CN108802017A - The low-temperature catalyzed luminous sensitive material of benzene - Google Patents
The low-temperature catalyzed luminous sensitive material of benzene Download PDFInfo
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- CN108802017A CN108802017A CN201810893745.3A CN201810893745A CN108802017A CN 108802017 A CN108802017 A CN 108802017A CN 201810893745 A CN201810893745 A CN 201810893745A CN 108802017 A CN108802017 A CN 108802017A
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Abstract
A kind of low-temperature catalyzed luminous sensitive material of benzene, it is characterized in that by MoO atom doped Pt3、WO3And Al2O3The composite powder material of composition, the wherein mass percent of each component ranging from 1.6-2.2%Pt, 26-30%MoO3, 36-42%WO3And 27-31%Al2O3, preparation method is:Tungsten salt is dissolved in aqueous hydrochloric acid solution, aluminium salt is dissolved in aqueous citric acid solution, agar powder is added after the two mixing, then ammonium molybdate crystal is dissolved in into this solution, then glucose and chloroplatinic acid is added, flows back, it is cooling, gel is formed, by the drying of this gel, roasting, natural cooling obtains sensitive material.The gas sensor made using sensitive material provided by the present invention, can be in the micro-benzene in the measurement air quick at use temperature no more than 200 DEG C without being interfered by other common concurrents.
Description
Technical field
The present invention relates to a kind of low-temperature catalyzed luminous sensitive material of benzene, especially pt atom doping by MoO3、WO3With
Al2O3The composite powder material of composition, belongs to field of sensing technologies.
Background technology
Benzene is a kind of industrial chemicals with aromatic odor, and yield and production technology level are a national oil chemical industry
One of mark of development level.At normal temperatures, benzene is a kind of colourless, pleasantly sweet transparency liquid, and density is less than water, is had strong
Strong aromatic odor.The boiling point of benzene is 80.1 DEG C, and fusing point is 5.5 DEG C;Benzene is a kind of good organic solvent, dissolves organic molecule
It is very capable with some nonpolar inorganic molecules, glycerine is removed, the polyalcohols such as ethylene glycol external enwergy is mixed with most of organic solvents
It is molten.Benzene in air is mainly derived from building coating, paint for decoration, adhesive solvent and vehicle exhaust etc..Benzene is mainly by exhaling
It inhales the mode that road sucking (47-80%), stomach and intestine and skin absorb and enters human body.A part of benzene can be discharged by urine, be not discharged
Benzene epoxy benzene (7- oxabicyclos are then oxidized to by oxygen molecule under cytochrome P 450 monooxygenases effect first in liver
[4.1.0] hept- 2,4- diene).Epoxy benzene exists with its rearrangement product oxepin to be balanced, and is produced in benzene metabolic process
Raw toxic intermediate.After the metabolin of benzene enters cell, is combined with the DNA (DNA) in nucleus, dye can be made
Colour solid changes, and some is broken the combination having, and here it is cancerations, for a long time in this way, will cause cancer.Due to everyone be good for
Health situation and contact conditions difference, also differ the sensitivity of benzene.When can smell the smell of benzene in air, its concentration
Probably it is 1.5ppm, at this moment just it should be noted that the danger of poisoning.When checking, can be easy to by the inspection of urine and blood
Find the degree of intoxication of benzene.Benzene energy Central nervous system generates paralysis effect, causes acute poisoning.Severe one will appear headache,
Nausea and vomiting, in a certain state of delirium, unconsciousness, stupor, twitch etc., severe patient can be dead because of cental system paralysis.A small amount of benzene
Also can make one generate sleepiness, giddy, increased heart rate, have a headache, tremble, Bewu βtseinstrubung, obnubilation phenomena such as.Intake is excessive containing benzene
Food can lead to the symptoms such as vomiting, stomachache, giddy, insomnia, twitch, increased heart rate, or even it is dead.Suck the benzene of 20000ppm
Steam has fatal risk in 5-10 minutes.Long Term Contact benzene can cause great damage to blood, cause slow poisoning, moreover it is possible to cause
Neurasthenia syndrome.Benzene can damage marrow, and red blood cell, leucocyte, platelet counts is made to reduce, and make chromosome aberration,
So as to cause leukaemia, or even there is alpastic anemia.Benzene can cause to bleed profusely, to inhibit the work(of immune system
With making disease have an opportunity to take advantage of.There is research report to point out, incubation period of the benzene in human body is 12-15.Ben Shiyibei is international
The carcinogen that Cancer Research Center (IARC) confirms, is the major pollutants of room air.
The conventional detection means of benzene mainly have:Spectrophotometry, gas chromatography, liquid chromatography and electrochemical process etc..
Since these methods are required for preconcentration, desorption and proper treatment that could complete to measure by analytical instrument, time-consuming
It is not easy live realization.The on-site measurement method of benzene mainly has detection pipe colorimetric method, and this method stability and sensitivity are all insufficient,
It can not complete the Accurate Determining of micro-benzene.2006, our seminar delivered entitled " nano combined material on assay office
The research paper of benzene homologues in material catalytic luminescence method measurement air ", it has been found that copper ferromanganese composite nano materials have very benzene
High catalytic luminescence activity, still, the temperature in use of this sensitive material is 320 DEG C, is minimized using this sensitive material
When design, compared with operation at high temperature stability contorting at problem, and compared with intense radiant heat background signal noise caused by high temperature fluctuations
(especially long wavelength region) has seriously affected the sensitivity of sensor.
Invention content
The purpose of the present invention is overcoming the shortcomings of conventional art, provide a kind of having greater catalytic hair to benzene at a lower temperature
The sensitive material of photolytic activity and selectivity.The gas sensor made of this sensitive material, can more delicately survey at the scene
The micro-benzene in air is determined without being interfered by concurrent.
Sensitive material of the present invention is Pt atom doped by MoO3、WO3And Al2O3The composite powder material of composition,
Preparation method is as follows:Tungsten salt is dissolved in the aqueous hydrochloric acid solution that mass fraction is 12-15% and forms solution A, aluminium salt is dissolved in
Mass fraction is to form solution B in 15-18% aqueous citric acid solutions, with continuous stirring, solution B is slowly dropped to solution A
In, agar powder is added, is warming up to 95 DEG C and is continuously stirring to solution clarification, ammonium molybdate crystal is directly added into this solution & stir extremely
Be completely dissolved, glucose and chloroplatinic acid be then added, flows back 3-5 hours at a temperature of 100-110 DEG C, be cooled to room temperature to be formed it is solidifying
Glue is warming up to 180-200 DEG C with the speed per minute for being no more than 2 DEG C in chamber type electric resistance furnace, keeps this after drying this gel
Temperature 3-5 hours continues to be warming up to 300-350 DEG C with the speed per minute for being no more than 2 DEG C, keeps this temperature 2-3 hours, natural
It is cooled to room temperature to obtain Pt atom doped by MoO3、WO3And Al2O3The composite powder material of composition.
Wherein, tungsten salt be the anhydride of ammonium tungstate, ammonium paratungstate, ammonium metatungstate and tungsten hexachloride or one kind of hydrate or
Several mixtures, aluminium salt be aluminum nitrate, aluminum sulfate, aluminum perchlorate, aluminium chloride and aluminum acetate anhydride or hydrate one
Kind or several mixtures.
Composite powder material each component mass fraction obtained meets Pt (1.6-2.2), MoO3(26-30%), WO3(36-
And Al 42%)2O3When (27-31%) and grain size are 15-40 nanometers, it is used as the catalytic luminescence sensitive material of benzene in air,
It just has very high catalytic luminescence activity at 200 DEG C or less.
Specific implementation mode
Embodiment 1
Ammonium tungstate is dissolved in the aqueous hydrochloric acid solution that mass fraction is 14% and forms solution A, nine water aluminum nitrates are dissolved in matter
Amount score is to form solution B in 16% aqueous citric acid solution, and with continuous stirring, solution B is slowly dropped in solution A, is added
Enter agar powder, is warming up to 95 DEG C and is continuously stirring to solution clarification, ammonium molybdate crystal is directly added into this solution & stir to complete
Then dissolving is added glucose and chloroplatinic acid, flows back 4 hours at a temperature of 105 DEG C, be cooled to room temperature to form gel, this is coagulated
After glue drying, 185 DEG C are warming up to the speed per minute for being no more than 2 DEG C in chamber type electric resistance furnace, keeps this temperature 5 hours, after
It is continuous to be warming up to 310 DEG C with the speed per minute for being no more than 2 DEG C, keep this temperature 3 hours, cooled to room temperature obtains Pt atoms
Doping is by MoO3、WO3And Al2O3The composite powder material of composition.
Analysis:Constituent analysis is carried out to composite powder material, it is 1.7%Pt, 26.6%MoO to measure mass percent3、
39.9%WO3And 31.8%Al2O3;It is 20-35nm that transmission electron microscope, which measures particle diameter distribution,.
Using:Using this powder body material as the catalytic luminescence sensitive material of detection benzene in air, operating temperature is 186 DEG C,
The range of linearity is 0.8-55mg/m3, detect and be limited to formaldehyde 0.4mg/m3, common concurrent do not interfere with.
Embodiment 2
Ammonium paratungstate is dissolved in the aqueous hydrochloric acid solution that mass fraction is 13% and forms solution A, aluminum sulfate octadecahydrate is molten
It is to form solution B in 17% aqueous citric acid solution in mass fraction, with continuous stirring, solution B is slowly dropped to solution A
In, agar powder is added, is warming up to 95 DEG C and is continuously stirring to solution clarification, ammonium molybdate crystal is directly added into this solution & stir extremely
It is completely dissolved, glucose and chloroplatinic acid is then added, flows back 3 hours at a temperature of 108 DEG C, is cooled to room temperature to form gel, it will
After the drying of this gel, 190 DEG C are warming up to the speed per minute for being no more than 2 DEG C in chamber type electric resistance furnace, keeps this temperature 4 small
When, continue to be warming up to 320 DEG C with the speed per minute for being no more than 2 DEG C, keeps this temperature 2 hours, cooled to room temperature obtains
Pt is atom doped by MoO3、WO3And Al2O3The composite powder material of composition.
Analysis:Constituent analysis is carried out to composite powder material, it is 1.9%Pt, 27.7%MoO to measure mass percent3、
41.8%WO3And 28.6%Al2O3;It is 15-35nm that transmission electron microscope, which measures particle diameter distribution,.
Using:Using this powder body material as the catalytic luminescence sensitive material of detection benzene in air, operating temperature is 181 DEG C,
The range of linearity is 0.9-58mg/m3, detect and be limited to formaldehyde 0.4mg/m3, common concurrent do not interfere with.
Embodiment 3
Ammonium metatungstate and tungsten hexachloride are dissolved in the aqueous hydrochloric acid solution that mass fraction is 15% and form solution A, Jiang Jiushui
It is to form solution B in 15% aqueous citric acid solution that aluminum perchlorate and aluminum acetate, which are dissolved in mass fraction, with continuous stirring, by solution
B is slowly dropped in solution A, and agar powder is added, and is warming up to 95 DEG C and is continuously stirring to solution clarification, ammonium molybdate crystal is directly added
Enter this solution & stir to being completely dissolved, glucose and chloroplatinic acid is then added, flows back 3 hours, is cooled at a temperature of 109 DEG C
Gel formed at room temperature is warming up to 195 DEG C in chamber type electric resistance furnace after drying this gel with the speed per minute for being no more than 2 DEG C,
It keeps this temperature 3 hours, continues to be warming up to 340 DEG C with the speed per minute for being no more than 2 DEG C, keep this temperature 2 hours, it is naturally cold
But it is atom doped by MoO to obtain Pt to room temperature3、WO3And Al2O3The composite powder material of composition.
Analysis:Constituent analysis is carried out to composite powder material, it is 2.1%Pt, 26.5%MoO to measure mass percent3、
41.0%WO3And 30.4%Al2O3;It is 20-35nm that transmission electron microscope, which measures particle diameter distribution,.
Using:Using this powder body material as the catalytic luminescence sensitive material of detection benzene in air, operating temperature is 178 DEG C,
The range of linearity is 1.0-59mg/m3, detect and be limited to formaldehyde 0.5mg/m3, common concurrent do not interfere with.
Embodiment 4
Tungsten hexachloride will be hydrated and be dissolved in mass fraction to form solution A in 12% aqueous hydrochloric acid solution, by Aluminum Chloride Hexahydrate
It is to form solution B in 18% aqueous citric acid solution to be dissolved in mass fraction with acetate dihydrate aluminium, and with continuous stirring, solution B is delayed
Slowly it is added drop-wise in solution A, agar powder is added, be warming up to 95 DEG C and be continuously stirring to solution clarification, ammonium molybdate crystal is directly added into
Then this solution & stir is added glucose and chloroplatinic acid, flows back 5 hours at a temperature of 104 DEG C, be cooled to room to being completely dissolved
Temperature forms gel, and after this gel is dried, 198 DEG C are warming up to the speed per minute for being no more than 2 DEG C in chamber type electric resistance furnace, is protected
It holds this temperature 3 hours, continues to be warming up to 345 DEG C with the speed per minute for being no more than 2 DEG C, keep this temperature 2 hours, natural cooling
It is atom doped by MoO that Pt is obtained to room temperature3、WO3And Al2O3The composite powder material of composition.
Analysis:Constituent analysis is carried out to composite powder material, it is 2.2%Pt, 27.6%MoO to measure mass percent3、
40.7%WO3And 29.5%Al2O3;It is 18-35nm that transmission electron microscope, which measures particle diameter distribution,.
Using:Using this powder body material as the catalytic luminescence sensitive material of detection benzene in air, operating temperature is 196 DEG C,
The range of linearity is 0.8-65mg/m3, detect and be limited to formaldehyde 0.4mg/m3, common concurrent do not interfere with.
Embodiment 5
Ammonium tungstate and hydration tungsten hexachloride are dissolved in the aqueous hydrochloric acid solution that mass fraction is 14% and form solution A, by vinegar
It is to form solution B in 17% aqueous citric acid solution that sour aluminium, which is dissolved in mass fraction, and with continuous stirring, solution B is slowly dropped to
In solution A, agar powder is added, is warming up to 95 DEG C and is continuously stirring to solution clarification, ammonium molybdate crystal is directly added into this solution simultaneously
Then stirring is added glucose and chloroplatinic acid, flows back 5 hours at a temperature of 102 DEG C to being completely dissolved, be cooled to room temperature to be formed it is solidifying
Glue is warming up to 182 DEG C with the speed per minute for being no more than 2 DEG C in chamber type electric resistance furnace, keeps this temperature after drying this gel
5 hours, continues to be warming up to 305 DEG C with the speed per minute for being no more than 2 DEG C, keep this temperature 3 hours, cooled to room temperature obtains
It is atom doped by MoO to Pt3、WO3And Al2O3The composite powder material of composition.
Analysis:Constituent analysis is carried out to composite powder material, it is 1.6%Pt, 28.3%MoO to measure mass percent3、
39.5%WO3And 30.6%Al2O3;It is 15-28nm that transmission electron microscope, which measures particle diameter distribution,.
Using:Using this powder body material as the catalytic luminescence sensitive material of detection benzene in air, operating temperature is 180 DEG C,
The range of linearity is 0.8-71mg/m3, detect and be limited to formaldehyde 0.4mg/m3, common concurrent do not interfere with.
Claims (2)
1. the low-temperature catalyzed luminous sensitive material of benzene, it is characterized in that by MoO atom doped Pt3、WO3And Al2O3What is formed is compound
Powder body material, the wherein mass percent of each component ranging from 1.6-2.2%Pt, 26-30%MoO3, 36-42%WO3And 27-
31%Al2O3, preparation method is:Tungsten salt is dissolved in the aqueous hydrochloric acid solution that mass fraction is 12-15% and forms solution A, by aluminium
It is to form solution B in 15-18% aqueous citric acid solutions that salt, which is dissolved in mass fraction, and with continuous stirring, solution B is slowly dropped to
In solution A, agar powder is added, is warming up to 95 DEG C and is continuously stirring to solution clarification, ammonium molybdate crystal is directly added into this solution simultaneously
Then stirring is added glucose and chloroplatinic acid, flows back 3-5 hours, be cooled to room temperature at a temperature of 100-110 DEG C to being completely dissolved
Gel is formed, after this gel is dried, 180-200 DEG C is warming up to the speed per minute for being no more than 2 DEG C in chamber type electric resistance furnace,
It keeps this temperature 3-5 hours, continues to be warming up to 300-350 DEG C with the speed per minute for being no more than 2 DEG C, keep this temperature 2-3 small
When, it is atom doped by MoO that cooled to room temperature obtains Pt3、WO3And Al2O3The composite powder material of composition.
2. the low-temperature catalyzed luminous sensitive material of benzene according to claim 1, it is characterized in that the tungsten salt be ammonium tungstate,
One or more of mixtures of ammonium paratungstate, the anhydride of ammonium metatungstate and tungsten hexachloride or hydrate, aluminium salt be aluminum nitrate,
Aluminum sulfate, aluminum perchlorate, aluminium chloride and the anhydride of aluminum acetate or one or more of mixtures of hydrate.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109490375A (en) * | 2018-11-30 | 2019-03-19 | 北京联合大学 | The low-temperature sensitive material of formaldehyde and benzene |
CN110658186A (en) * | 2019-10-22 | 2020-01-07 | 北京联合大学 | Sensitive material for simultaneously measuring formaldehyde, benzene and carbon monoxide |
Citations (1)
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CN102600842A (en) * | 2012-03-02 | 2012-07-25 | 山西盛驰科技有限公司 | Catalyst for preparing ethanol through hydrogenation of acetic acid as well as preparation method and application thereof |
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CN102600842A (en) * | 2012-03-02 | 2012-07-25 | 山西盛驰科技有限公司 | Catalyst for preparing ethanol through hydrogenation of acetic acid as well as preparation method and application thereof |
Non-Patent Citations (2)
Title |
---|
JAZAER DAWODY等: "《The effect of metal oxide additives (WO3, MoO3, V2O5, Ga2O3) on the oxidation of NO and SO2 over Pt/Al2O3 and Pt/BaO/Al2O3 catalysts》", 《JOURNAL OF MOLECULAR CATALYSIS A:CHEMICAL》 * |
徐潇潇: "《Pt基催化剂用于NO催化还原性能研究》", 《浙江工业大学硕士学位论文》 * |
Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109490375A (en) * | 2018-11-30 | 2019-03-19 | 北京联合大学 | The low-temperature sensitive material of formaldehyde and benzene |
CN110658186A (en) * | 2019-10-22 | 2020-01-07 | 北京联合大学 | Sensitive material for simultaneously measuring formaldehyde, benzene and carbon monoxide |
CN110658186B (en) * | 2019-10-22 | 2021-08-13 | 北京联合大学 | Sensitive material for simultaneously measuring formaldehyde, benzene and carbon monoxide |
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