CN105778895A - Preparation and application of CdS-PAMAM nanocomposite in detecting Cu2+ - Google Patents

Preparation and application of CdS-PAMAM nanocomposite in detecting Cu2+ Download PDF

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CN105778895A
CN105778895A CN201610215546.8A CN201610215546A CN105778895A CN 105778895 A CN105778895 A CN 105778895A CN 201610215546 A CN201610215546 A CN 201610215546A CN 105778895 A CN105778895 A CN 105778895A
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pamam
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CN105778895B (en
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来守军
关晓琳
张东海
靳其军
孟丽
景新颖
常张博
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LANZHOU UNIVERSITY OF ARTS AND SCIENCE
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    • G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/64—Fluorescence; Phosphorescence
    • G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
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Abstract

The invention discloses preparation and application of a CdS-PAMAM nanocomposite in detecting Cu2+, and belongs to the technical field of composites and ion detection.A polyamidoamine (PAMAM) dendrimer is used as a template, CdS is used a light emitting center (chromic nitrate and sodium sulfide are ion sources for synthesizing CdS), and the molecule CdS-PAMAM nanocomposite of a tree structure is synthesized in situ.According to selective testing of the CdS-PAMAM nanocomposite for metal ions, the result proves that the only the addition of copper ions has the remarkable effect on the fluorescence intensity of the composite (fluorescence of the composite is quenched and reduced from 1678 to 957), and the addition of other metal ions will not greatly change fluorescence of the composite.Accordingly, the CdS-PAMAM nanocomposite can be used for copper ions in the specific selectivity fluorescence detection environment.

Description

The preparation of CdS/PAMAM nano composite material and at detection Cu2+In application
Technical field
The present invention relates to the preparation of a kind of CdS/PAMAM nano composite material, the present invention also relates to CdS/PAMAM and receives Nano composite material is at detection Cu2+In application, belong to technical field of composite materials and ion detection technical field.
Background technology
Copper is trace element necessary to animal and plant growth, plays very important work in organism life process With.But the copper of excess not only can bring murder by poisoning to animal and plant growth, also can accumulate in the environment, food chain be enriched with, finally endangers Evil health.Therefore, the detection for copper ion becomes the important indicator in environmental monitoring.Detection copper ion is conventional at present Method has atomic emission spectrometry, atomic absorption spectrography (AAS), electrochemical method and inductivity coupled plasma mass spectrometry (ICP-MS) Etc., but these methods often operate complexity, and need expensive experimental facilities, it is impossible to realize quick detection at the scene. The most quickly detect the content of copper ion in sewage, drinking water, river and organism and just seem particularly significant and urgent.
Quantum dot, is also called nanocrystalline, is a kind of nano-particle elementary composition by II-VI group or iii-v.Quantum dot Particle diameter be typically in the range of between 1 ~ 10nm, owing to electronics and hole are by quantum confinement, continuous print band structure becomes and has molecule The discrete energy levels structure of characteristic, can launch fluorescence after being excited.Based on quantum effect, quantum dot is at solaode, luminous organ The fields such as part, optical bio labelling are with a wide range of applications.From the discovery of quantum dot in 1998, it is applied to many most soon On color fluorescent probe and biological fluorescent labelling.Compared to traditional fluorescent dye, quantum dot shows lot of advantages: wide this Lentor displacement, excitation spectrum wide ranges, optical stability is good, and quantum yield is high, and based on size, launch the adjustable of wavelength Control property etc..Nanocrystalline size, form and surface ligand is all the key factor affecting quantum dot optical property.CdS quasiconductor Nano-cluster has the optical, electrical performance of uniqueness, is used to prepare the window material of solaode.
Polyamide-amide (PAMAM) dendrimer is a kind of typical nano material, multiple in electronic sensor, nanometer Compound, molecular template have good using value.Polyamide-amide (PAMAM) dendrimer surface is by intensive side chain Constitute with group, define nano level cavity at intramolecule so that dendrimer can carry out selectivity as host molecule Ground accommodates guest molecule, and himself also has preferable fluorescence emitting characteristics.The face finish materials such as pamam dendrimer molecule It is not only able to change the electronic state of nano-particle, reactivity, moreover it is possible to strengthen its stability and dispersibility.Solution environmental is the most miscellaneous The photoluminescence performance of quantum dot also can be caused the biggest impact by the factors such as matter metal ion, solvent.Vazquez-Olmos reports In a mild condition, CdS-Cu nanoparticle and 1 and 2.5 PAMAM type dendrimers interact in road Form new complex metal ion, and the existence of metal ion copper can reduce defect and launch, thus be effectively improved band edge and send out Penetrating, the final light that strengthens is stablized and dispersion.Can be monitored by means such as ultraviolet spectra, emission spectrum and electron paramagnetic resonance The carrying out of reaction.
Therefore, CdS quasiconductor is combined with pamam dendrimer molecule, the composite of formation be expected to be used for detect metal from Son.
Summary of the invention
The problem that it is an object of the invention to exist for prior art, it is provided that a kind of can the CdS/ of fluoroscopic examination copper ion PAMAM nano composite material；
It is a further object of the present invention to provide the preparation method of CdS/PAMAM nano composite material；
It is a further aim of the invention provide this CdS/PAMAM nano composite material at detection Cu2+In application.
One, the preparation of CdS/PAMAM nano composite material
Polyamide-amide (PAMAM) is added the methanol solution of chromic nitrate, after logical nitrogen protection stirring 5 ~ 15h, adds sodium sulfide Methanol solution, stirred under nitrogen atmosphere 0.5 ~ 2h, obtain faint yellow clear shape liquid, be CdS/PAMAM nanometer multiple Condensation material.
Polyamide-amide is G3.0, the PAMAM of G3.5, G4.0, G4.5, G5.0.Its synthesis technique is (bent referring now to document Ancient sacrificial bronze ware, Li Jinhuan, Ai Shiyun, the synthesis of dendrimer, dendritic polymer PAMAM and performance study [J] thereof, Journal of Shandong agri.Univ, 2008,39 (3): 429-432.) PAMAM of different algebraically (G3.0, G3.5, G4.0, G4.5, G5.0), has been synthesized.
Polyamide-amide is 1:0.005 ~ 1:0.25 with the mass ratio of chromic nitrate；Polyamide-amide with the mass ratio of sodium sulfide is 1:0.01~1:0.1。
In the methanol solution of chromic nitrate, the content of chromic nitrate is 0.0075 ~ 0.015 mol/L；The methanol of sodium sulfide is molten In liquid, the content of sodium sulfide is 0.0075 ~ 0.015 mol/L.
Two, the sign of CdS/PAMAM nano composite material
1, infrared spectrum analysis
Fig. 1 is CdS/PAMAM nano composite material infrared spectrum.It will be seen from figure 1 that 3.0G ~ 5.0G CdS/PAMAM's is red Outer spectrogram is similar, at 3450cm-1~3250cm-1There is amino (-NH2) absworption peak, but owing to molecular weight is too big, peak shape is wider；Half generation CdS/PAMAM is at 1720cm-1There is the stretching vibration absworption peak of carbonyl in ester group (C=O)；Whole generation CdS/PAMAM is at 1640cm-1Have The stretching vibration absworption peak of carbonyl (C=O) in amido link, at 1560cm-1There is the deformation vibration absworption peak of (N-H) left and right；1240 ~1030cm-1There is primary, secondary, the stretching vibration peak (C-N) of tertiary amine of fat, this absworption peak is more weak.
2, sem analysis
Fig. 2 is the electron-microscope scanning figure of CdS/PAMAM nano composite material, and the most left figure is 8.0 × 10-5 mol/L 4.0G CdS/ The SEM of PAMAM nano composite material, right figure is 8.0 × 10-5 Mol/L 4.0G CdS/PAMAM nano composite material adds 1.0×10-5 mol/L Cu2+SEM.Figure it is seen that 4.0G CdS/PAMAM nano composite material is closelypacked Netted tree structure.It is added thereto to Cu2+After, due to Cu2+The coordination stronger with amino makes tree structure be broken, Tree becomes corynebacterium structure.
3, ultraviolet spectral analysis
Fig. 3 is the uv absorption figure of CdS/PAMAM nano composite material.By ultra-violet analysis, 3.0G～5.0G CdS/P A M All there is maximum absorption band between 240 nm ~ 270 nm in A M nano composite material, increases with its uv absorption of increase of algebraically Add, but the maximum absorption band of 5.0 G CdS/P A M A M nano composite materials reduces on the contrary.This is because near ultraviolet-visible The feature of the spectral absorption peak reflection conjugated electrons in district, the conjugated degree of condensation polymer and absorption have certain relation, different polymer Middle electron delocalization degree is different, causes uv absorption intensity different.
4, thermogravimetric (TG) is analyzed
Fig. 4 is the thermogravimetric collection of illustrative plates (TG) of CdS/PAMAM nano composite material.Analyzed it can be seen that CdS/ by thermogravimetric (TG) PAMAM nano composite material is when 800 DEG C, and 3.0G CdS/PAMAM nano composite material only has 3% because molecule is smaller Residue, other have 20% ~ 30% residue, illustrate that CdS has well loaded on PAMAM.
Three, CdS/PAMAM nano composite material application in detection copper ion
1, the fluorescence response performance to metal ion
Take 1mL 8.0 × 10-4Mol/L CdS/PAMAM nano composite material, adds 1mL1.0 × 10-4 Cu2+Solution, dilution Fluorometric investigation is carried out to 10 mL.Fig. 5 is the CdS/PAMAM nano composite material difference algebraically response diagram to metal copper ion.By Fig. 5 is it is found that whole generation CdS/PAMAM nano composite material is to Cu2+Response than half Dai Qiang, 4.0G CdS/ in the most whole generation PAMAM nano composite material is to Cu2+Response is the strongest, and 4.0G CdS/PAMAM nano composite material fluorescence is the strongest, so Choose 4.0G CdS/PAMAM nano composite material and carry out Cu at optimum conditions2+Detection.
2, the selectivity to different metal ion
Investigate the impact for the photoluminescent property of composite nano materials of the different metal ion, i.e. selectivity to investigate.First prepare Pb2+、 Hg2+、Cu2+、Mn2+、Ni2+、Zn2+、Ag+、Na+、K+、Cr3+Deng the solution of metal ion, concentration is 1 × 10-6 mol/L.Take CdS/PAMAM nano composite material 0.5mL, is separately added into above-mentioned different metal ion 0.1 mL, dilutes with redistilled water To 5.0mL.Set excitation wavelength as 362nm, a length of 470nm of transmitted wave, measure the fluorescence after composite adds metal ion Intensity.Fig. 6 is the CdS/PAMAM nano composite material selectivity to metal ion.Shown by the measurement result of Fig. 6, only copper The adding of ion (fluorescent quenching making composite) is had a significant impact for the fluorescence intensity of composite (to drop to from 1678 957).High valence ion Cr3+Though addition have certain impact (dropping to 1540 from 1678), but consider chromium ion in actual sample Often differ greatly with the ion concentration coexisted of copper ion, do not interfere with the Copper Ion of actual sample.Therefore, CdS/ PAMAM nano composite material can be used for the copper ion in single-minded selectivity fluoroscopic examination environment.
Accompanying drawing explanation
Fig. 1 is CdS/PAMAM nano composite material infrared spectrum.
Fig. 2 is the electron-microscope scanning figure of CdS/PAMAM nano composite material.
Fig. 3 is the uv absorption figure of CdS/PAMAM nano composite material
Fig. 4 is the thermogravimetric collection of illustrative plates (TG) of CdS/PAMAM nano composite material.
Fig. 5 is the CdS/PAMAM nano composite material difference algebraically response diagram to metal copper ion.
Fig. 6 is the CdS/PAMAM nano composite material selectivity to metal ion.
Fig. 7 is that 4.0G CdS/PAMAM nano composite material is to Cu2+Response fluorescent emission spectrogram.
Fig. 8 is that 4.0G CdS/PAMAM nano composite material is to Cu2+Response linear relation.
Fig. 9 is that 4.0G CdS/PAMAM nano composite material is to Cu in tap water2+Fluoremetry.
Detailed description of the invention
Below by specific embodiment to the preparation of CdS/PAMAM nano composite material of the present invention and detection copper from Application in son is described further.
1, the preparation of the tree-shaped nano composite material of CdS/PAMAM
(1) weigh 0.5860 g chromic nitrate, be settled to 250 mL with methanol as solvent, be made into the methanol solution of chromic nitrate (0.009932 mol/L)；
(2) weigh 0.2480 g nine hydrated sodium sulfide, be settled to 100 mL with methanol as solvent, be made into the methanol of sodium sulfide Solution (0.01033 mol/L)；
(3) 100mL 0.0004 mol/L 4.0G PAMAM and 20 mL(0.009932 mol/L is taken) methanol of chromic nitrate is molten Liquid, after logical nitrogen protection stirring 10 h, adds 10 mL(0.01022 mol/L) methanol solution of sodium sulfide, under nitrogen protection Quickly stir 1h, obtain faint yellow clear shape liquid, obtain the tree-shaped nano composite material of CdS/PAMAM.
2, the application in detection copper ion
Take 0.5 mL 8 × 10 respectively-4Mol/L 4.0G CdS/PAMAM nano composite material, in 10 color comparison tubes, adds respectively Enter 0,0.05mL, 0.10mL, 0.15mL, 0.20mL, 0.25mL, 0.30mL, 0.35mL, 0.40mL, 0.45mL, 0.50 mL 1 ×10-6mol/L Cu2+Solution, is diluted to 4.0G CdS/PAMAM in 10 mL(gained solution with redistilled water nano combined The concentration of material is 8 × 10-5 Mol/L, Cu2+Concentration is respectively 0, and 1 × 10-8, 2 × 10-8, 3 × 10-8, 4 × 10-8, 5 × 10-8, 6×10-8, 7 × 10-8, 8 × 10-8, 9 × 10-8, 1 × 10-7 Mol/L), fluorometric investigation is carried out.Find that 4.0G CdS/PAMAM receives Nano composite material is to Cu2+Respond and present good linear relationship: y=-7.5 × 109X+1701, y: fluorescence intensity level, x:Cu2+ Concentration value mol/L.
According to linear relationship to the Cu in tap water2+Detect, take 0.5 mL8 × 10 respectively-4The 4.0G of mol/L CdS/PAMAM nano composite material, in 6 color comparison tubes, is separately added into tap water and takes 0.1 mL, 0.2 mL, 0.4 mL respectively, 0.6 mL, 0.8 mL tap water is made into 5 mL solution, carries out fluorometric investigation, calculates Cu according to fluorescence intensity level2+Concentration.Result is shown in Table 1.When being 0.1 mL due to tap water, record Cu2+Concentration values and other numerical bias are relatively big, therefore cast out.By remaining copper from Sub-concentration value is averaged, and records Cu after in tap water2+Concentration is 6.75 × 10-7 Mol/L, the response rate is 95% ~ 102%.
Table 1 4.0G CdS/PAMAM composite add after the tap water of different volumes in fluorescence intensity and tap water Cu2+The mensuration analysis of concentration:
。

Claims (9)

1. a preparation method for CdS/PAMAM nano composite material, is the methanol solution that polyamide-amide adds chromic nitrate, After logical nitrogen protection stirring 5 ~ 15 h, add the methanol solution of sodium sulfide, stirred under nitrogen atmosphere 0.5 ~ 2h, obtain faint yellow Clear shape liquid, the CdS/PAMAM nano composite material being.
2. the preparation method of CdS/PAMAM nano composite material as claimed in claim 1, it is characterised in that: polyamide-amide is generation Number G3.0, the PAMAM of G3.5, G4.0, G4.5, G5.0.
3. the preparation method of CdS/PAMAM nano composite material as claimed in claim 1, it is characterised in that: polyamide-amide and nitre The mass ratio of acid chromium is 1:0.01 ~ 1:0.2.
4. the preparation method of CdS/PAMAM nano composite material as claimed in claim 1, it is characterised in that: polyamide-amide and sulfur The mass ratio changing sodium is 1:0.01 ~ 1:0.1.
5. the preparation method of CdS/PAMAM nano composite material as claimed in claim 1, it is characterised in that: the methanol of chromic nitrate In solution, the content of chromic nitrate is 0.009 ~ 0.010 mol/L.
6. the preparation method of CdS/PAMAM nano composite material as claimed in claim 1, it is characterised in that: the methanol of sodium sulfide In solution, the content of sodium sulfide is 0.009 ~ 0.011 mol/L.
7. the CdS/PAMAM nano composite material that as claimed in claim 1 prepared by method application in detection copper ion.
8. CdS/PAMAM nano composite material application in detection copper ion as claimed in claim 7, it is characterised in that: In CdS/PAMAM nano composite material, only copper ion adds and makes the fluorescence generation quencher of composite, and other metal ion Addition will not make the fluorescence of composite that big change occurs.
9. CdS/PAMAM nano composite material application in detection copper ion as claimed in claim 7, it is characterised in that: The fluorescence intensity of CdS/PAMAM nano composite material and Cu2+Concentration is presented below as linear relationship:
y=-7.5×109X+1701, y: fluorescence intensity level, x:Cu2+Concentration value mol/L.
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