CN105628856A - Luminescent sensitive material catalyzed by benzene and sulfur dioxide - Google Patents
Luminescent sensitive material catalyzed by benzene and sulfur dioxide Download PDFInfo
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Abstract
The invention discloses a luminescent sensitive material catalyzed by benzene and sulfur dioxide, which is characterized in that the material is a graphene-loaded composite material prepared from Bi2O3, PbO and In2O3. The preparation method comprises the following steps of oxidizing natural graphite by utilization of fuming sulfuric acid, a potassium permanganate concentrated sulfuric acid solution and hydrogen peroxide respectively so as to prepare graphene oxide; preparing bismuth oxalate, lead acetate and indium nitrate into a solution, adding agar powder to form gel, and drying, sintering and cooling the gel so as to obtain a complex metal oxide composed of Bi2O3, PbO and In2O3; adding the complex metal oxide and the graphene oxide into a hydrazine hydrate solution, illuminating the solution by utilization of an xenon lamp, and filtering and drying to obtain the graphene-loaded composite material prepared from Bi2O3, PbO and In2O3. The sensitive material provided by the invention has the advantage that the operation of quickly and accurately measuring trace benzene and sulfur dioxide in the air on site can be performed without the interference of common coexistent substances by a gas sensor made of the sensitive material.
Description
Technical field
The present invention relates to the catalytic luminescence sensitive material of a kind of benzene and sulfur dioxide, particularly by graphene-supported Bi2O3, PbO and In2O3The composite of composition, belongs to new catalytic material technical field.
Background technology
Benzene is a kind of industrial chemicals with aromatic odor, and the benzene in air is mainly derived from building coating, paint for decoration, adhesive solvent and vehicle exhaust etc. Skin, eyes and upper respiratory tract are mainly had stimulation by Chronic Benzene Poisoning; Often in contact with benzene, skin can because of defat desiccation desquamation, some appearance allergic eczemas; The long-term benzene that sucks can cause aplastic anemia. Benzene is confirmed as carcinogen by IARC (IARC), is the major pollutants of room air.
Sulfur dioxide is one of major pollutants in air, and sulfur dioxide has acidity, with other substance reactions in air, can generate small sulphite and sulphate particle. When these granules are inhaled into, they will be gathered in pulmonary, be the one of the main reasons of Respiratory symptoms and disease. During with eye contact, redness and pain can be caused. After sulfur dioxide enters respiratory tract, because it is soluble in water, therefore major part is arrested in upper respiratory tract, generates and has corrosive sulfurous acid, sulphuric acid and sulfate, make stimulation strengthen on moistening mucosa. When sulfur dioxide concentration is 10��15ppm, the secretory function of respiratory tract ciliary movement and mucosa all can be suppressed. When concentration reaches 20ppm, cause cough and stimulate eyes. If every day, inhaled concentration was that 100ppm reaches 8 hours, there is obvious irritation in bronchus and pulmonary, make damaged lung tissue. People can be made when concentration reaches 400ppm to produce dyspnea. Sulfur dioxide is inhaled into together with floating dust, and floating dust aerosol particles can take pulmonary to sulfur dioxide makes toxicity increase by 3��4 times. If floating dust surface adsorption metal particle, under its catalytic action, making oxidizing sulfur dioxide is sulfuric acid mist, and its stimulation is more higher than sulfur dioxide. Live in the environment of atmospheric pollution for a long time, due to the synergy of sulfur dioxide and floating dust, alveolar fibroplasia can be promoted. If hypertrophy scope involves extensively, forming fibrous lesions, development goes down to make fibrous fracture to form emphysema. Sulfur dioxide can add the carcinogenesis of strong carcinogen benzopyrene. According to animal experiment, under the synergy of sulfur dioxide and benzopyrene, the sickness rate of animal pulmonary carcinoma, higher than the sickness rate of the single factor, can bring out pulmonary's squamous cell carcinoma in a short time.
The detection method of benzene in air and sulfur dioxide mainly has: spectrophotography, fluorimetry, Flow Injection Chemiluminescence, gas chromatography, liquid chromatography and electrochemical process etc. These method sensitivity are all higher, but complicated operation, it is necessary to complete at laboratory, it is impossible to on-the-spot realization.
Summary of the invention
It is an object of the invention to overcome the deficiency of conventional art, it is provided that a kind of have higher selective catalytic luminescence sensitive material to benzene and sulfur dioxide. The monitoring benzene made of this sensitive material and the gas sensor of sulfur dioxide, it is possible to micro-benzene and sulfur dioxide at the scene quickly, in Accurate Determining air and not by the interference of common concurrent.
The catalytic luminescence sensitive material of a kind of benzene of the present invention and sulfur dioxide is graphene-supported by Bi2O3, PbO and In2O3The composite of composition, it is possible to prepared by native graphite, bismuth salt, lead salt and indium salts. Wherein, the preparation method being primary raw material with Oxalic acid bismuth salt., lead acetate and indium nitrate is:
(1) being slowly added to by native graphite in the oleum of 40 DEG C with continuous stirring, constant temperature stirs and is slowly added to after 2 hours and the phosphoric acid of the weight such as native graphite, continues constant temperature and stirs 3 hours, and much filtrate is also washed to neutrality by sucking filtration; Filter cake is added in the potassium permanganate concentrated sulfuric acid solution that mass fraction is 15%, it is warming up to 45-55 DEG C of also continuous stirring 2 hours, it is slowly added to aqueous hydrogen peroxide solution that mass fraction is 25% to bubble-free, continue constant temperature to stir 1 hour, much filtrate is also washed to neutrality by sucking filtration, obtains graphene oxide;
(2) Oxalic acid bismuth salt. is dissolved in the aqueous hydrochloric acid solution that mass fraction is 10-20% and forms solution A, it is formation solution B in 20-30% aqueous citric acid solution that lead acetate is dissolved in mass fraction, is dissolved in by indium nitrate in the isobutanol aqueous solution that mass fraction is 30-40% and forms solution C; With continuous stirring, solution A and solution B are slowly added in solution C successively, after stirring 2 hours, add a small amount of agar powder and continue stirring formation gel; After this gel is dried, chamber type electric resistance furnace is warming up to 200-250 DEG C with the speed less than 3 DEG C per minute, keeps this temperature 4 hours, continue to be warming up to 450-500 DEG C with the speed less than 3 DEG C per minute, keep this temperature 3 hours, naturally cool to room temperature and obtain by Bi2O3, PbO and In2O3The metal composite oxide of composition; With continuous stirring, this metal composite oxide is added in the hydrazine hydrate aqueous solution that mass fraction is 20%, then aforesaid graphene oxide is also added wherein, it is warming up to 40 DEG C, constant temperature stirs 4 hours, irradiates 3 hours with the xenon lamps of 300 watts, uses deionized water wash 3 times after filtration, it is subsequently placed in 60 DEG C of vacuum drying ovens to dry, namely obtains graphene-supported by Bi2O3, PbO and In2O3The composite powder material of composition.
Wherein, bismuth salt is the mixture of one or more of the anhydride of bismuth acetate, Oxalic acid bismuth salt., bismuth nitrate, bismuth sulfate, Bismugel (Biothrax). and bismuth trichloride or hydrate, lead salt is the mixture of one or more of the anhydride of plumbi nitras, lead acetate and Lead sulfocyanate. or hydrate, and indium salts is one or both mixture of the anhydride of indium chloride, indium nitrate, indium sulfate, indium acetate and indium phosphate or hydrate.
When the prepared each constituent mass mark of composite meets Bi2O3(10-20%), PbO (15-25%), In2O3(14-24%) time with C (45-60%), for there is significantly high susceptiveness and selectivity as the catalytic luminescence sensitive material measuring benzene and sulfur dioxide.
Detailed description of the invention
Embodiment 1
[1] being slowly added to by native graphite in the oleum of 40 DEG C with continuous stirring, constant temperature stirs and is slowly added to after 2 hours and the phosphoric acid of the weight such as native graphite, continues constant temperature and stirs 3 hours, and much filtrate is also washed to neutrality by sucking filtration; Filter cake is added in the potassium permanganate concentrated sulfuric acid solution that mass fraction is 15%, it is warming up to 50 DEG C of also continuous stirring 2 hours, it is slowly added to aqueous hydrogen peroxide solution that mass fraction is 25% to bubble-free, continue constant temperature to stir 1 hour, much filtrate is also washed to neutrality by sucking filtration, obtains graphene oxide;
[2] seven water Oxalic acid bismuth salt .s are dissolved in the aqueous hydrochloric acid solution that mass fraction is 15% and form solution A, it is formation solution B in 25% aqueous citric acid solution that acetate trihydrate lead is dissolved in mass fraction, is dissolved in by nitrate trihydrate indium in the isobutanol aqueous solution that mass fraction is 35% and forms solution C; With continuous stirring, solution A and solution B are slowly added in solution C successively, after stirring 2 hours, add a small amount of agar powder and continue stirring formation gel; After this gel is dried, in chamber type electric resistance furnace, it is warming up to 220 DEG C with the speed less than 3 DEG C per minute, keeps this temperature 4 hours, continue to be warming up to 480 DEG C with the speed less than 3 DEG C per minute, keep this temperature 3 hours, naturally cool to room temperature and obtain by Bi2O3, PbO and In2O3The metal composite oxide of composition; With continuous stirring, this metal composite oxide is added in the hydrazine hydrate aqueous solution that mass fraction is 20%, then aforesaid graphene oxide is also added wherein, it is warming up to 40 DEG C, constant temperature stirs 4 hours, irradiates 3 hours with the xenon lamps of 300 watts, uses deionized water wash 3 times after filtration, it is subsequently placed in 60 DEG C of vacuum drying ovens to dry, namely obtains graphene-supported by Bi2O3, PbO and In2O3The composite powder material of composition.
Analyze: composite powder material is carried out component analysis, records the mass percent respectively 12.1%Bi of each component2O3, 23.5%PbO, 19.2%In2O3And 45.2%C.
Application: using this composite powder material as the catalytic luminescence sensitive material measuring benzene and sulfur dioxide, the range of linearity is benzene 0.2-156mg/m3With sulfur dioxide 0.15-79mg/m3, detection is limited to benzene 0.1mg/m3With sulfur dioxide 0.08mg/m3, other common concurrent does not interfere with.
Embodiment 2
[1] being slowly added to by native graphite in the oleum of 40 DEG C with continuous stirring, constant temperature stirs and is slowly added to after 2 hours and the phosphoric acid of the weight such as native graphite, continues constant temperature and stirs 3 hours, and much filtrate is also washed to neutrality by sucking filtration; Filter cake is added in the potassium permanganate concentrated sulfuric acid solution that mass fraction is 15%, it is warming up to 46 DEG C of also continuous stirring 2 hours, it is slowly added to aqueous hydrogen peroxide solution that mass fraction is 25% to bubble-free, continue constant temperature to stir 1 hour, much filtrate is also washed to neutrality by sucking filtration, obtains graphene oxide;
[2] bismuth acetate is dissolved in the aqueous hydrochloric acid solution that mass fraction is 11% and forms solution A, it is formation solution B in 21% aqueous citric acid solution that plumbi nitras is dissolved in mass fraction, is dissolved in by nitrate trihydrate indium in the isobutanol aqueous solution that mass fraction is 39% and forms solution C; With continuous stirring, solution A and solution B are slowly added in solution C successively, after stirring 2 hours, add a small amount of agar powder and continue stirring formation gel; After this gel is dried, in chamber type electric resistance furnace, it is warming up to 210 DEG C with the speed less than 3 DEG C per minute, keeps this temperature 4 hours, continue to be warming up to 460 DEG C with the speed less than 3 DEG C per minute, keep this temperature 3 hours, naturally cool to room temperature and obtain by Bi2O3, PbO and In2O3The metal composite oxide of composition; With continuous stirring, this metal composite oxide is added in the hydrazine hydrate aqueous solution that mass fraction is 20%, then aforesaid graphene oxide is also added wherein, it is warming up to 40 DEG C, constant temperature stirs 4 hours, irradiates 3 hours with the xenon lamps of 300 watts, uses deionized water wash 3 times after filtration, it is subsequently placed in 60 DEG C of vacuum drying ovens to dry, namely obtains graphene-supported by Bi2O3, PbO and In2O3The composite powder material of composition.
Analyze: composite powder material is carried out component analysis, records the mass percent respectively 18.8%Bi of each component2O3, 16.1%PbO, 14.3%In2O3And 50.8%C.
Application: using this composite powder material as the catalytic luminescence sensitive material measuring benzene and sulfur dioxide, the range of linearity is benzene 0.15-125mg/m3With sulfur dioxide 0.2-87mg/m3, detection is limited to benzene 0.08mg/m3With sulfur dioxide 0.1mg/m3, other common concurrent does not interfere with.
Embodiment 3
[1] being slowly added to by native graphite in the oleum of 40 DEG C with continuous stirring, constant temperature stirs and is slowly added to after 2 hours and the phosphoric acid of the weight such as native graphite, continues constant temperature and stirs 3 hours, and much filtrate is also washed to neutrality by sucking filtration; Filter cake is added in the potassium permanganate concentrated sulfuric acid solution that mass fraction is 15%, it is warming up to 54 DEG C of also continuous stirring 2 hours, it is slowly added to aqueous hydrogen peroxide solution that mass fraction is 25% to bubble-free, continue constant temperature to stir 1 hour, much filtrate is also washed to neutrality by sucking filtration, obtains graphene oxide;
[2] five water bismuth nitrate are dissolved in the aqueous hydrochloric acid solution that mass fraction is 19% and form solution A, it is formation solution B in 24% aqueous citric acid solution that Lead sulfocyanate. is dissolved in mass fraction, is dissolved in by five water indium sulfates in the isobutanol aqueous solution that mass fraction is 31% and forms solution C; With continuous stirring, solution A and solution B are slowly added in solution C successively, after stirring 2 hours, add a small amount of agar powder and continue stirring formation gel; After this gel is dried, in chamber type electric resistance furnace, it is warming up to 230 DEG C with the speed less than 3 DEG C per minute, keeps this temperature 4 hours, continue to be warming up to 470 DEG C with the speed less than 3 DEG C per minute, keep this temperature 3 hours, naturally cool to room temperature and obtain by Bi2O3, PbO and In2O3The metal composite oxide of composition; With continuous stirring, this metal composite oxide is added in the hydrazine hydrate aqueous solution that mass fraction is 20%, then aforesaid graphene oxide is also added wherein, it is warming up to 40 DEG C, constant temperature stirs 4 hours, irradiates 3 hours with the xenon lamps of 300 watts, uses deionized water wash 3 times after filtration, it is subsequently placed in 60 DEG C of vacuum drying ovens to dry, namely obtains graphene-supported by Bi2O3, PbO and In2O3The composite powder material of composition.
Analyze: composite powder material is carried out component analysis, records the mass percent respectively 11.5%Bi of each component2O3, 16.2%PbO, 15.1%In2O3And 57.2%C.
Application: using this composite powder material as the catalytic luminescence sensitive material measuring benzene and sulfur dioxide, the range of linearity is benzene 0.25-142mg/m3With sulfur dioxide 0.2-88mg/m3, detection is limited to benzene 0.15mg/m3With sulfur dioxide 0.1mg/m3, other common concurrent does not interfere with.
Embodiment 4
[1] being slowly added to by native graphite in the oleum of 40 DEG C with continuous stirring, constant temperature stirs and is slowly added to after 2 hours and the phosphoric acid of the weight such as native graphite, continues constant temperature and stirs 3 hours, and much filtrate is also washed to neutrality by sucking filtration; Filter cake is added in the potassium permanganate concentrated sulfuric acid solution that mass fraction is 15%, it is warming up to 52 DEG C of also continuous stirring 2 hours, it is slowly added to aqueous hydrogen peroxide solution that mass fraction is 25% to bubble-free, continue constant temperature to stir 1 hour, much filtrate is also washed to neutrality by sucking filtration, obtains graphene oxide;
[2] being dissolved in by bismuth sulfate in the aqueous hydrochloric acid solution that mass fraction is 14% and form solution A, it is formation solution B in 29% aqueous citric acid solution that plumbi nitras is dissolved in mass fraction, is dissolved in by indium acetate in the isobutanol aqueous solution that mass fraction is 36% and forms solution C; With continuous stirring, solution A and solution B are slowly added in solution C successively, after stirring 2 hours, add a small amount of agar powder and continue stirring formation gel; After this gel is dried, in chamber type electric resistance furnace, it is warming up to 240 DEG C with the speed less than 3 DEG C per minute, keeps this temperature 4 hours, continue to be warming up to 470 DEG C with the speed less than 3 DEG C per minute, keep this temperature 3 hours, naturally cool to room temperature and obtain by Bi2O3, PbO and In2O3The metal composite oxide of composition; With continuous stirring, this metal composite oxide is added in the hydrazine hydrate aqueous solution that mass fraction is 20%, then aforesaid graphene oxide is also added wherein, it is warming up to 40 DEG C, constant temperature stirs 4 hours, irradiates 3 hours with the xenon lamps of 300 watts, uses deionized water wash 3 times after filtration, it is subsequently placed in 60 DEG C of vacuum drying ovens to dry, namely obtains graphene-supported by Bi2O3, PbO and In2O3The composite powder material of composition.
Analyze: composite powder material is carried out component analysis, records the mass percent respectively 13.2%Bi of each component2O3, 15.3%PbO, 23.1%In2O3And 48.4%C.
Application: using this composite powder material as the catalytic luminescence sensitive material measuring benzene and sulfur dioxide, the range of linearity is benzene 0.1-85mg/m3With sulfur dioxide 0.2-84mg/m3, detection is limited to benzene 0.05mg/m3With sulfur dioxide 0.1mg/m3, other common concurrent does not interfere with.
Embodiment 5
[1] being slowly added to by native graphite in the oleum of 40 DEG C with continuous stirring, constant temperature stirs and is slowly added to after 2 hours and the phosphoric acid of the weight such as native graphite, continues constant temperature and stirs 3 hours, and much filtrate is also washed to neutrality by sucking filtration; Filter cake is added in the potassium permanganate concentrated sulfuric acid solution that mass fraction is 15%, it is warming up to 48 DEG C of also continuous stirring 2 hours, it is slowly added to aqueous hydrogen peroxide solution that mass fraction is 25% to bubble-free, continue constant temperature to stir 1 hour, much filtrate is also washed to neutrality by sucking filtration, obtains graphene oxide;
[2] Bismugel (Biothrax). is dissolved in the aqueous hydrochloric acid solution that mass fraction is 17% and forms solution A, it is formation solution B in 25% aqueous citric acid solution that plumbi nitras and lead acetate are dissolved in mass fraction, nitrate trihydrate indium and indium phosphate is dissolved in the isobutanol aqueous solution that mass fraction is 32% and forms solution C; With continuous stirring, solution A and solution B are slowly added in solution C successively, after stirring 2 hours, add a small amount of agar powder and continue stirring formation gel; After this gel is dried, in chamber type electric resistance furnace, it is warming up to 205 DEG C with the speed less than 3 DEG C per minute, keeps this temperature 4 hours, continue to be warming up to 490 DEG C with the speed less than 3 DEG C per minute, keep this temperature 3 hours, naturally cool to room temperature and obtain by Bi2O3, PbO and In2O3The metal composite oxide of composition; With continuous stirring, this metal composite oxide is added in the hydrazine hydrate aqueous solution that mass fraction is 20%, then aforesaid graphene oxide is also added wherein, it is warming up to 40 DEG C, constant temperature stirs 4 hours, irradiates 3 hours with the xenon lamps of 300 watts, uses deionized water wash 3 times after filtration, it is subsequently placed in 60 DEG C of vacuum drying ovens to dry, namely obtains graphene-supported by Bi2O3, PbO and In2O3The composite powder material of composition.
Analyze: composite powder material is carried out component analysis, records the mass percent respectively 12.6%Bi of each component2O3, 24.7%PbO, 16.4%In2O3And 46.3%C.
Application: using this composite powder material as the catalytic luminescence sensitive material measuring benzene and sulfur dioxide, the range of linearity is benzene 0.18-132mg/m3With sulfur dioxide 0.25-118mg/m3, detection is limited to benzene 0.1mg/m3With sulfur dioxide 0.15mg/m3, other common concurrent does not interfere with.
Claims (1)
1. a catalytic luminescence sensitive material for benzene and sulfur dioxide, is characterized in that graphene-supported by Bi2O3, PbO and In2O3The composite of composition, each constituent mass mark is 10-20%Bi2O3, 15-25%PbO, 14-24%In2O3And 45-60%C, its preparation method is:
(1) being slowly added to by native graphite in the oleum of 40 DEG C with continuous stirring, constant temperature stirs and is slowly added to after 2 hours and the phosphoric acid of the weight such as native graphite, continues constant temperature and stirs 3 hours, and much filtrate is also washed to neutrality by sucking filtration; Filter cake is added in the potassium permanganate concentrated sulfuric acid solution that mass fraction is 15%, it is warming up to 45-55 DEG C of also continuous stirring 2 hours, it is slowly added to aqueous hydrogen peroxide solution that mass fraction is 25% to bubble-free, continue constant temperature to stir 1 hour, much filtrate is also washed to neutrality by sucking filtration, obtains graphene oxide;
(2) Oxalic acid bismuth salt. is dissolved in the aqueous hydrochloric acid solution that mass fraction is 10-20% and forms solution A, it is formation solution B in 20-30% aqueous citric acid solution that lead acetate is dissolved in mass fraction, is dissolved in by indium nitrate in the isobutanol aqueous solution that mass fraction is 30-40% and forms solution C; With continuous stirring, solution A and solution B are slowly added in solution C successively, after stirring 2 hours, add a small amount of agar powder and continue stirring formation gel; After this gel is dried, chamber type electric resistance furnace is warming up to 200-250 DEG C with the speed less than 3 DEG C per minute, keeps this temperature 4 hours, continue to be warming up to 450-500 DEG C with the speed less than 3 DEG C per minute, keep this temperature 3 hours, naturally cool to room temperature and obtain by Bi2O3, PbO and In2O3The metal composite oxide of composition; With continuous stirring, this metal composite oxide is added in the hydrazine hydrate aqueous solution that mass fraction is 20%, then aforesaid graphene oxide is also added wherein, it is warming up to 40 DEG C, constant temperature stirs 4 hours, irradiates 3 hours with the xenon lamps of 300 watts, uses deionized water wash 3 times after filtration, it is subsequently placed in 60 DEG C of vacuum drying ovens to dry, namely obtains graphene-supported by Bi2O3, PbO and In2O3The composite of composition.
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| CN109490374A (en) * | 2018-11-30 | 2019-03-19 | 北京联合大学 | The cross sensitivity material of formaldehyde in air, benzene, ammonia and carbon monoxide |
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| CN109490372A (en) * | 2018-11-30 | 2019-03-19 | 北京联合大学 | A kind of catalytic luminescence sensitive material of ethyl alcohol |
| CN109490374B (en) * | 2018-11-30 | 2020-11-13 | 北京联合大学 | Cross sensitive material for formaldehyde, benzene, ammonia and carbon monoxide in air |
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