CN104237347A - Method for manufacturing carbo nano tube electrode for formaldehyde test - Google Patents
Method for manufacturing carbo nano tube electrode for formaldehyde test Download PDFInfo
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- CN104237347A CN104237347A CN201410529696.7A CN201410529696A CN104237347A CN 104237347 A CN104237347 A CN 104237347A CN 201410529696 A CN201410529696 A CN 201410529696A CN 104237347 A CN104237347 A CN 104237347A
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Abstract
The invention relates to a method for manufacturing a carbo nano tube for formaldehyde test and an electrochemical sensor manufactured based on the electrode and for the formaldehyde test. La(NO3), Co(NO3), the carbo nano tube (CNT) and citric acid are utilized to prepare LaCoO3-CNT with the nanometer structure and enable the LaCoO3-CNT to coat the surface of a glass carbon electrode to prepare the LaCoO3-CNT/GC electrode and prepare the electrochemical sensor. When the electrochemical sensor based on the LaCoO3-CNT/GC electrode is used for detecting formaldehyde content, the electrochemical sensor has the advantages of being convenient to carry and use, small in size, low in detection limit, high in response speed, good in selectivity and the like and can serve as a normal inspection instrument in daily life.
Description
Technical field
The present invention relates to electrochemical sensor electrodes field, be specifically related to a kind of preparation method of carbon nano-tube combination electrode and the purposes in electrochemical sensor thereof.
Background technology
Formaldehyde, as a kind of important raw material of industry, has a wide range of applications in chemical industry, food, building materials etc.But the pollution problem of formaldehyde is also paid close attention to by people always, especially in building, after house decoration, residual formaldehyde has spread effect to mucocutaneous, can people be made poisoning with the protein bound in human body, and formaldehyde also have very high carcinogenic and teratogenesis shape, therefore, can detect formaldehyde in quantitative and qualitative analysis ground exactly, be the prerequisite solving formaldehyde pollution problem.
The method of traditional mensuration formaldehyde is mainly physico-chemical method and measures, there are absorption photometry, chromatography, polarography, kinetic analysis, Using Flow Injection Analysis etc., the shortcoming of these methods is to need collection in worksite sample, analyze in laboratory again, the requirements such as the detection of quick real-time online, continuous detecting can not be met.
In the sensor of the detection formaldehyde of current application, the shortcoming that the sensitivity of metal oxide sensor ubiquity is not high, selectivity is bad; The detectability of surface acoustic wave type sensor PARA FORMALDEHYDE PRILLS(91,95) requires high, can not detect the formaldehyde of trace; The research of Optochemical sensor in formaldehyde examination is also immature; And electrochemical sensor has larger progress in formaldehyde examination, especially in prepared by nano-electrode, but about LaCoO
3report is not had with the electrochemical sensor of carbon nano-tube combination electrode.
Summary of the invention
Based on the defect of prior art, the present invention has prepared a kind of LaCoO that can be used for detecting formaldehyde
3-CNT/GC electrode, and based on this electrode, prepared a kind of electrochemical sensor, the content of formaldehyde in air can be measured quickly and easily.
A kind of LaCoO
3the preparation method of-CNT/GC electrode, comprises the steps:
(1) dosing: get 1 ~ 3 part of La (NO
3)
3, 1 ~ 3 part of Co (NO
3)
3, 3 ~ 9 parts of carbon nano-tube (CNT), 10 ~ 30 parts of citric acids, join in 100 ~ 300 parts of water and shake, and carry out magnetic agitation, temperature is 50 DEG C, and stir speed (S.S.) is 120 ~ 200r/min, and mixing time is 1 ~ 3h.
(2) toast: the complex solution mixed is put into ventilation, with dense drying equipment such as hot-blast oven etc., complex solution is baked into powdery solid granules, solid particle is put into muffle furnace high-temperature calcination 3 ~ 9h, calcining heat is 600 ~ 900 DEG C, after having calcined, the solid of cooling is carefully ground in mortar, obtain black gray expandable powder.
(3) LaCoO
3the preparation of-CNT: black gray expandable powder initial product step (2) obtained gets 1 ~ 3 part, join in the NaOH solution of 100 ~ 300 parts 30%, sonic oscillation 15 ~ 30min, to make suspension more even, suspension is positioned in baking oven, temperature is set to 80 ~ 160 DEG C, reaction 10 ~ 24h, react rear cooling, spent deionized water 5 ~ 8 times, namely obtain LaCoO
3-CNT, by the method for sonic oscillation by LaCoO
3-CNT is dispersed in water, is mixed with the LaCoO of 1mg/mL
3-CNT suspension.
(4) preparation of electrode: the glassy carbon electrode getting a diameter 2mm, uses Al
2o
3sanding and polishing, then use deionized water rinsing 3 ~ 5 times, get the LaCoO of 1 ~ 5 μ L
3-CNT suspension is coated in the glassy carbon electrode surface of above-mentioned sanding and polishing, and dry 10 ~ 15h, namely obtains LaCoO at ambient temperature
3-CNT/GC electrode.
LaCoO of the present invention
3-CNT/GC electrode can be used for preparing electrochemical sensor, and for the detection of formaldehyde, is specially: by LaCoO
3-CNT/GC electrode is as working electrode, together be fixed in the components and parts of electrochemical sensor with contrast electrode, and be encapsulated on components and parts substrate, a part for electrode contacts with electrolyte, one deck filtering membrane is covered above electrolyte, formaldehyde gas enters into dielectric substrate by filtering membrane, thus by LaCoO
3-CNT/GC electrode and contrast electrode detect, produce electric potential difference between the two, and this electric potential difference is delivered in external circuit as electronic signals, and external circuit, by data processing, the concentration values of formaldehyde directly shows by external display device.
The LaCoO that the present invention relates to
3in-CNT/GC electrode, LaCoO
3pARA FORMALDEHYDE PRILLS(91,95) has good selectivity, and carbon nano-tube can increase the specific surface area that electrode contacts with formaldehyde gas, by the LaCoO of carbon nano-tube modification
3the advantage that glassy carbon electrode had both had a nano material also remains the high selectivity of PARA FORMALDEHYDE PRILLS(91,95) own.
The LaCoO that the present invention relates to
3-CNT/GC electrode and base be the electrochemical sensor prepared of electrode therewith, has features such as portably using conveniently, volume is little, detectability is low, fast response time, selectivity are good, has in daily life as the prospect of conventional sense instrument.
Embodiment
Below by specific embodiment, further technical scheme of the present invention is specifically described.Should be appreciated that, the following examples just as illustrating, and do not limit the scope of the invention, and the apparent change made according to the present invention of those skilled in the art simultaneously and modification are also contained within the scope of the invention.
Embodiment 1
A kind of LaCoO
3the preparation method of-CNT/GC electrode, comprises the steps:
(1) dosing: get 1 part of La (NO
3)
3, 1 part of Co (NO
3)
3, 3 parts of carbon nano-tube (CNT), 10 parts of citric acids, join in 100 parts of water and shake, and to carry out magnetic agitation temperature be 50 DEG C, stir speed (S.S.) is 120r/min, and mixing time is 1h.
(2) toast: the complex solution mixed is put into ventilation, with dense drying equipment, complex solution is baked into powdery solid granules, solid particle is put into muffle furnace high-temperature calcination 3h, calcining heat is 800 DEG C, after having calcined, the solid of cooling is carefully ground in mortar, obtain black gray expandable powder.
(3) LaCoO
3the preparation of-CNT: black gray expandable powder initial product step (2) obtained gets 1 part, joins in the NaOH solution of 100 parts 30%, sonic oscillation 30min, to make suspension more even.Be positioned over by suspension in baking oven, temperature be set to 160 DEG C, reaction 10h, has reacted rear cooling, has spent deionized water 8 times, namely obtained LaCoO
3-CNT, by the method for sonic oscillation by LaCoO
3-CNT is dispersed in water, is mixed with the LaCoO of 1mg/mL
3-CNT suspension.
(4) preparation of electrode: the glassy carbon electrode getting a diameter 2mm, uses Al
2o
3sanding and polishing, then use deionized water rinsing 3 ~ 5 times, get the LaCoO of 1 μ L
3-CNT suspension is coated in the glassy carbon electrode surface of above-mentioned sanding and polishing, and dry 10h, namely obtains LaCoO at ambient temperature
3-CNT/GC electrode.
Embodiment 2
A kind of LaCoO
3the preparation method of-CNT/GC electrode, comprises the steps:
(1) dosing: get 2 parts of La (NO
3)
3, 2 parts of Co (NO
3)
3, 6 parts of carbon nano-tube (CNT), 20 parts of citric acids, join in 200 parts of water and shake, and to carry out magnetic agitation temperature be 50 DEG C, stir speed (S.S.) is 160r/min, and mixing time is 2h.
(2) toast: the complex solution mixed is put into ventilation, with hot-blast oven, complex solution is baked into powdery solid granules, solid particle is put into muffle furnace high-temperature calcination 5h, calcining heat is 700 DEG C, after having calcined, the solid of cooling is carefully ground in mortar, obtain black gray expandable powder.
(3) LaCoO
3the preparation of-CNT: black gray expandable powder initial product step (2) obtained gets 2 parts, joins in the NaOH solution of 200 parts 30%, sonic oscillation 25min, to make suspension more even.Be positioned over by suspension in baking oven, temperature be set to 120 DEG C, reaction 17h, has reacted rear cooling, has spent deionized water 6 times, obtained LaCoO
3-CNT, by the method for sonic oscillation by LaCoO
3-CNT is dispersed in water, is mixed with the LaCoO3-CNT suspension of 1mg/mL.
(4) preparation of electrode: the glassy carbon electrode getting a diameter 2mm, uses Al
2o
3sanding and polishing, then use deionized water rinsing 3 ~ 5 times, get the LaCoO of 3 μ L
3-CNT suspension is coated in the glassy carbon electrode surface of above-mentioned sanding and polishing, and dry 13h, namely obtains LaCoO at ambient temperature
3-CNT/GC electrode.
Claims (5)
1., for the preparation method of the carbon nanotube electrode of formaldehyde examination, its step is as follows:
(1) dosing: get 1 ~ 3 part of La (NO
3)
3, 1 ~ 3 part of Co (NO
3)
3, 3 ~ 9 parts of carbon nano-tube (CNT), 10 ~ 30 parts of citric acids, join in 100 ~ 300 parts of water and shake, and carry out magnetic agitation, temperature is 50 DEG C, and stir speed (S.S.) is 120 ~ 200r/min, and mixing time is 1 ~ 3h;
(2) toast: the complex solution mixed is put into ventilation, with dense drying equipment, complex solution is baked into powdery solid granules, solid particle is put into muffle furnace high-temperature calcination 3 ~ 9h, calcining heat is 600 ~ 900 DEG C, after having calcined, the solid of cooling is carefully ground in mortar, obtains black gray expandable powder;
(3) LaCoO
3the preparation of-CNT: black gray expandable powder initial product step (2) obtained gets 1 ~ 3 part, joins in the NaOH solution of 100 ~ 300 parts 30%, sonic oscillation 15 ~ 30min, forms suspension; Be positioned over by suspension in 80 ~ 160 DEG C of baking ovens, reaction 10 ~ 24h, has reacted rear cooling, has spent deionized water 5 ~ 8 times, obtained LaCoO
3-CNT, by the method for sonic oscillation by LaCoO
3-CNT is dispersed in water, is mixed with the LaCoO of 1mg/mL
3-CNT suspension;
(4) preparation of electrode: the glassy carbon electrode getting a diameter 2mm, uses Al
2o
3sanding and polishing, then use deionized water rinsing 3 ~ 5 times, get the LaCoO of 1 ~ 5 μ L
3-CNT suspension is coated in the glassy carbon electrode surface of above-mentioned sanding and polishing, and dry 10 ~ 15h, namely obtains LaCoO at ambient temperature
3-CNT/GC electrode.
2. the preparation method of electrode according to claim 1, is characterized in that: the described dense drying equipment of step (2) is hot-blast oven.
3., based on an electrochemical sensor for claim 1 or 2, it is characterized in that: by LaCoO
3-CNT/GC electrode, as working electrode, is together fixed in the components and parts of electrochemical sensor with contrast electrode, and is encapsulated on components and parts substrate, and a part for electrode contacts with electrolyte, covers one deck filtering membrane above electrolyte.
4. based on a purposes for the electrochemical sensor of claim 3, it is characterized in that: described electrochemical sensor is for detecting the concentration of formaldehyde gas.
5. based on the electrochemical sensor of claim 3 for detecting a method for concentration of formaldehyde, it is characterized in that: formaldehyde gas enters into dielectric substrate by filtering membrane, by LaCoO
3-CNT/GC electrode and contrast electrode detect, produce electric potential difference between the two, and this electric potential difference is delivered in external circuit as electronic signals, and external circuit, by data processing, the concentration values of formaldehyde directly shows by external display device.
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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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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5393495A (en) * | 1992-08-17 | 1995-02-28 | Intoximeters, Inc. | Method and apparatus for testing gases, particularly breath alcohol |
| US5395494A (en) * | 1990-10-18 | 1995-03-07 | Georgia-Pacific Resins, Inc. | Dynamic microchamber for measuring formaldehyde emissions |
| KR100823516B1 (en) * | 2006-11-21 | 2008-04-21 | 포항공과대학교 산학협력단 | A sensor for formaldehyde using piezoresistive cantilever |
| CN101970990A (en) * | 2008-02-15 | 2011-02-09 | 佐治亚科技研究公司 | Systems and methods for providing environment monitoring |
| CN102183568A (en) * | 2011-02-10 | 2011-09-14 | 深圳市联祥瑞智能设备有限公司 | Formaldehyde electrochemical sensor |
-
2014
- 2014-10-09 CN CN201410529696.7A patent/CN104237347B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5395494A (en) * | 1990-10-18 | 1995-03-07 | 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 |
| CN101970990A (en) * | 2008-02-15 | 2011-02-09 | 佐治亚科技研究公司 | Systems and methods for providing environment monitoring |
| CN102183568A (en) * | 2011-02-10 | 2011-09-14 | 深圳市联祥瑞智能设备有限公司 | Formaldehyde electrochemical sensor |
Non-Patent Citations (3)
| Title |
|---|
| FEI TENG 等: "Carbon nanotubes-templated assembly of LaCoO3 nanowires at low temperatures and its excellent catalytic properties for CO oxidation", 《CATALYSIS COMMUNICATIONS》, 12 February 2007 (2007-02-12) * |
| SHAOFANG LI 等: "A novel and sensitive formaldehyde gas sensor utilizing thermal desorption coupled with cataluminescence", 《SENSORS AND ACTUATORS B: CHEMICAL》, 18 November 2009 (2009-11-18) * |
| 杜卫民 等: "LaCoO3 复合氧化物纳米材料的制备及其甲醛敏感性能", 《漯河职业技术学院学报》, 30 September 2008 (2008-09-30) * |
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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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