CN108445141A - A kind of low temperature formaldehyde catalytic luminescence sensitive material - Google Patents
A kind of low temperature formaldehyde catalytic luminescence sensitive material Download PDFInfo
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- CN108445141A CN108445141A CN201810087483.1A CN201810087483A CN108445141A CN 108445141 A CN108445141 A CN 108445141A CN 201810087483 A CN201810087483 A CN 201810087483A CN 108445141 A CN108445141 A CN 108445141A
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- 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
Abstract
A kind of low temperature formaldehyde catalytic luminescence sensitive material, it is characterized in that by atom doped Pd CoO, TiO2And Al2O3The composite powder material of composition, preparation method are：Cobalt salt, titanium salt and aluminium salt are codissolved in aqueous hydrochloric acid solution, citric acid is added, ammonium hydroxide is added dropwise and adjusts pH value, rotary evaporation obtains gel after ageing, after this gel drying is ground, is roasted in chamber type electric resistance furnace and obtains mixed powder；Hydrazine hydrate is added in palladium dichloride solution, above-mentioned mixed powder is added after reduction, dries, two-stage roasting under state is vacuumized in tube furnace, cooled to room temperature in the state that argon gas is protected obtains CoO, TiO for being mixed up by Pd atoms2And Al2O3The composite powder material of composition.The gas sensor made using sensitive material provided by the present invention, can be in the trace formaldehyde 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 formaldehyde catalytic luminescence sensitive materials, especially by atom doped Pd CoO, TiO2With
Al2O3The composite powder material of composition, belongs to field of sensing technologies.
Background technology
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 various concentration 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 declines, damages 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.
Measure 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., since these methods are required for preconcentration and proper treatment that could pass through analytical instrument
It completes to measure, therefore time-consuming is not easy live realization.Inventor is in 2006 in Sensors＆Actuators：B.Chemical
On delivered entitled " On-line Monitoring of Formaldehyde in Air by Cataluminescence-
Use nanoscale vanadium titanium (atomic ratio 1: 2) composite oxides, can as sensitive material in the paper of based gas Sensor "
With 0.1~40mg/m of on-line checking3Formaldehyde, detection limit is up to 0.06mg/m3, temperature in use is 370 DEG C；In 2008《Change
Learn journal》On deliver it is entitled " nano composite oxide catalytic luminescence method measure air in formaldehyde " paper in using improve
Nanoscale molybdenum vanadium titanium (atomic ratio 2: 3: 5) composite oxides as sensitive material, can be with 0.07~34mg/m of on-line checking3
Formaldehyde, detection limit is up to 0.04mg/m3, temperature in use is 265 DEG C.But carry out Miniaturization Design using this sensitive material
When, compared with operation at high temperature stability contorting at problem, and make an uproar compared with intense radiant heat background signal caused by the minor fluctuations of high temperature
Sound (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, providing one kind, PARA FORMALDEHYDE PRILLS(91,95) has compared with high selection at a lower temperature
The sensitive material of property and catalytic activity.The gas sensor made of this sensitive material, can more delicately measure at the scene
Trace formaldehyde in air by concurrent without being interfered.
Sensitive material of the present invention is by atom doped Pd CoO, TiO2And Al2O3The composite powder material of composition,
Preparation method is as follows：
(1) cobalt salt, titanium salt and aluminium salt are codissolved in the aqueous hydrochloric acid solution of 10-15%, are warming up to 55 DEG C in high-speed stirred
Citric acid is added under state and solution is made to keep clear state, 8-10% ammonium hydroxide, which is added dropwise, makes solution ph be 5.5-6.1, is cooled to
Room temperature is simultaneously 5-7 hours still aging, and solution is obtained gel in 80-85 DEG C of rotary evaporation, and gel drying 2 hours is fully ground
After mill, it is warming up to 380-400 DEG C with the speed per minute for being no more than 5 DEG C in chamber type electric resistance furnace, keeps this temperature 5 hours, from
So cooling obtains mixed powder；
(2) palladium chloride is dissolved in the aqueous hydrochloric acid solution that mass fraction is 6%, mass fraction is added dropwise under constant stirring
It for 20% hydrazine hydrate aqueous solution, is warming up to 50 DEG C and continuously stirs 4 hours, be cooled to room temperature and disperseed ultrasonic wave above-mentioned
Mixed powder is added thereto, and is uniformly mixed, is dried in drying box, be subsequently placed in tube furnace and be evacuated to 1 × 10-2Pa, with
The speed per minute for being no more than 3 DEG C is warming up to 530-560 DEG C, keeps this temperature 3-4 hours, keeps 1 × 10-2The vacuum state of Pa
Continue with the speed per minute for being no more than 3 DEG C to be warming up to 950 DEG C, keep this temperature 2 hours, is passed through argon gas to 50kPa, it is naturally cold
But to being vented after room temperature, CoO, TiO for being mixed up by Pd atoms are obtained2And Al2O3The composite powder material of composition.
Wherein, cobalt salt is the anhydride or hydrate of cobalt nitrate, cobalt carbonate, cobaltous sulfate, cobalt chloride, cobalt acetate and cobalt phosphate
One or more of mixtures, titanium salt is the anhydride or hydrate of titanium sulfate, titanyl sulfate, titanium trichloride and titanium tetrachloride
One or more of mixtures, aluminium salt is the anhydrous of aluminum nitrate, aluminum sulfate, aluminum perchlorate, aluminum phosphate, aluminium chloride and aluminum acetate
One or more of mixtures of object or hydrate.
Each component mass fraction meets Pd (2-4%), CoO (25-35%), TiO in composite powder material obtained2(30-
And Al 40%)2O3When (25-35%), it is used as the catalytic luminescence sensitive material of formaldehyde in air, just at 200 DEG C or less
There is very high catalytic luminescence activity.
Specific implementation mode
Embodiment 1
(1) cobalt nitrate hexahydrate, nine water titanium sulfates and nine water aluminum nitrates are codissolved in 10% aqueous hydrochloric acid solution, are warming up to
55 DEG C citric acid is added under high-speed stirred state and solution is made to keep clear state, and 10% ammonium hydroxide, which is added dropwise, makes the solution ph be
5.6, it is cooled to room temperature and 5 hours still aging, solution is obtained into gel in 80 DEG C of rotary evaporations, gel drying 2 hours fills
After dividing grinding, 380 DEG C are warming up to the speed per minute for being no more than 5 DEG C in chamber type electric resistance furnace, keeps this temperature 5 hours, from
So cooling obtains mixed powder；
(2) palladium chloride is dissolved in the aqueous hydrochloric acid solution that mass fraction is 6%, mass fraction is added dropwise under constant stirring
It for 20% hydrazine hydrate aqueous solution, is warming up to 50 DEG C and continuously stirs 4 hours, be cooled to room temperature and disperseed ultrasonic wave above-mentioned
Mixed powder is added thereto, and is uniformly mixed, is dried in drying box, be subsequently placed in tube furnace and be evacuated to 1 × 10-2Pa, with
The speed per minute for being no more than 3 DEG C is warming up to 535 DEG C, keeps this temperature 4 hours, keeps 1 × 10-2The vacuum state of Pa continue with
The speed per minute for being no more than 3 DEG C is warming up to 950 DEG C, keeps this temperature 2 hours, is passed through argon gas to 50kPa, naturally cools to room
It is vented after temperature, obtains CoO, TiO for being mixed up by Pd atoms2And Al2O3The composite powder material of composition.
Analysis：To composite powder material carry out constituent analysis, measure mass percent be 2.5%Pd, 27.8%CoO,
36.2%TiO2And 33.5%Al2O3。
Using：Using this powder body material as the catalytic luminescence sensitive material of detection formaldehyde, operating temperature is 167 DEG C, linearly
Ranging from 0.05-50mg/m3, detect and be limited to 0.02mg/m3, common concurrent do not interfere with.
Embodiment 2
(1) hydration cobalt carbonate, titanyl sulfate and aluminum sulfate octadecahydrate are codissolved in 14% aqueous hydrochloric acid solution, are warming up to
55 DEG C citric acid is added under high-speed stirred state and solution is made to keep clear state, and 9% ammonium hydroxide, which is added dropwise, makes the solution ph be
6.0, it is cooled to room temperature and 7 hours still aging, solution is obtained into gel in 85 DEG C of rotary evaporations, gel drying 2 hours fills
After dividing grinding, 385 DEG C are warming up to the speed per minute for being no more than 5 DEG C in chamber type electric resistance furnace, keeps this temperature 5 hours, from
So cooling obtains mixed powder；
(2) palladium chloride is dissolved in the aqueous hydrochloric acid solution that mass fraction is 6%, mass fraction is added dropwise under constant stirring
It for 20% hydrazine hydrate aqueous solution, is warming up to 50 DEG C and continuously stirs 4 hours, be cooled to room temperature and disperseed ultrasonic wave above-mentioned
Mixed powder is added thereto, and is uniformly mixed, is dried in drying box, be subsequently placed in tube furnace and be evacuated to 1 × 10-2Pa, with
The speed per minute for being no more than 3 DEG C is warming up to 540 DEG C, keeps this temperature 4 hours, keeps 1 × 10-2The vacuum state of Pa continue with
The speed per minute for being no more than 3 DEG C is warming up to 950 DEG C, keeps this temperature 2 hours, is passed through argon gas to 50kPa, naturally cools to room
It is vented after temperature, obtains CoO, TiO for being mixed up by Pd atoms2And Al2O3The composite powder material of composition.
Analysis：To composite powder material carry out constituent analysis, measure mass percent be 3.3%Pd, 33.2%CoO,
34.7%TiO2And 28.8%Al2O3。
Using：Using this powder body material as the catalytic luminescence sensitive material of detection formaldehyde, operating temperature is 165 DEG C, linearly
Ranging from 0.06-51mg/m3, detect and be limited to 0.03mg/m3, common concurrent do not interfere with.
Embodiment 3
(1) cobalt sulfate hydrate, CoCL2 6H2O, titanium trichloride and Aluminum Chloride Hexahydrate are codissolved in 12% aqueous hydrochloric acid solution
In, it is warming up to 55 DEG C and citric acid is added under high-speed stirred state and solution is made to keep clear state, 8% ammonium hydroxide, which is added dropwise, makes solution
PH value is 5.8, is cooled to room temperature and 6 hours still aging, solution is obtained gel in 81 DEG C of rotary evaporations, by gel drying 2
Hour, after being fully ground, 390 DEG C are warming up to the speed per minute for being no more than 5 DEG C in chamber type electric resistance furnace, keeps this temperature 5
Hour, natural cooling obtains mixed powder；
(2) palladium chloride is dissolved in the aqueous hydrochloric acid solution that mass fraction is 6%, mass fraction is added dropwise under constant stirring
It for 20% hydrazine hydrate aqueous solution, is warming up to 50 DEG C and continuously stirs 4 hours, be cooled to room temperature and disperseed ultrasonic wave above-mentioned
Mixed powder is added thereto, and is uniformly mixed, is dried in drying box, be subsequently placed in tube furnace and be evacuated to 1 × 10-2Pa, with
The speed per minute for being no more than 3 DEG C is warming up to 545 DEG C, keeps this temperature 3 hours, keeps 1 × 10-2The vacuum state of Pa continue with
The speed per minute for being no more than 3 DEG C is warming up to 950 DEG C, keeps this temperature 2 hours, is passed through argon gas to 50kPa, naturally cools to room
It is vented after temperature, obtains CoO, TiO for being mixed up by Pd atoms2And Al2O3The composite powder material of composition.
Analysis：To composite powder material carry out constituent analysis, measure mass percent be 3.8%Pd, 34.4%CoO,
35.6%TiO2And 26.2%Al2O3。
Using：Using this powder body material as the catalytic luminescence sensitive material of detection formaldehyde, operating temperature is 175 DEG C, linearly
Ranging from 0.05-50mg/m3, detect and be limited to 0.02mg/m3, common concurrent do not interfere with.
Embodiment 4
(1) Cobalt diacetate tetrahydrate, titanium tetrachloride, aluminum phosphate and nine water aluminum perchlorates are codissolved in 13% aqueous hydrochloric acid solution
In, it is warming up to 55 DEG C and citric acid is added under high-speed stirred state and solution is made to keep clear state, 9% ammonium hydroxide, which is added dropwise, makes solution
PH value is 5.7, is cooled to room temperature and 5 hours still aging, solution is obtained gel in 83 DEG C of rotary evaporations, by gel drying 2
Hour, after being fully ground, 395 DEG C are warming up to the speed per minute for being no more than 5 DEG C in chamber type electric resistance furnace, keeps this temperature 5
Hour, natural cooling obtains mixed powder；
(2) palladium chloride is dissolved in the aqueous hydrochloric acid solution that mass fraction is 6%, mass fraction is added dropwise under constant stirring
It for 20% hydrazine hydrate aqueous solution, is warming up to 50 DEG C and continuously stirs 4 hours, be cooled to room temperature and disperseed ultrasonic wave above-mentioned
Mixed powder is added thereto, and is uniformly mixed, is dried in drying box, be subsequently placed in tube furnace and be evacuated to 1 × 10-2Pa, with
The speed per minute for being no more than 3 DEG C is warming up to 550 DEG C, keeps this temperature 3 hours, keeps 1 × 10-2The vacuum state of Pa continue with
The speed per minute for being no more than 3 DEG C is warming up to 950 DEG C, keeps this temperature 2 hours, is passed through argon gas to 50kPa, naturally cools to room
It is vented after temperature, obtains CoO, TiO for being mixed up by Pd atoms2And Al2O3The composite powder material of composition.
Analysis：To composite powder material carry out constituent analysis, measure mass percent be 2.1%Pd, 32.9%CoO,
33.9%TiO2And 31.1%Al2O3。
Using：Using this powder body material as the catalytic luminescence sensitive material of detection formaldehyde, operating temperature is 170 DEG C, linearly
Ranging from 0.07-54mg/m3, detect and be limited to 0.03mg/m3, common concurrent do not interfere with.
Embodiment 5
(1) eight water cobalt phosphates, nine water titanium sulfates and acetate dihydrate aluminium are codissolved in 15% aqueous hydrochloric acid solution, are warming up to
55 DEG C citric acid is added under high-speed stirred state and solution is made to keep clear state, and 10% ammonium hydroxide, which is added dropwise, makes the solution ph be
6.0, it is cooled to room temperature and 6 hours still aging, solution is obtained into gel in 84 DEG C of rotary evaporations, gel drying 2 hours fills
After dividing grinding, 400 DEG C are warming up to the speed per minute for being no more than 5 DEG C in chamber type electric resistance furnace, keeps this temperature 5 hours, from
So cooling obtains mixed powder；
(2) palladium chloride is dissolved in the aqueous hydrochloric acid solution that mass fraction is 6%, mass fraction is added dropwise under constant stirring
It for 20% hydrazine hydrate aqueous solution, is warming up to 50 DEG C and continuously stirs 4 hours, be cooled to room temperature and disperseed ultrasonic wave above-mentioned
Mixed powder is added thereto, and is uniformly mixed, is dried in drying box, be subsequently placed in tube furnace and be evacuated to 1 × 10-2Pa, with
The speed per minute for being no more than 3 DEG C is warming up to 560 DEG C, keeps this temperature 3 hours, keeps 1 × 10-2The vacuum state of Pa continue with
The speed per minute for being no more than 3 DEG C is warming up to 950 DEG C, keeps this temperature 2 hours, is passed through argon gas to 50kPa, naturally cools to room
It is vented after temperature, obtains CoO, TiO for being mixed up by Pd atoms2And Al2O3The composite powder material of composition.
Analysis：To composite powder material carry out constituent analysis, measure mass percent be 2.4%Pd, 25.7%CoO,
39.3%TiO2And 32.6%Al2O3。
Using：Using this powder body material as the catalytic luminescence sensitive material of detection formaldehyde, operating temperature is 162 DEG C, linearly
Ranging from 0.06-48mg/m3, detect and be limited to 0.02mg/m3, common concurrent do not interfere with.
Claims (2)
1. a kind of low temperature formaldehyde catalytic luminescence sensitive material, it is characterized in that by atom doped Pd CoO, TiO2And Al2O3Composition
Composite powder material, the wherein mass percent of each component ranging from 2-4%Pd, 25-35%CoO, 30-40%TiO2And 25-
35%Al2O3, preparation method is：(1) cobalt salt, titanium salt and aluminium salt are codissolved in the aqueous hydrochloric acid solution of 10-15%, are warming up to
55 DEG C citric acid is added under high-speed stirred state and solution is made to keep clear state, and 8-10% ammonium hydroxide, which is added dropwise, makes the solution ph be
5.5-6.1 is cooled to room temperature and 5-7 hours still aging, and solution is obtained gel in 80-85 DEG C of rotary evaporation, gel is done
Dry 2 hours, after being fully ground, it is warming up to 380-400 DEG C with the speed per minute for being no more than 5 DEG C in chamber type electric resistance furnace, is kept
This temperature 5 hours, natural cooling obtains mixed powder；(2) palladium chloride is dissolved in the aqueous hydrochloric acid solution that mass fraction is 6%
In, the hydrazine hydrate aqueous solution that mass fraction is 20% is added dropwise under constant stirring, is warming up to 50 DEG C and continuously stirs 4 hours, it is cooling
It is added thereto to room temperature and by the above-mentioned mixed powder that ultrasonic wave disperseed, is uniformly mixed, dries, be subsequently placed in drying box
1 × 10 is evacuated in tube furnace-2Pa is warming up to 530-560 DEG C with the speed per minute for being no more than 3 DEG C, keeps this temperature 3-4
Hour, keep 1 × 10-2The vacuum state of Pa continues to be warming up to 950 DEG C with the speed per minute for being no more than 3 DEG C, keeps this temperature 2
Hour, argon gas is passed through to 50kPa, is vented after cooled to room temperature, is obtained CoO, TiO for being mixed up by Pd atoms2And Al2O3Group
At composite powder material.
2. a kind of low temperature formaldehyde catalytic luminescence sensitive material according to claim 1, it is characterized in that the cobalt salt is nitre
Sour cobalt, cobalt carbonate, cobaltous sulfate, cobalt chloride, cobalt acetate and the anhydride of cobalt phosphate or one or more of mixtures of hydrate,
Titanium salt is the anhydride of titanium sulfate, titanyl sulfate, titanium trichloride and titanium tetrachloride or one or more of mixtures of hydrate,
Aluminium salt is the anhydride of aluminum nitrate, aluminum sulfate, aluminum perchlorate, aluminum phosphate, aluminium chloride and aluminum acetate or one kind of hydrate or several
The mixture of kind.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810087483.1A CN108445141B (en) | 2018-01-30 | 2018-01-30 | Low-temperature formaldehyde catalytic luminescent sensitive material |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810087483.1A CN108445141B (en) | 2018-01-30 | 2018-01-30 | Low-temperature formaldehyde catalytic luminescent sensitive material |
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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 |
| CN110095559A (en) * | 2019-04-03 | 2019-08-06 | 北京联合大学 | The catalytic luminescence sensitive material of low temperature formaldehyde, benzene and ammonia |
| CN111638207A (en) * | 2020-05-13 | 2020-09-08 | 北京联合大学 | Sensitive material for low-temperature formaldehyde, ammonia and carbon monoxide |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106964348A (en) * | 2017-04-14 | 2017-07-21 | 南京工业大学 | A kind of formaldehyde pollutants room temperature catalytic oxidation catalyst and its preparation method and application |
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2018
- 2018-01-30 CN CN201810087483.1A patent/CN108445141B/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106964348A (en) * | 2017-04-14 | 2017-07-21 | 南京工业大学 | A kind of formaldehyde pollutants room temperature catalytic oxidation catalyst and its preparation method and application |
Non-Patent Citations (1)
| Title |
|---|
| JINGJING PEI AND JIANSHUN S.ZHANG: "《Critical review of catalytic oxidization and chemisorption methods for indoor formaldehyde removal》", 《TAYLOR & FRANCIS》 * |
Cited By (5)
| 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 |
| CN110095559A (en) * | 2019-04-03 | 2019-08-06 | 北京联合大学 | The catalytic luminescence sensitive material of low temperature formaldehyde, benzene and ammonia |
| CN110095559B (en) * | 2019-04-03 | 2021-09-14 | 北京联合大学 | Catalytic luminous sensitive material of low-temperature formaldehyde, benzene and ammonia |
| CN111638207A (en) * | 2020-05-13 | 2020-09-08 | 北京联合大学 | Sensitive material for low-temperature formaldehyde, ammonia and carbon monoxide |
| CN111638207B (en) * | 2020-05-13 | 2023-04-21 | 北京联合大学 | Sensitive material for low temperature formaldehyde, ammonia and carbon monoxide |
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