CN104237347B - Preparation method for the carbon nanotube electrode of formaldehyde examination - Google Patents
Preparation method for the carbon nanotube electrode of formaldehyde examination Download PDFInfo
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- CN104237347B CN104237347B CN201410529696.7A CN201410529696A CN104237347B CN 104237347 B CN104237347 B CN 104237347B CN 201410529696 A CN201410529696 A CN 201410529696A CN 104237347 B CN104237347 B CN 104237347B
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Abstract
The present invention relates to the preparation method of a kind of carbon nanotube electrode for formaldehyde examination, and be prepared for a kind of electrochemical sensor based on this electrode, for the detection of formaldehyde.The present invention passes through La (NO3)3、Co(NO3)3, CNT (CNT), citric acid prepare the LaCoO with nanostructured3CNT is also coated to glassy carbon electrode surface, is prepared as LaCoO3CNT/GC electrode, and prepare electrochemical sensor.The present invention relates to based on LaCoO3The electrochemical sensor of CNT/GC electrode, when being used for detecting content of formaldehyde, has and carries the features such as easy to use, volume is little, detection limit is low, fast response time, selectivity are good, have the prospect in daily life as conventional sense instrument.
Description
Technical field
The present invention relates to electrochemical sensor electrodes field, be specifically related to the system of a kind of carbon nano-tube combination electrode
Preparation Method and the purposes in terms of electrochemical sensor thereof.
Background technology
Formaldehyde, as a kind of important raw material of industry, has widely at aspects such as chemical industry, food, building materials
Application.But the pollution problem of formaldehyde is paid close attention to by people the most always, especially in terms of building, after house decoration,
The formaldehyde of residual has stimulation to mucocutaneous, people can be made to be poisoned with the protein bound in human body, and
Formaldehyde also has the highest carcinogenic and teratogenesis shape, therefore, it is possible to the most qualitatively and quantitatively detect formaldehyde,
It it is the premise solving formaldehyde pollution problem.
Traditional method measuring formaldehyde is mainly physico-chemical method and measures, and has absorption photometry, chromatography, pole
Spectrometry, kinetic analysis, Flow Injection Analysis etc., these methods disadvantage is that collection in worksite sample,
It is analyzed in laboratory again, it is impossible to meet the requirements such as the detection of quick real-time online, continuous detecting.
In the sensor of the detection formaldehyde of at present application, metal oxide sensor generally exist sensitivity the highest,
The shortcoming that selectivity is bad；The detection limit of surface acoustic wave type sensor PARA FORMALDEHYDE PRILLS(91,95) requires height, can not detect
The formaldehyde of trace；Optochemical sensor research in terms of formaldehyde examination is the most immature；And electrochemical sensor
In terms of formaldehyde examination, there is bigger progress, especially prepare aspect at nano-electrode, but about LaCoO3
Do not have been reported that with the electrochemical sensor of carbon nano-tube combination electrode.
Summary of the invention
Defect based on prior art, the present invention is prepared for a kind of can be used for and detects formaldehyde
LaCoO3-CNT/GC electrode, and based on this electrode, it is prepared for a kind of electrochemical sensor, can facilitate
Measure the content of formaldehyde in air quickly.
A kind of LaCoO3The preparation method of-CNT/GC electrode, comprises the steps:
(1) dosing: take 1～3 part of La (NO3)3, 1～3 part of Co (NO3)3, 3～9 parts of CNTs (CNT),
10～30 parts of citric acids, join in 100～300 parts of water and shake, and carry out magnetic agitation, and temperature is 50 DEG C,
Stir speed (S.S.) is 120～200r/min, and mixing time is 1～3h.
(2) baking: the complex solution of mix homogeneously is put into ventilation, bakes with dense drying equipment such as hot blast
Complex solution is baked into powdery solid granules by casees etc., and solid particle is put into high-temperature calcination in Muffle furnace
3～9h, calcining heat is 600～900 DEG C, is carefully ground by the solid of cooling after having calcined in mortar,
To black gray expandable powder.
(3)LaCoO3The preparation of-CNT: black gray expandable powder initial product step (2) obtained takes 1～3
Part, join in the NaOH solution of 30% of 100～300 parts, sonic oscillation 15～30min, so that suspended
Liquid is more uniform, is positioned in baking oven by suspension, temperature is set to 80～160 DEG C, reacts 10～24h,
Cool down after having reacted, be washed with deionized 5～8 times, i.e. obtain LaCoO3-CNT, with sonic oscillation
Method is by LaCoO3-CNT is dispersed in water, is configured to the LaCoO of 1mg/mL3-CNT suspension.
(4) preparation of electrode: take the glassy carbon electrode of a diameter 2mm, use Al2O3Sanding and polishing, then
With deionized water rinsing 3～5 times, take the LaCoO of 1～5 μ L3-CNT suspension is coated in above-mentioned sanding and polishing
Glassy carbon electrode surface, be dried 10～15h at ambient temperature, i.e. obtain LaCoO3-CNT/GC electrode.
The LaCoO of the present invention3-CNT/GC electrode can be used for preparing electrochemical sensor, and for the inspection of formaldehyde
Survey, particularly as follows: by LaCoO3-CNT/GC electrode, as working electrode, is together fixed to electricity with reference electrode
In the components and parts of chemical sensor, and it is encapsulated on components and parts substrate, a part for electrode and electrolyte contact,
Covering one layer of filter membrane above electrolyte, formaldehyde gas can enter into dielectric substrate by filter membrane, thus quilt
LaCoO3-CNT/GC electrode detects with reference electrode, produces electric potential difference between the two, this electric potential difference with
The form of the signal of telecommunication is delivered in external circuit, and external circuit is processed by data, in external display device
Directly display out by the concentration values of formaldehyde.
The LaCoO that the present invention relates to3In-CNT/GC electrode, LaCoO3PARA FORMALDEHYDE PRILLS(91,95) has good selectivity,
CNT can increase the specific surface area that electrode contacts with formaldehyde gas, by the LaCoO of carbon nano-tube modification3
Glassy carbon electrode had both had the advantage of nano material and had also remained the high selectivity of PARA FORMALDEHYDE PRILLS(91,95) own.
The LaCoO that the present invention relates to3The electrochemical sensor that-CNT/GC electrode and base are prepared with this electrode, tool
Carry the features such as easy to use, volume is little, detection limit is low, fast response time, selectivity are good, have
As the prospect of conventional sense instrument in daily life.
Detailed description of the invention
Below by specific embodiment, further technical scheme is specifically described.Should manage
Solving, the following examples are intended only as illustrating, and do not limit the scope of the invention, simultaneously this area
Technical staff obvious is changed and within modification is also contained in the scope of the invention according to what the present invention made.
Embodiment 1
A kind of LaCoO3The preparation method of-CNT/GC electrode, comprises the steps:
(1) dosing: take 1 part of La (NO3)3, 1 part of Co (NO3)3, 3 parts of CNTs (CNT), 10
Part citric acid, joins in 100 parts of water and shakes, and to carry out magnetic agitation temperature be 50 DEG C, and stir speed (S.S.) is
120r/min, mixing time is 1h.
(2) baking: the complex solution of mix homogeneously is put into ventilation, with dense drying equipment, complexation is molten
Liquid is baked into powdery solid granules, and solid particle is put into high-temperature calcination 3h in Muffle furnace, and calcining heat is
800 DEG C, after having calcined, the solid of cooling is carefully ground in mortar, obtain black gray expandable powder.
(3)LaCoO3The preparation of-CNT: black gray expandable powder initial product step (2) obtained takes 1
Part, join in the NaOH solution of 30% of 100 parts, sonic oscillation 30min, so that suspension is more
Uniformly.Suspension is positioned in baking oven, temperature is set to 160 DEG C, react 10h, cold after having reacted
But, it is washed with deionized 8 times, i.e. obtains LaCoO3-CNT, will by the method for sonic oscillation
LaCoO3-CNT is dispersed in water, is configured to the LaCoO of 1mg/mL3-CNT suspension.
(4) preparation of electrode: take the glassy carbon electrode of a diameter 2mm, use Al2O3Sanding and polishing, then
With deionized water rinsing 3～5 times, take the LaCoO of 1 μ L3-CNT suspension is coated in above-mentioned sanding and polishing
Glassy carbon electrode surface, is dried 10h at ambient temperature, i.e. obtains LaCoO3-CNT/GC electrode.
Embodiment 2
A kind of LaCoO3The preparation method of-CNT/GC electrode, comprises the steps:
(1) dosing: take 2 parts of La (NO3)3, 2 parts of Co (NO3)3, 6 parts of CNTs (CNT), 20
Part citric acid, joins in 200 parts of water and shakes, and to carry out magnetic agitation temperature be 50 DEG C, and stir speed (S.S.) is
160r/min, mixing time is 2h.
(2) baking: the complex solution of mix homogeneously is put into ventilation, dries complex solution with hot-blast oven
Being roasted into powdery solid granules, solid particle is put into high-temperature calcination 5h in Muffle furnace, calcining heat is 700 DEG C,
After having calcined, the solid of cooling is carefully ground in mortar, obtain black gray expandable powder.
(3)LaCoO3The preparation of-CNT: black gray expandable powder initial product step (2) obtained takes 2
Part, join in the NaOH solution of 30% of 200 parts, sonic oscillation 25min, so that suspension is more
Uniformly.Suspension is positioned in baking oven, temperature is set to 120 DEG C, react 17h, cold after having reacted
But, it is washed with deionized 6 times, obtains LaCoO3-CNT, by the method for sonic oscillation by LaCoO3-CNT
It is dispersed in water, is configured to the LaCoO3-CNT suspension of 1mg/mL.
(4) preparation of electrode: take the glassy carbon electrode of a diameter 2mm, use Al2O3Sanding and polishing, then
With deionized water rinsing 3～5 times, take the LaCoO of 3 μ L3-CNT suspension is coated in above-mentioned sanding and polishing
Glassy carbon electrode surface, is dried 13h at ambient temperature, i.e. obtains LaCoO3-CNT/GC electrode.
Claims (5)
1. being used for the preparation method of the carbon nanotube electrode of formaldehyde examination, its step is as follows:
(1) dosing: take 1～3 part of La (NO3)3, 1～3 part of Co (NO3)3, 3～9 parts of CNTs (CNT),
10～30 parts of citric acids, join in 100～300 parts of water and shake, and carry out magnetic agitation, and temperature is 50 DEG C,
Stir speed (S.S.) is 120～200r/min, and mixing time is 1～3h；
(2) baking: the complex solution of mix homogeneously is put into ventilation, with dense drying equipment, complexation is molten
Liquid is baked into powdery solid granules, and solid particle is put into high-temperature calcination 3～9h, calcining heat in Muffle furnace
It is 600～900 DEG C, after having calcined, the solid of cooling is carefully ground in mortar, obtain black gray expandable powder；
(3)LaCoO3The preparation of-CNT: black gray expandable powder initial product step (2) obtained takes 1～3
Part, join in the NaOH solution of 30% of 100～300 parts, sonic oscillation 15～30min, formed suspended
Liquid；Suspension is positioned in 80～160 DEG C of baking ovens, react 10～24h, cool down after having reacted, spend from
Sub-water washs 5～8 times, obtains LaCoO3-CNT, by the method for sonic oscillation by LaCoO3-CNT is uniform
It is dispersed in water, is configured to the LaCoO of 1mg/mL3-CNT suspension；
(4) preparation of electrode: take the glassy carbon electrode of a diameter 2mm, use Al2O3Sanding and polishing, then
With deionized water rinsing 3～5 times, take the LaCoO of 1～5 μ L3-CNT suspension is coated in above-mentioned sanding and polishing
Glassy carbon electrode surface, be dried 10～15h at ambient temperature, i.e. obtain LaCoO3-CNT/GC electrode.
The preparation method of electrode the most according to claim 1, it is characterised in that: step (2) is described close
Integrate roasting plant as hot-blast oven.
3. possess an electrochemical sensor for electrode prepared by method according to claim 1 or claim 2, its
It is characterised by: by LaCoO3-CNT/GC electrode, as working electrode, is together fixed to electrification with reference electrode
Learn in the components and parts of sensor, and be encapsulated on components and parts substrate, a part for electrode and electrolyte contact,
One layer of filter membrane is covered above electrolyte.
4. the purposes of an electrochemical sensor based on claim 3, it is characterised in that: described electrochemistry
Sensor is for detecting the concentration of formaldehyde gas.
5. electrochemical sensor based on claim 3 is for the method detecting concentration of formaldehyde, its feature
It is: formaldehyde gas enters into dielectric substrate by filter membrane, by LaCoO3-CNT/GC electrode and reference electricity
Pole detects, produces electric potential difference between the two, and this electric potential difference is delivered to external circuit as electronic signals
In, external circuit is processed by data, is directly displayed out by the concentration values of formaldehyde in external display device
Come.
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| CN201410529696.7A CN104237347B (en) | 2014-10-09 | 2014-10-09 | Preparation method for the carbon nanotube electrode of formaldehyde examination |
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| CN201410529696.7A CN104237347B (en) | 2014-10-09 | 2014-10-09 | Preparation method for the carbon nanotube electrode of formaldehyde examination |
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Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5286363A (en) * | 1990-10-18 | 1994-02-15 | Georgia-Pacific Resins, Inc. | Dynamic microchamber for measuring formaldehyde emissions |
| US5393495A (en) * | 1992-08-17 | 1995-02-28 | Intoximeters, Inc. | Method and apparatus for testing gases, particularly breath alcohol |
| KR100823516B1 (en) * | 2006-11-21 | 2008-04-21 | 포항공과대학교 산학협력단 | A sensor for formaldehyde using piezoresistive cantilever |
| AU2009214455A1 (en) * | 2008-02-15 | 2009-08-20 | Georgia Tech Research Corporation | Systems and methods for providing environment monitoring |
| CN102183568B (en) * | 2011-02-10 | 2013-03-27 | 深圳市联祥瑞智能设备有限公司 | Formaldehyde electrochemical sensor |
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Effective date of registration: 20171116 Address after: Group 21, 538000 the Guangxi Zhuang Autonomous Region Dongxing city jiangpingzhen million tail village 22 groups and 23 groups of Interchange Patentee after: DONGXING HONGSHENG INDUSTRIAL CO., LTD. Address before: Xishan Economic Development Zone, Jiangsu province 214192 Technology Park in Wuxi city (three Furong Road No. 99) cloud six Patentee before: Wuxi Bailing Sensing Technology Co., Ltd. |
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Granted publication date: 20160824 Termination date: 20181009 |