CN102051047A - Method for preparing carbon nitride tube-polyaniline-gold composite material and application method thereof - Google Patents
Method for preparing carbon nitride tube-polyaniline-gold composite material and application method thereof Download PDFInfo
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- CN102051047A CN102051047A CN 201010551737 CN201010551737A CN102051047A CN 102051047 A CN102051047 A CN 102051047A CN 201010551737 CN201010551737 CN 201010551737 CN 201010551737 A CN201010551737 A CN 201010551737A CN 102051047 A CN102051047 A CN 102051047A
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- polyaniline
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Abstract
The invention discloses a method for preparing a carbon nitride tube-polyaniline-gold composite material and an application method thereof. The method comprises the following steps: the acidified carbon nitride tube solution is alternatively treated by aqueous solutions, in which polydiene propyl dimethyl ammonium chloride and polystyrene sodium sulfonate sodium chloride serve as solutes respectively, and is then dissolved in hydrochloric acid solution; aniline monomer is added into the mixed solution, and hydrochloric acid solution serving as an oxidant and containing ammonium persulphate is added after the carbon nitride tube solution and the hydrochloric acid solution are uniformly mixed; carbon nitride tube-polyaniline is gained by washing, centrifuging and drying a reaction product obtained after the carbon nitride tube solution is reacted with the ammonium persulphate for 24 hours, and is dispersed in gold colloid; and carbon nitride tube-polyaniline-gold is obtained by centrifuging and drying a reaction product obtained after the carbon nitride tube-polyaniline is reacted with the gold colloid for 30 minutes. The pipe diameter of the two prepared composite materials is 60 nm, the carbon nitride tube-polyaniline and a modified electrode compose a dopamine biosensor, the detectability of the dopamine biosensor is 0.01 MuM, and the linearity range of the dopamine biosensor is 1-80 MuM and 1.5-3.5 mM. The carbon nitride tube-polyaniline-gold and a modified electrode compose a peroxide biosensor, the detectability of the peroxide biosensor is 1.4 MuM, and the linearity range of the peroxide biosensor is 0.02-2.05 mM.
Description
Technical field
The present invention relates to the synthetic and application in biosensor of carbon nitrogen pipe/polyaniline and carbon nitrogen pipe/polyaniline/metal/composite material.Specifically, be carbon nitrogen pipe/polyaniline and carbon nitrogen pipe/polyaniline/metal/composite material, and made up Dopamine HCL and biosensor of hydrogen peroxide with the self-assembly method preparation.
Background technology
The development new bio transmitter that synthesizes of novel nano-material provides new approach.Carbon nanomaterial is a kind of ideal electrode materials, the carbon modified electrode has lot of advantages, as: the time of response is fast, specific conductivity is high, good biocompatibility etc. [referring to Alwarappan S, Erdem A, Liu C and Li C 2009 J.Phys.Chem.C 113 8853].Wherein, carbon nanotube is because its particular structure and peculiar physics, chemistry, mechanical characteristic and potential application prospect thereof have attracted numerous researchers that its structure, character and application are studied [referring to (a) Boussaad S, Tao N J, Hopson T and Nagahara L A 2003 Chem.Commun.1502; (b) He P G.and Dai L M 2004 Chem.Commun.3 348; (c) Lee D, Lee J, Kim J, Kim J, Na H B, Kim B, Shin C-H, Kwak J H, Dohnalkova A, Grate J W, Hyeon T and Kim H-S 2005 Adv.Mater.17 2828], existing not major general's carbon nanotube is used for the report of biosensor research [referring to (a) Katz E and Willner I 2004 Angew.Chem.Int.Ed.43 6042; (b) Zayats M, Katz E, Baron R and Willner I 2005 J.Am.Chem.Soc.127 12400].But because carbon nanotube poorly soluble, can have influence on the preparation of transmitter and circulation ratio [referring to Salimi A, Compton RG and Hallaj R2004 Anal.Biochem.333 49].Compare with traditional carbon pipe, nitrogen doped carbon nanotubes (carbon nitrogen pipe) has more avtive spot, good biocompatibility and catalytic performance, thereby makes it have more wide application prospect at biological field.Because the existence of C-N active sites, make the easier acquisition functional composite material that combines with other material of carbon nitrogen pipe, thereby widen its range of application [referring to Jiang K, Eitan A, Schadler L S, AjayanP M and Siegel R W 2003 Nanoletters 3 275].
Polyaniline (PANI) mainly is because it has high specific conductivity as one of most important conducting polymer, easily preparation, good advantages such as environmental stability with and use widely.Because the doping that the doping level of PANI can be by acid and the process of dedoping is controlled thereby be unique in conjugated highpolymer.But PANI is usually under acidic conditions, generally is that pH＜4 o'clock just have redox active [referring to Tian S J, Liu J Y, ZhuT and Knoll W 2004 Chem.Mater.16 4103].This has just limited its application in biosensor greatly, because this needs neutrallty condition usually.
The Organic of being made up of different components has special physicochemical character and potential application prospect and causes widely in scientific circles and to pay close attention to.The existing report of mixture [Liu J, Tian S and Knoll W 2005 Langmuir 21 5596] about polyaniline and carbon nanotube.
In addition, receive much concern owing to the unique electricity of golden nanometer particle and optical property and widespread use in multiple field.Relevant PANI/Au nano composite material also has report [Peng Z more, Guo L, Zhang Z, Tesche B, Wilke T, Ogermann D, Hu S and Kleinermanns K 2006 Langmuir 2210915], but, have the carbon nitrogen pipe/polyaniline of high electrochemical activity and the carbon nitrogen pipe/polyaniline/report of gold nano matrix material also seldom, particularly its application in biosensor.
Summary of the invention
Technical problem: the purpose of this invention is to provide the synthetic method of the carbon nitrogen pipe/polyaniline and the carbon nitrogen pipe/polyaniline/gold nano matrix material of high electrochemical activity, make up the method for Dopamine HCL and hydrogen peroxide sensor.
Technical scheme: the synthetic method of carbon nitrogen pipe/polyaniline of the present invention and carbon nitrogen pipe/polyaniline/gold nano matrix material is:
At first the carbon nitrogen pipe solution of acidifying is used the NaCl aqueous solution alternate treatment of diallyl dimethyl ammoniumchloride (PDDA) and sodium polystyrene sulfonate (PSS) respectively, be dissolved in the hydrochloric acid soln then, add aniline monomer, the hydrochloric acid soln that adds the oxygenant ammonium persulphate after stirring, react after 24 hours, obtain carbon nitrogen pipe/polyaniline through washing, centrifugal, oven dry; Carbon nitrogen pipe/polyaniline is distributed in the gold size, stirred 30 minutes, centrifugal, oven dry obtains carbon nitrogen pipe/polyaniline/gold.
The carbon nitrogen pipe solution of described acidifying, wherein the carbon nitrogen pipe of acidifying: water=2mg: 1mL.
The NaCl aqueous solution of described PDDA, wherein PDDA: NaCl: water=10mg: 29mg: 1mL.
The NaCl aqueous solution of described PSS, wherein PSS: NaCl: water=10mg: 29mg: 1mL.
The consumption of described aniline monomer is 10 μ L.
The hydrochloric acid soln of described ammonium persulphate, wherein ammonium persulphate: hydrochloric acid: water=4.8mg: 36.5mg: 1mL.
Carbon nitrogen pipe/polyaniline is used for modified electrode, makes up the biosensor of Dopamine HCL, and this biosensor detects and is limited to 0.01 μ M, linearity range: 1-80 μ M and 1.5-3.5mM.Carbon nitrogen pipe/polyaniline/gold is used for modified electrode, makes up biosensor of hydrogen peroxide, and this sensor detecting is limited to 1.4 μ M, linearity range: 0.02-2.05mM.
Beneficial effect: the method raw material for preparing carbon nitrogen pipe/polyaniline and carbon nitrogen pipe/polyaniline/gold nano matrix material of the present invention be simple and easy to, mild condition.The electrochemical activity of product is very high, and the biosensor of preparation is highly sensitive, stability and favorable reproducibility, and immunity from interference is strong.
Description of drawings
Fig. 1 is the cyclic voltammogram of carbon nitrogen pipe/polyaniline nano-composite material of the present invention;
Fig. 2 is the cyclic voltammogram of carbon nitrogen pipe/polyaniline of the present invention/gold nano matrix material;
Fig. 3 is the time current curve of hydrogen peroxide sensor of the present invention.
Fig. 4 is the time current curve of Dopamine HCL biosensor of the present invention.
Embodiment
The method for preparing carbon nitrogen pipe/polyaniline and carbon nitrogen pipe/polyaniline/gold nano matrix material, carbon nitrogen pipe and acidification thereof are synthetic [referring to Chen H, Yang Y, Hu Z according to literature method, Huo K F, Ma Y W and ChenY 2006 J.Phys.Chem.B 110 16422].Carbon nitrogen pipe (2mg/mg) 5mL of acidifying is dissolved in 10mLNaCl (0.5M) aqueous solution of 1% diallyl dimethyl ammoniumchloride (PDDA), stir after 20 minutes, washing, be dissolved in again in 10mLNaCl (0.5M) aqueous solution of 1% sodium polystyrene sulfonate (PSS), restir 20 minutes, washing is dissolved in after the separation in the HCl solution of 1mol/L, adds aniline monomer 10 μ L, stir after 30 minutes, add the 1mol/L hydrochloric acid soln 5mL that contains 24.38mg oxygenant ammonium persulphate, react after 24 hours, through washing, centrifugal, oven dry obtains carbon nitrogen pipe/polyaniline, and carbon nitrogen pipe/polyaniline is scattered in the gold size, and gold size is according to synthetic [the Yan W of literature method, Feng X M, Chen X J, Hou W H and Zhu J-J 2008Biosens.Bioelectron.23 925], obtain carbon nitrogen pipe/polyaniline/gold nano nano composite material.
Respectively 5 μ L carbon nitrogen pipe/polyanilines and carbon nitrogen pipe/polyaniline/Jinsui River solution (2mg/mL) are dripped and be coated onto electrode surface, after room temperature is dried, make Dopamine HCL and biosensor of hydrogen peroxide.
Carbon nitrogen pipe/polyaniline and carbon nitrogen pipe/polyaniline/gold nano matrix material in a tubular form, the mean diameter of golden nanometer particle is distributed on the tube wall at 5nm, the about 60nm of caliber.The biosensor of the Dopamine HCL that makes up detects and is limited to 0.01 μ M, linearity range: 1-80 μ M and 1.5-3.5mM; The biosensor of hydrogen peroxide that makes up detects and is limited to 1.4 μ M, linearity range: 0.02-2.05mM; Stability and circulation ratio are better.
The preparation of embodiment 1. carbon nitrogen pipe/polyaniline nano-composite materials
Carbon nitrogen pipe and acidification thereof are according to literature method synthetic [referring to Chen H, Yang Y, Hu Z, Huo K F, Ma Y W and Chen Y 2006 J.Phys.Chem.B 110 16422].Carbon nitrogen pipe (2mg/mg) 5mL of acidifying is dissolved in 10mLNaCl (0.5M) aqueous solution of 1% diallyl dimethyl ammoniumchloride (PDDA), stir after 20 minutes, washing, be dissolved in again in 10mLNaCl (0.5M) aqueous solution of 1% sodium polystyrene sulfonate (PSS), restir 20 minutes, washing, be dissolved in after the separation in the HCl solution of 1mol/L, add aniline monomer 10 μ L, stir after 30 minutes, add the 1mol/L hydrochloric acid soln 5mL that contains 24.38mg oxygenant ammonium persulphate, react after 24 hours, through washing, centrifugal, oven dry obtains carbon nitrogen pipe/polyaniline.
The preparation of embodiment 2. carbon nitrogen pipe/polyaniline/gold nano matrix materials
Carbon nitrogen pipe/polyaniline is scattered in the gold size, gold size is according to literature method synthetic [Yan W, Feng X M, Chen X J, Hou W H and Zhu J-J 2008 Biosens.Bioelectron.23 925], obtain carbon nitrogen pipe/polyaniline/gold nano nano composite material.
The electrochemical activity test of embodiment 3. carbon nitrogen pipe/polyanilines and carbon nitrogen pipe/polyaniline/gold nano matrix material
Is pH from 1～8 phosphoric acid hydrochlorate buffered soln with carbon nitrogen pipe/polyaniline and carbon nitrogen pipe/polyaniline/golden modified electrode at electrolytic solution, and potential window is-0.4-0.8v to sweep speed for carrying out the cyclic voltammetric test under the situation of 100mV/s.
The preparation of embodiment 4. Dopamine HCL biosensors
5 μ L carbon nitrogen pipe/polyaniline aqueous solution (2mg/mL) are dripped be coated onto electrode surface, after room temperature is dried, make the Dopamine HCL biosensor.
The preparation of embodiment 5. hydrogen peroxide sensors
5 μ L carbon nitrogen pipe/polyaniline/Jinsui River solution (2mg/mL) are dripped be coated onto electrode surface, after room temperature is dried, make hydrogen peroxide and get biosensor.
The detection of 6. pairs of Dopamine HCLs of embodiment
Electrolytic solution is the phosphoric acid hydrochlorate buffered soln of pH=7, and the detection current potential is 0.4V, and the Dopamine HCL that adds different concns continuously carries out the ampere experiment.
The detection of 7. pairs of hydrogen peroxide of embodiment
Electrolytic solution is the phosphoric acid hydrochlorate buffered soln of pH=7, detects current potential to be-0.18V, and the hydrogen peroxide that adds different concns continuously carries out the ampere experiment.
Anti-interference, the circulation ratio of embodiment 5. biosensors and stability
At electrolytic solution is the phosphoric acid hydrochlorate buffered soln of pH=7, is that the concentration of hydrogen peroxide is 0.1mM H under the situation of 100mV/s sweeping speed
2O
2, or dopamine concentration is that the uric acid of 10 μ M and xitix are for the influence of peak current under the 20 μ M situations; The biosensor for preparing a plurality of different electrodes is investigated circulation ratio; In the refrigerator of 4 degree, placed 1 month, investigate stability.
Claims (7)
1. the synthetic method of carbon nitrogen pipe-polyaniline-gold nano matrix material, it is characterized in that this method is: the NaCl aqueous solution alternate treatment of at first the carbon nitrogen pipe solution of acidifying being used diallyl dimethyl ammoniumchloride and sodium polystyrene sulfonate respectively, be dissolved in the hydrochloric acid soln then, add aniline monomer, the hydrochloric acid soln that adds the oxygenant ammonium persulphate after stirring, react after 24 hours, through washing, centrifugal, oven dry obtains carbon nitrogen pipe-polyaniline, carbon nitrogen pipe-polyaniline is distributed in the gold size, stirred 30 minutes, centrifugal, oven dry obtains carbon nitrogen pipe-polyaniline-Jin.
2. the synthetic method of carbon nitrogen pipe-polyaniline according to claim 1-gold nano matrix material is characterized in that in the carbon nitrogen pipe solution of described acidifying the carbon nitrogen pipe of acidifying: water=2mg: 1mL.
3. the synthetic method of carbon nitrogen pipe-polyaniline according to claim 1-gold nano matrix material is characterized in that in the NaCl aqueous solution of described PDDA PDDA: NaCl: water=10mg: 29mg: 1mL.
4. the synthetic method of carbon nitrogen pipe-polyaniline according to claim 1-gold nano matrix material is characterized in that in the NaCl aqueous solution of described PSS PSS: NaCl: water=10mg: 29mg: 1mL.
5. the synthetic method of carbon nitrogen pipe-polyaniline according to claim 1-gold nano matrix material, the consumption that it is characterized in that described aniline monomer are 10 μ L.
6. the synthetic method of carbon nitrogen pipe-polyaniline according to claim 1-gold nano matrix material is characterized in that in the hydrochloric acid soln of described ammonium persulphate ammonium persulphate: hydrochloric acid: water=4.8mg: 36.5mg: 1mL.
7. the application method of carbon nitrogen pipe-polyaniline-gold nano matrix material, it is characterized in that this nano composite material is used for modified electrode, biosensor with carbon nitrogen pipe-polyaniline modified electrode structure Dopamine HCL detects and is limited to 0.01 μ M, linearity range: 1-80 μ M and 1.5-3.5mM; Carbon nitrogen pipe/polyaniline/golden modified electrode is made up biosensor of hydrogen peroxide, detect and be limited to 1.4 μ M, linearity range: 0.02-2.05mM; Stability and circulation ratio are better.
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| CN102520187A (en) * | 2011-11-23 | 2012-06-27 | 江南大学 | Manufacture method and application of immune sensor based on polyaniline nano-particle composite membrane |
| CN102645461A (en) * | 2012-03-31 | 2012-08-22 | 无锡百灵传感技术有限公司 | Preparation method of electrochemical sensor based on polyaniline nanofiber |
| CN104297479A (en) * | 2014-09-24 | 2015-01-21 | 济南大学 | Preparation method and application of electrochemiluminescence immunoassay sensor for detecting tumor marker |
| CN108587159A (en) * | 2018-05-11 | 2018-09-28 | 东南大学 | One type graphene carbonitride/ferroso-ferric oxide/polyaniline nano composite wave-suction material and preparation method thereof |
| CN115746296A (en) * | 2022-11-11 | 2023-03-07 | 浙江大学杭州国际科创中心 | Three-dimensional mesoporous gold nanoparticle modified polyaniline nanowire array/carbon nanotube composite material and preparation method and application thereof |
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| CN102520187A (en) * | 2011-11-23 | 2012-06-27 | 江南大学 | Manufacture method and application of immune sensor based on polyaniline nano-particle composite membrane |
| CN102520187B (en) * | 2011-11-23 | 2014-06-18 | 江南大学 | Manufacture method and application of immune sensor based on polyaniline nano-particle composite membrane |
| CN102645461A (en) * | 2012-03-31 | 2012-08-22 | 无锡百灵传感技术有限公司 | Preparation method of electrochemical sensor based on polyaniline nanofiber |
| CN104297479A (en) * | 2014-09-24 | 2015-01-21 | 济南大学 | Preparation method and application of electrochemiluminescence immunoassay sensor for detecting tumor marker |
| CN108587159A (en) * | 2018-05-11 | 2018-09-28 | 东南大学 | One type graphene carbonitride/ferroso-ferric oxide/polyaniline nano composite wave-suction material and preparation method thereof |
| CN108587159B (en) * | 2018-05-11 | 2020-08-14 | 东南大学 | Graphene-like carbon nitride/ferroferric oxide/polyaniline nano composite wave-absorbing material and preparation method thereof |
| CN115746296A (en) * | 2022-11-11 | 2023-03-07 | 浙江大学杭州国际科创中心 | Three-dimensional mesoporous gold nanoparticle modified polyaniline nanowire array/carbon nanotube composite material and preparation method and application thereof |
| CN115746296B (en) * | 2022-11-11 | 2024-04-05 | 浙江大学杭州国际科创中心 | Three-dimensional mesoporous gold nanoparticle modified polyaniline nanowire array/carbon nanotube composite material, and preparation method and application thereof |
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