The detection limit is 0.03mg/m of formaldehyde3And carbon monoxide 0.2mg/m3And the working temperature is 190 ℃.
Example 3
Slowly adding natural graphite into aqueous hydrogen peroxide solution with the mass fraction of 15% of 1/2 natural graphite under continuous stirring, adding 2/3 parts of potassium permanganate with the weight of the natural graphite and concentrated sulfuric acid with the weight equal to that of the natural graphite under continuous stirring, heating to 57 ℃, continuously stirring for 5 hours, naturally cooling to room temperature, carrying out suction filtration, and washing a filtrate to be neutral to obtain A; dissolving readily water-soluble cobalt acetate tetrahydrate and ammonium niobium oxalate in 10% hydrochloric acid aqueous solution, heating to 50 deg.C, adding sorbic acid under high speed stirring to maintain the solution clear, cooling to room temperatureStanding and aging for hours, heating to 60 ℃, continuously adding sorbic acid under the high-speed stirring state, keeping the solution clear, rotatably evaporating 1/2 moisture of the solution at 87 ℃, cooling to room temperature to obtain gel, drying the gel for 2 hours, fully grinding, heating to 230 ℃ in a box-type resistance furnace at the speed of not more than 3 ℃ per minute, keeping the temperature for 5 hours, continuously heating to 320 ℃ 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; under the condition of continuous stirring, chloroplatinic acid is added into 22 percent glucose aqueous solution by mass fraction, the mixture is stirred at the constant temperature of 32 ℃ until the mixture is clear, then A is added, the mixture is heated to 50 ℃, the mixture is stirred at the constant temperature for 4 hours, B is added, the mixture is stirred at the constant temperature for 5 hours, the mixture is naturally cooled to the room temperature, the mixture is filtered, a filter cake is washed for 3 times by deionized water and then is placed in a vacuum oven at the temperature of 60 ℃ for drying, and the graphene-loaded Pt atom-doped CoO and Nb are obtained2O5To 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, 18.5 percent of CoO and 17.2 percent of Nb2O5And 63.7% C.
The application comprises the following steps: the powder material is used as a sensitive material for detecting formaldehyde and carbon monoxide, and the linear range of the powder material is 0.05-44mg/m of formaldehyde3And carbon monoxide 0.5-56mg/m3The detection limit is 0.02mg/m of formaldehyde3And carbon monoxide 0.2mg/m3And the working temperature is 210 ℃.
Example 4
Slowly adding natural graphite into aqueous hydrogen peroxide solution with the mass fraction of 15% of 1/2 natural graphite under continuous stirring, adding 2/3 parts of potassium permanganate with the weight of the natural graphite and concentrated sulfuric acid with the weight equal to that of the natural graphite under continuous stirring, heating to 58 ℃, continuously stirring for 5 hours, naturally cooling to room temperature, carrying out suction filtration, and washing a filtrate to be neutral to obtain A; dissolving water-soluble cobalt sulfate heptahydrate, cobalt acetate tetrahydrate and ammonium niobium oxalate in 10% hydrochloric acid aqueous solution, heating to 50 deg.C, adding sorbic acid under high-speed stirring to make the solution clear, cooling to room temperature, standing and aging for 8 hr, heating to 60 deg.C, and aging at high speedContinuously adding sorbic acid while stirring, keeping the solution clear, rotationally evaporating 1/2 moisture of the solution at 88 ℃, cooling to room temperature to obtain gel, drying the gel for 2 hours, fully grinding, heating to 220 ℃ in a box-type resistance furnace at a speed of not more than 3 ℃ per minute, keeping the temperature for 5 hours, continuously heating to 330 ℃ 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, chloroplatinic acid is added into a glucose aqueous solution with the mass fraction of 21%, the mixture is stirred at the constant temperature of 31 ℃ until the mixture is clear, then A is added, the mixture is heated to 50 ℃, the mixture is stirred at the constant temperature for 3 hours, B is added, the mixture is stirred at the constant temperature for 5 hours, the mixture is naturally cooled to the room temperature, filtered, filter cakes are washed for 3 times by deionized water and then placed in a vacuum oven at the temperature of 60 ℃ for drying, and the graphene-loaded Pt atom-doped CoO and Nb are obtained2O5To 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 1.2 percent of Pt, 16.7 percent of CoO and 19.6 percent of Nb2O5And 62.5% C.
The application comprises the following steps: the powder material is used as a sensitive material for detecting formaldehyde and carbon monoxide, and the linear range of the powder material is 0.07-65g/m of formaldehyde3And carbon monoxide 0.5-63mg/m3The detection limit is 0.03mg/m of formaldehyde3And carbon monoxide 0.2mg/m3And the working temperature is 185 ℃.
Example 5
Slowly adding natural graphite into aqueous hydrogen peroxide solution with the mass fraction of 15% of 1/2 natural graphite under continuous stirring, adding 2/3 parts of potassium permanganate with the weight of the natural graphite and concentrated sulfuric acid with the weight equal to that of the natural graphite under continuous stirring, heating to 60 ℃, continuously stirring for 5 hours, naturally cooling to room temperature, carrying out suction filtration, and washing a filtrate to be neutral to obtain A; dissolving cobalt chloride hexahydrate and ammonium niobium oxalate which are easy to dissolve in water into 10 percent hydrochloric acid aqueous solution by mass fraction, heating to 50 ℃, adding sorbic acid under the condition of high-speed stirring to keep the solution clear, cooling to room temperature, standing and aging for 6 hours, heating to 60 ℃, continuing to add sorbic acid under the condition of high-speed stirring to keep the solution clear, adding sodium bicarbonate into the mixture, stirring the mixture to obtain the product, and stirring the product to obtain the productRotationally evaporating 1/2 water from the solution at 90 ℃, cooling to room temperature to obtain gel, drying the gel for 2 hours, fully grinding, heating to 210 ℃ in a box-type resistance furnace at a speed of not more than 3 ℃ per minute, keeping the temperature for 5 hours, continuously heating to 340 ℃ 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, chloroplatinic acid is added into a glucose aqueous solution with the mass fraction of 20%, the mixture is stirred at the constant temperature of 30 ℃ until the mixture is clear, then A is added, the mixture is heated to 50 ℃, the mixture is stirred at the constant temperature for 4 hours, B is added, the mixture is stirred at the constant temperature for 4 hours, the mixture is naturally cooled to the room temperature, filtered, filter cakes are washed for 3 times by deionized water and then placed in a vacuum oven at the temperature of 60 ℃ for drying, and the graphene-loaded Pt atom-doped CoO and Nb are obtained2O5To 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 1.1 percent of Pt, 17.3 percent of CoO and 15.5 percent of Nb2O5And 66.1% C.
The application comprises the following steps: the powder material is used as a sensitive material for detecting formaldehyde and carbon monoxide, and the linear range of the powder material is 0.06-52mg/m of formaldehyde3And carbon monoxide 0.5-56mg/m3The detection limit is 0.02mg/m of formaldehyde3And carbon monoxide 0.2mg/m3And the working temperature is 190 ℃.
Claims (2)
1. A low-temperature carbon monoxide and formaldehyde cross-sensitive material is characterized in that a graphene-loaded Pt atom is doped with CoO and Nb2O5The composite powder material comprises 0.6-1.2% of Pt, 15-20% of CoO and 15-20% of Nb in percentage by mass2O5And 61-69% C, prepared by: slowly adding natural graphite into aqueous hydrogen peroxide solution with the mass fraction of 15% of 1/2 natural graphite under continuous stirring, adding 2/3 parts of potassium permanganate with the weight of the natural graphite and concentrated sulfuric acid with the weight equal to that of the natural graphite under continuous stirring, heating to 55-60 ℃, continuously stirring for 5 hours, naturally cooling to room temperature, carrying out suction filtration, and washing a filtrate to be neutral to obtain A; co-dissolving cobalt salt and ammonium niobium oxalate which are easy to dissolve in waterHeating to 50 ℃ in a 10 mass percent hydrochloric acid aqueous solution, adding sorbic acid under the high-speed stirring state to keep the solution clear, cooling to room temperature, standing and aging for 6-8 hours, heating to 60 ℃, continuing to add sorbic acid under the high-speed stirring state to keep the solution clear, rotationally evaporating the solution at 85-90 ℃ to remove 1/2 moisture, cooling to room temperature to obtain gel, drying the gel for 2 hours, fully grinding, heating to 250 ℃ at a speed of not more than 3 ℃ per minute in a box-type resistance furnace, keeping the temperature for 5 hours, continuing to heat to 350 ℃ 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, chloroplatinic acid is added into a glucose aqueous solution with the mass fraction of 20-25%, the mixture is stirred at the constant temperature of 30-35 ℃ until the mixture is clear, then A is added, the mixture is heated to 50 ℃, the mixture is stirred at the constant temperature for 3-4 hours, B is added, the mixture is stirred at the constant temperature for 4-5 hours, the mixture is naturally cooled to the room temperature, filtered, a filter cake is washed for 3 times by deionized water and then placed in a vacuum oven at the temperature of 60 ℃ for drying, and the graphene-loaded Pt atom-doped CoO and Nb are obtained2O5To form the composite powder material.
2. The material of claim 1, wherein the cobalt salt is one or more of cobalt nitrate, cobalt sulfate, cobalt acetate, and cobalt chloride anhydride or hydrate.
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