CN108802016B - A kind of high selection measures the sensitive material of trace formaldehyde in air - Google Patents
A kind of high selection measures the sensitive material of trace formaldehyde in air Download PDFInfo
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- CN108802016B CN108802016B CN201810893743.4A CN201810893743A CN108802016B CN 108802016 B CN108802016 B CN 108802016B CN 201810893743 A CN201810893743 A CN 201810893743A CN 108802016 B CN108802016 B CN 108802016B
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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 present invention relates to the sensitive materials of trace formaldehyde in a kind of high selection measurement air, it is characterized in that by graphene-supported MgO, ZrO2And Cr2O3The composite powder material of composition, partial size are no more than 45nm, and wherein the mass percent range of each component is 8-12%MgO, 5-8%ZrO2, 7-13%Cr2O3And 70-80%C.Preparation method is: converting graphene oxide for natural graphite first, secondly prepares nanoscale magnesium zirconium chromic composite metal oxide using magnesium salts, zirconates and chromic salts, metal composite oxide is finally loaded during graphene oxide is reduced to graphene.The gas sensor made using sensitive material provided by the present invention, can at the scene the trace formaldehyde in Accurate Determining air without the interference by other common concurrents.
Description
Technical field
The present invention relates to a kind of high selection measurement air in trace formaldehyde sensitive material, it is especially graphene-supported by
MgO、ZrO2And Cr2O3The composite powder material of composition, belongs to field of sensing technologies.
Background technique
Formaldehyde is a kind of colourless volatile industrial chemicals, as adhesive raw materials, disinfectant, preservative and finishing agent quilt
It is widely used in the products such as compression plate, coating, paint, cosmetics and packaging material.First of the people to concentration various in air
Aldehyde has different reflections, when concentration of formaldehyde reaches 0.06~0.07mg/m in air3When, children will occur slightly to pant,
Reach 0.1mg/m3When just have peculiar smell and sense of discomfort, reach 0.5mg/m3When eyes can be stimulated to cause to shed tears, reach 0.6mg/m3It can
Cause throat discomfort or pain, reaches 1mg/m3When can cause largely to shed tears, reach 10mg/m3When then feel to have difficulty in breathing, reach
30mg/m3When can make one to suffocate.Long Term Contact low dosage formaldehyde (0.1mg/m3It can cause chronic respiratory disease, female below)
Property pregnancy syndrome, newborn's constitution reduces and the lesions such as chromosome abnormality.
Formaldehyde is confirmed as carcinogen by International Cancer Research Center (IARC), is the main pollution in room air
Object.Animal experiments show that formaldehyde can increase Micronucleus and rate of teratosperm, cause pregnant mouse abortion ratio rise and
Litter size decline, damage mouse spleen and lungs.Studies have reported that the formaldehyde of low concentration can induce leukaemia, since we give birth to
Living and work Formaldehyde in Environment is ubiquitous, therefore the method for studying trace formaldehyde in rapid and accurate determination air has very by force
Realistic meaning.
Measurement trace formaldehyde method mainly have photometry, electrochemical process, chromatography, chemoluminescence method, gas chromatography mass spectrometry method,
Liquid Chromatography/Mass Spectrometry and the chromatography of ions etc. could pass through analysis instrument since these methods require preconcentration and proper treatment
Measurement is completed, therefore time-consuming is not easy live realization.Inventor is in 2006 in Sensors & Actuators:
Entitled " On-line Monitoring of Formaldehyde in Air by has been delivered on B.Chemical
Nanoscale vanadium titanium (atomic ratio 1: 2) combined oxidation is used in the paper of Cataluminescence-based gas Sensor "
Object, can be with 0.1~40mg/m of on-line checking as sensitive material3Formaldehyde, detection limit is up to 0.06mg/m3, but acetaldehyde and first
Alcohol has interference；Delivered on " chemical journal " in 2008 it is entitled " nano composite oxide catalytic luminescence method measure air in
Formaldehyde " paper in use improved nanoscale molybdenum vanadium titanium (atomic ratio 2: 3: 5) composite oxides, can as sensitive material
With 0.07~34mg/m of on-line checking3Formaldehyde, detection limit is up to 0.04mg/m3, but acetaldehyde still has certain interference.
Summary of the invention
The purpose of the present invention is overcoming the shortcomings of conventional art, a kind of the quick of trace formaldehyde in high selection measurement air is provided
Feel material and preparation method thereof.It, can be quick at the scene, quasi- with the gas sensor for the monitoring formaldehyde that this sensitive material makes
Really the trace formaldehyde in measurement air is without the interference by other concurrents.
Sensitive material of the present invention is graphene-supported by MgO, ZrO2And Cr2O3The composite powder material of composition,
Preparation method is as follows:
(1) natural graphite is slowly added in oleum with continuous stirring, after being warming up to 45 DEG C and stirring 2-3 hours
It is slowly added to the oxalic acid with weight such as natural graphites, continues that temperature is kept to stir 1 hour, filters and be washed to much filtrate
Property；Filter cake is added in the potassium permanganate concentrated sulfuric acid solution that mass fraction is 15%, is warming up to 50-55 DEG C and to continuously stir 2 small
When, until being slowly added to the aqueous hydrogen peroxide solution to bubble-free that mass fraction is 25%, continues constant temperature and stir 1 hour, filter
And much filtrate is washed to neutrality, obtain graphene oxide；
(2) magnesium salts and zirconates are dissolved in the aqueous hydrochloric acid solution that mass fraction is 15-20% and form solution A, chromic salts is molten
It is to form solution B in 20-30% aqueous citric acid solution in mass fraction, with continuous stirring, solution A is slowly added to solution B
In, agar powder is added after stirring 2 hours, after being warming up to 92-95 DEG C and stirs to being completely dissolved, is cooled to room temperature to form gel, it will
After the drying of this gel, it is warming up to 200-250 DEG C with the speed for being no more than 3 DEG C per minute in chamber type electric resistance furnace, keeps this temperature 4
Hour, continue to be warming up to 400-450 DEG C with the speed for being no more than 3 DEG C per minute, keeps this temperature 3 hours, naturally cool to room
Temperature is obtained by MgO, ZrO2And Cr2O3The metal composite oxide of composition；
(3) with continuous stirring, the hydrazine hydrate aqueous solution that mass fraction is 15-20% is added in this metal composite oxide
In, then graphene oxide above-mentioned is also added thereto, is warming up to 45 DEG C, constant temperature stirs 4-5 hours, and natural cooling simultaneously filters
After be washed with deionized 3 times, be subsequently placed in 65 DEG C of vacuum drying oven drying to get to graphene-supported by MgO, ZrO2With
Cr2O3The composite powder material of composition.
Wherein, magnesium salts is anhydride or the hydration of magnesium chloride, magnesium sulfate, magnesium nitrate, magnesium oxalate, magnesium citrate and magnesium acetate
One or more of mixtures of object, zirconates is the nothing of basic zirconium chloride, acetic acid zirconium, zirconium sulfate, zirconium chloride and nitric acid oxidation zirconium
One or more of mixtures of water object or hydrate, chromic salts be chromium chloride, perchloric acid chromium, chromic acetate, chromium+oxalic acid, chromic nitrate and
The anhydride of chromium sulfate or one or more of mixtures of hydrate.
Each component mass fraction meets MgO (8-12%), ZrO in composite powder material obtained2(5-8%), Cr2O3(7-
13%) when and C (70-80%), and maximum particle diameter is no more than 45nm, it is used as the sensitive material of trace formaldehyde in measurement air
Material.
Specific embodiment
Embodiment 1
(1) natural graphite is slowly added in oleum with continuous stirring, is warming up to 45 DEG C and delayed after stirring 2 hours
The slow oxalic acid being added with weight such as natural graphites continues that temperature is kept to stir 1 hour, filters and much filtrate is washed to neutrality；
Filter cake is added in the potassium permanganate concentrated sulfuric acid solution that mass fraction is 15%, is warming up to 51 DEG C and continuously stirs 2 hours, slowly
Until the aqueous hydrogen peroxide solution to bubble-free that mass fraction is 25% is added, continues constant temperature and stir 1 hour, filter and will filter out
Object is washed to neutrality, obtains graphene oxide；
(2) magnesium chloride hexahydrate and zirconium oxychloride octahydrate are dissolved in the aqueous hydrochloric acid solution that mass fraction is 15% and form solution
A, it is to form solution B in 21% aqueous citric acid solution that chromium chloride hexahydrate, which is dissolved in mass fraction, with continuous stirring, by solution A
It is slowly added in solution B, agar powder is added after stirring 2 hours, after being warming up to 92 DEG C and stirs to being completely dissolved, is cooled to room temperature shape
205 DEG C are warming up to the speed for being no more than 3 DEG C per minute in chamber type electric resistance furnace, keeps this after the drying of this gel at gel
Temperature 4 hours, continues to be warming up to 410 DEG C with the speed for being no more than 3 DEG C per minute, keep this temperature 3 hours, naturally cool to room
Temperature is obtained by MgO, ZrO2And Cr2O3The metal composite oxide of composition；
(3) with continuous stirring, this metal composite oxide is added in the hydrazine hydrate aqueous solution that mass fraction is 17%,
Then graphene oxide above-mentioned is also added thereto, is warming up to 45 DEG C, constant temperature stirs 4 hours, uses after natural cooling and filtering
Deionized water is washed 3 times, and it is graphene-supported by MgO, ZrO to get arriving to be subsequently placed in 65 DEG C of vacuum drying oven drying2And Cr2O3
The composite powder material of composition.
Analysis: this composite powder material is tested with transmission electron microscope, maximum particle diameter is no more than 43nm, average grain diameter
About 32nm；Constituent analysis is carried out to it, measuring each component mass percent is respectively 11.2%MgO, 7.4%ZrO2、
11.1%Cr2O3And 70.3%C.
Using: the formaldehyde in air, range of linearity 0.03- are detected using this composite granule as catalytic luminescence sensitive material
15mg/m3, detect and be limited to 0.01mg/m3, other common concurrents do not interfere with.
Embodiment 2
(1) natural graphite is slowly added in oleum with continuous stirring, is warming up to 45 DEG C and delayed after stirring 3 hours
The slow oxalic acid being added with weight such as natural graphites continues that temperature is kept to stir 1 hour, filters and much filtrate is washed to neutrality；
Filter cake is added in the potassium permanganate concentrated sulfuric acid solution that mass fraction is 15%, is warming up to 54 DEG C and continuously stirs 2 hours, slowly
Until the aqueous hydrogen peroxide solution to bubble-free that mass fraction is 25% is added, continues constant temperature and stir 1 hour, filter and will filter out
Object is washed to neutrality, obtains graphene oxide；
(2) by epsom salt, magnesium acetate and acetic acid zirconium be dissolved in mass fraction be 18% aqueous hydrochloric acid solution in formed it is molten
Liquid A, it is to form solution B in 23% aqueous citric acid solution that perchlorate hexahydrate's chromium and chromium sulfate, which are dissolved in mass fraction, is continuously being stirred
It mixes down, solution A is slowly added in solution B, agar powder is added after stirring 2 hours, after being warming up to 93 DEG C and stirs to being completely dissolved,
It is cooled to room temperature to form gel, after the drying of this gel, be warming up in chamber type electric resistance furnace with the speed for being no more than 3 DEG C per minute
It 220 DEG C, keeps this temperature 4 hours, continues to be warming up to 415 DEG C with the speed for being no more than 3 DEG C per minute, keep this temperature 3 hours,
Cooled to room temperature is obtained by MgO, ZrO2And Cr2O3The metal composite oxide of composition；
(3) with continuous stirring, this metal composite oxide is added in the hydrazine hydrate aqueous solution that mass fraction is 18%,
Then graphene oxide above-mentioned is also added thereto, is warming up to 45 DEG C, constant temperature stirs 5 hours, uses after natural cooling and filtering
Deionized water is washed 3 times, and it is graphene-supported by MgO, ZrO to get arriving to be subsequently placed in 65 DEG C of vacuum drying oven drying2And Cr2O3
The composite powder material of composition.
Analysis: this composite powder material is tested with transmission electron microscope, maximum particle diameter is no more than 40nm, average grain diameter
About 30nm；Constituent analysis is carried out to it, measuring each component mass percent is respectively 9.8%MgO, 6.3%ZrO2, 12.4%
Cr2O3And 71.5%C.
Using: the formaldehyde in air, range of linearity 0.05- are detected using this composite granule as catalytic luminescence sensitive material
17mg/m3, detect and be limited to 0.02mg/m3, other common concurrents do not interfere with.
Embodiment 3
(1) natural graphite is slowly added in oleum with continuous stirring, is warming up to 45 DEG C and delayed after stirring 2 hours
The slow oxalic acid being added with weight such as natural graphites continues that temperature is kept to stir 1 hour, filters and much filtrate is washed to neutrality；
Filter cake is added in the potassium permanganate concentrated sulfuric acid solution that mass fraction is 15%, is warming up to 52 DEG C and continuously stirs 2 hours, slowly
Until the aqueous hydrogen peroxide solution to bubble-free that mass fraction is 25% is added, continues constant temperature and stir 1 hour, filter and will filter out
Object is washed to neutrality, obtains graphene oxide；
(2) magnesium nitrate hexahydrate and tetrahydrated zirconium sulfate are dissolved in the aqueous hydrochloric acid solution that mass fraction is 19% and form solution A,
It is to form solution B in 25% aqueous citric acid solution that six water acetic acid chromium and chromium sulfate, which are dissolved in mass fraction, with continuous stirring, will
Solution A is slowly added in solution B, and agar powder is added after stirring 2 hours, after being warming up to 95 DEG C and stirs to being completely dissolved, is cooled to
Gel formed at room temperature is warming up to 240 DEG C in chamber type electric resistance furnace after the drying of this gel with the speed for being no more than 3 DEG C per minute,
It keeps this temperature 4 hours, continues to be warming up to 425 DEG C with the speed for being no more than 3 DEG C per minute, keep this temperature 3 hours, it is naturally cold
But it obtains to room temperature by MgO, ZrO2And Cr2O3The metal composite oxide of composition；
(3) with continuous stirring, this metal composite oxide is added in the hydrazine hydrate aqueous solution that mass fraction is 16%,
Then graphene oxide above-mentioned is also added thereto, is warming up to 45 DEG C, constant temperature stirs 4 hours, uses after natural cooling and filtering
Deionized water is washed 3 times, and it is graphene-supported by MgO, ZrO to get arriving to be subsequently placed in 65 DEG C of vacuum drying oven drying2And Cr2O3
The composite powder material of composition.
Analysis: this composite powder material is tested with transmission electron microscope, maximum particle diameter is no more than 45nm, average grain diameter
About 32nm；Constituent analysis is carried out to it, measuring each component mass percent is respectively 8.1%MgO, 5.7%ZrO2, 9.4%
Cr2O3And 76.8%C.
Using: the formaldehyde in air, range of linearity 0.03- are detected using this composite granule as catalytic luminescence sensitive material
15mg/m3, detect and be limited to 0.01mg/m3, other common concurrents do not interfere with.
Embodiment 4
(1) natural graphite is slowly added in oleum with continuous stirring, is warming up to 45 DEG C and delayed after stirring 3 hours
The slow oxalic acid being added with weight such as natural graphites continues that temperature is kept to stir 1 hour, filters and much filtrate is washed to neutrality；
Filter cake is added in the potassium permanganate concentrated sulfuric acid solution that mass fraction is 15%, is warming up to 53 DEG C and continuously stirs 2 hours, slowly
Until the aqueous hydrogen peroxide solution to bubble-free that mass fraction is 25% is added, continues constant temperature and stir 1 hour, filter and will filter out
Object is washed to neutrality, obtains graphene oxide；
(2) oxalic acid dihydrate magnesium and zirconium chloride are dissolved in the aqueous hydrochloric acid solution that mass fraction is 17% and form solution A, it will
It is to form solution B in 27% aqueous citric acid solution that chromium+oxalic acid, which is dissolved in mass fraction, and with continuous stirring, solution A is slowly added to
In solution B, agar powder is added after stirring 2 hours, after being warming up to 94 DEG C and stirs to being completely dissolved, is cooled to room temperature to form gel,
After the drying of this gel, 230 DEG C are warming up to the speed for being no more than 3 DEG C per minute in chamber type electric resistance furnace, keeps this temperature 4 small
When, continue to be warming up to 435 DEG C with the speed for being no more than 3 DEG C per minute, keeps this temperature 3 hours, cooled to room temperature obtains
By MgO, ZrO2And Cr2O3The metal composite oxide of composition:
(3) with continuous stirring, this metal composite oxide is added in the hydrazine hydrate aqueous solution that mass fraction is 19%,
Then graphene oxide above-mentioned is also added thereto, is warming up to 45 DEG C, constant temperature stirs 5 hours, uses after natural cooling and filtering
Deionized water is washed 3 times, and it is graphene-supported by MgO, ZrO to get arriving to be subsequently placed in 65 DEG C of vacuum drying oven drying2And Cr2O3
The composite powder material of composition.
Analysis: this composite powder material is tested with transmission electron microscope, maximum particle diameter is no more than 40nm, average grain diameter
About 30nm；Constituent analysis is carried out to it, measuring each component mass percent is respectively 8.9%MgO, 6.0%ZrO2, 7.3%
Cr2O3And 77.8%C.
Using: the formaldehyde in air, range of linearity 0.02- are detected using this composite granule as catalytic luminescence sensitive material
15mg/m3, detect and be limited to 0.01mg/m3, other common concurrents do not interfere with.
Embodiment 5
(1) natural graphite is slowly added in oleum with continuous stirring, is warming up to 45 DEG C and delayed after stirring 2 hours
The slow oxalic acid being added with weight such as natural graphites continues that temperature is kept to stir 1 hour, filters and much filtrate is washed to neutrality；
Filter cake is added in the potassium permanganate concentrated sulfuric acid solution that mass fraction is 15%, is warming up to 55 DEG C and continuously stirs 2 hours, slowly
Until the aqueous hydrogen peroxide solution to bubble-free that mass fraction is 25% is added, continues constant temperature and stir 1 hour, filter and will filter out
Object is washed to neutrality, obtains graphene oxide；
(2) magnesium citrate, magnesium acetate and two water nitric acid oxidation zirconiums are dissolved in the aqueous hydrochloric acid solution that mass fraction is 16%
Solution A is formed, it is to form solution B in 29% aqueous citric acid solution that nine water chromic nitrates, which are dissolved in mass fraction, with continuous stirring,
Solution A is slowly added in solution B, agar powder is added after stirring 2 hours, after being warming up to 93 DEG C and stirs to being completely dissolved, cools down
248 are warming up to the speed for being no more than 3 DEG C per minute in chamber type electric resistance furnace after the drying of this gel to gel formed at room temperature
DEG C, it keeps this temperature 4 hours, continues to be warming up to 445 DEG C with the speed for being no more than 3 DEG C per minute, keep this temperature 3 hours, from
So it is cooled to room temperature to obtain by MgO, ZrO2And Cr2O3The metal composite oxide of composition；
(3) with continuous stirring, this metal composite oxide is added in the hydrazine hydrate aqueous solution that mass fraction is 17%,
Then graphene oxide above-mentioned is also added thereto, is warming up to 45 DEG C, constant temperature stirs 4 hours, uses after natural cooling and filtering
Deionized water is washed 3 times, and it is graphene-supported by MgO, ZrO to get arriving to be subsequently placed in 65 DEG C of vacuum drying oven drying2And Cr2O3
The composite powder material of composition.
Analysis: this composite powder material is tested with transmission electron microscope, maximum particle diameter is no more than 44nm, average grain diameter
About 32nm；Constituent analysis is carried out to it, measuring each component mass percent is respectively 10.5%MgO, 5.2%ZrO2、
10.7%Cr2O3And 73.6%C.
Using: the formaldehyde in air, range of linearity 0.03- are detected using this composite granule as catalytic luminescence sensitive material
15mg/m3, detect and be limited to 0.01mg/m3, other common concurrents do not interfere with.
Claims (1)
1. the sensitive material of trace formaldehyde in a kind of high selection measurement air, it is characterized in that graphene-supported by MgO, ZrO2With
Cr2O3The partial size of composition be no more than 45nm composite powder material, wherein the mass percent range of each component be 8-12%MgO,
5-8%ZrO2, 7-13%Cr2O3And 70-80%C, preparation method are: (1) being with continuous stirring slowly added to natural graphite
It in oleum, is warming up to 45 DEG C and is slowly added to the oxalic acid with weight such as natural graphites after stirring 2-3 hours, continue to keep temperature
Degree stirring 1 hour, filters and much filtrate is washed to neutrality；The potassium permanganate concentrated sulfuric acid that mass fraction is 15% is added in filter cake
It in solution, is warming up to 50-55 DEG C and continuously stirs 2 hours, be slowly added to the aqueous hydrogen peroxide solution that mass fraction is 25% extremely
Until bubble-free, continues constant temperature and stir 1 hour, filter and much filtrate is washed to neutrality, obtain graphene oxide；(2) by magnesium
Salt and zirconates, which are dissolved in the aqueous hydrochloric acid solution that mass fraction is 15-20%, forms solution A, and it is 20- that chromic salts, which is dissolved in mass fraction,
Solution B is formed in 30% aqueous citric acid solution, and with continuous stirring, solution A is slowly added in solution B, after stirring 2 hours,
Agar powder is added after being warming up to 92-95 DEG C to stir to being completely dissolved, is cooled to room temperature to form gel, after the drying of this gel,
It is warming up to 200-250 DEG C with the speed for being no more than 3 DEG C per minute in chamber type electric resistance furnace, keeps this temperature 4 hours, is continued with every point
Speed of the clock no more than 3 DEG C is warming up to 400-450 DEG C, keeps this temperature 3 hours, cooled to room temperature is obtained by MgO, ZrO2
And Cr2O3The metal composite oxide of composition；(3) with continuous stirring, it is by this metal composite oxide addition mass fraction
In the hydrazine hydrate aqueous solution of 15-20%, then graphene oxide above-mentioned is also added thereto, is warming up to 45 DEG C, constant temperature stirring
It 4-5 hours, is washed with deionized 3 times after natural cooling and filtering, is subsequently placed in 65 DEG C of vacuum drying oven drying to get stone is arrived
The load of black alkene by MgO, ZrO2And Cr2O3The composite powder material of composition；The magnesium salts is magnesium chloride, magnesium sulfate, nitric acid
Magnesium, magnesium oxalate, the anhydride of magnesium citrate and magnesium acetate or hydrate one or more of mixtures, zirconates is oxychloride
Zirconium, acetic acid zirconium, zirconium sulfate, the anhydride of zirconium chloride and nitric acid oxidation zirconium or hydrate one or more of mixtures, chromium
Salt is the anhydride of chromium chloride, perchloric acid chromium, chromic acetate, chromium+oxalic acid, chromic nitrate and chromium sulfate or the one or more of hydrate
Mixture.
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| 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 |
| CN109490372B (en) * | 2018-11-30 | 2020-11-17 | 北京联合大学 | Catalytic luminous sensitive material of ethanol |
| CN110672591B (en) * | 2019-10-22 | 2021-10-12 | 北京联合大学 | Low-temperature response sensitive material for formaldehyde and trimethylamine in air |
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