CN106544012B - The synthesis of water soluble fluorescence nano silicon particles and application of highly selective measurement trace TNP - Google Patents
The synthesis of water soluble fluorescence nano silicon particles and application of highly selective measurement trace TNP Download PDFInfo
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- CN106544012B CN106544012B CN201610964476.6A CN201610964476A CN106544012B CN 106544012 B CN106544012 B CN 106544012B CN 201610964476 A CN201610964476 A CN 201610964476A CN 106544012 B CN106544012 B CN 106544012B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/06—Luminescent, e.g. electroluminescent, chemiluminescent materials containing organic luminescent materials
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic System
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/18—Compounds having one or more C—Si linkages as well as one or more C—O—Si linkages
- C07F7/1804—Compounds having Si-O-C linkages
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F7/00—Compounds containing elements of Groups 4 or 14 of the Periodic System
- C07F7/02—Silicon compounds
- C07F7/08—Compounds having one or more C—Si linkages
- C07F7/18—Compounds having one or more C—Si linkages as well as one or more C—O—Si linkages
- C07F7/1804—Compounds having Si-O-C linkages
- C07F7/1872—Preparation; Treatments not provided for in C07F7/20
- C07F7/1892—Preparation; Treatments not provided for in C07F7/20 by reactions not provided for in C07F7/1876 - C07F7/1888
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- 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"
- G01N21/643—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes" non-biological material
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
- 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"
- G01N2021/6432—Quenching
Abstract
The invention discloses a kind of new methods of water soluble fluorescence nano silicon particles (SiNPs) prepared with one kettle way high sensitivity and highly selective measurement 2,4,6- trinitrophenol (TNP) in water phase.At optimum conditions, the range of linearity of this method measurement TNP is 0.02-120mg/L, and linear equation is that detection is limited to 6.7 μ g/L.On this basis, it is prepared for can be used for the test paper of Visual retrieval TNP.
Description
Technical field
The invention belongs to chemical fields, and in particular to a kind of water solubility for detecting 2,4,6- trinitrophenols (TNP)
The synthetic method and its application of fluorescent nano particle.
Background technique
TNP also known as picric acid (PA), are a kind of nitryl aromatic explosives with strong electron-withdrawing group, and brisance is big
In 2,4,6- trinitrotoluene (TNT).TNP is widely used in dye industry, rocket fuel, pyrotechnics, drug and laboratory.
Its permissible value in drinking water is 0.5mg/L, and acceptable daily intake (ADI) is 1-37 μ g/ (kg per day).Therefore,
It largely can serious contaminated soil and surface water using TNP.It can cause skin mistake when people suck, swallow or largely contact TNP
The symptoms such as quick, anaemia, cancer, dysfunction of liver and respiratory system be impaired.In view of TNP to the serious pollution of environment and to the mankind
The threat of health, sensitive and selective enumeration method TNP have caused the extensive concern of people.In addition, nitryl aromatic explosive is such as
Dinitrotoluene (DNT) (DNT), nitrobenzene (NB) and TNT have interference to detection TNP.Since TNP and TNT have very strong electricity
Sub- affinity, TNT are particularly evident to the interference of detection TNP.So in the mixture of nitryl aromatic explosive detect TNP at
For a challenging task.So far, the method for detecting nitryl aromatic explosive mainly has surface-enhanced Raman light
Spectrum, high performance liquid chromatography, dynamic light scattering, solid phase microextraction-ion mobility spectrometry, electrochemistry and ELISA.On but
Stating method, there are some disadvantages, and such as Gao Chengben, instrumentation is complicated, extraction process is long and indistinguishable TNP and TNT, these
Disadvantage limits their extensive use.In contrast, fluorescence analysis method it is highly sensitive, highly selective, easy to operate with it,
The advantages that real-time detection, low cost and portability, causes the extensive concern of people and to establish a series of detection nitryl aromatics quick-fried
The fluorescence analysis method of fried object, as ZnS:Mn2+@allyl sulfhydrate nano-complex method, 8-hydroxyquinoline aluminium nanosphere method,
Graphene carbonitride (g-C3N4) method, metal organic frame (MOF) method based on Cd (II) and N doping carbon dots method etc..But
There are nano material synthesis, and time-consuming multistep reaction, material preparation, toxicity height and use to be needed to have when detecting TNP for above method
Solvent etc., these disadvantages limit the extensive use of these materials.Meanwhile for the safe examination system of various public places and
Speech remains a problem for whether containing TNP in suspicious item, is difficult have direct method quickly to examine.Therefore, develop one
The method of simple, harmless, the highly sensitive and selective detection aqueous solution TNP of kind is very necessary.
Summary of the invention
It is an object of the invention to:
Simple, time saving synthesis is established with toxicity is low, has good stability, the excellent water solubility SiNPs new method of optical property；
Synthesize the fluorescence SiNPs that TNP is detected in water phase；On this basis, detection is established using the excellent properties of fluorescence SiNPs
TNP fluorescence new method and the fluorescence SiNPs test paper for preparing detection TNP.
The present invention is realized by following steps:
(1) synthesis of SiNPs
A, deionized water is added in round-bottomed flask, DAMO is added in whipping process, catechol is then added, sufficiently
Stirring.
B, said mixture solution is transferred in polytetrafluoroethylene (PTFE) autoclave, 200 DEG C of whens react 4h, natural cooling
To room temperature.
C, the SiNPs solution prepared is dialysed 6h in the bag filter of 1000Da (molecular weight cutoff).
D, by the SiNPs solution storage dialysed in 4 DEG C of refrigerator to be used for subsequent detection.
Further, N- (2- aminoethyl) -3- aminopropyl trimethoxysilane and catechol molar ratio are as follows: 9.3:100.
(2) it is characterized with the structure of the methods of XPS, FT-IR to SiNPs.
(3) to the thermal stability of SiNPs, anti-light Bleachability, salt tolerance and different pH value fluorescence intensity when is examined
It examines.It determines determination condition, establishes the fluorescence SiNPs test paper of the method for measuring TNP in water phase, preparation detection TNP.
(4) in aqueous solution TNP measurement
(a) SiNPs solution PBS (pH=7.4) buffer solution prepared is diluted 1000 times；In SiNPs weak solution
The middle TNP solution that various concentration is added, places 1min；It is strong that fluorescence is surveyed when excitation wavelength is 430nm, and launch wavelength is 512nm
Degree；The slit width of excitation wavelength and launch wavelength is 5nm.
(b) SiNPs measures the selectivity of TNP as follows: a certain concentration is added in 3mL SiNPs weak solution
Inorganic ionic solution or nitryl aromatic explosive solution；According to the parametric measurement fluorescence intensity set in (a).All experiments are equal
It carries out at room temperature.
(5) preparation of fluorescent test paper strip and the Visual retrieval to TNP
(a) quantitative filter paper is immersed in the SiNPs solution for diluting 2.5 times with PBS (pH=7.4) buffer solution；It impregnates
It is after 20min, filter paper is dry in the baking oven for be placed in 50 DEG C from pipetting out in solution；It, will after filter paper cooled to room temperature
Filter paper is cut into test paper.
(b) the TNP solution that 10 μ L various concentrations are instilled in the test strips prepared will try after solvent natural evaporation
The color change that paper slip is placed in observation filter paper item under the ultraviolet lamp of 365nm determines that TNP whether there is.Above-mentioned experiment is at room temperature
It carries out.
Benefit of the invention is that:
This preparation method is easy to operate, time saving, and prepared SiNPs has good thermal stability, stronger salt tolerance
With excellent anti-light bleaching power；The method choice of TNP is good in the measurement water sample established, high sensitivity；The fluorescence of preparation
Test paper can be used for the Visual retrieval of TNP.In the present invention, it is utilized respectively N- (2- aminoethyl) -3- aminopropyl trimethoxy silicon
Alkane (DAMO) and catechol are that silicon source and reducing agent have synthesized water-soluble fluorescence SiNPs.Compared with existing method, the party
Method avoids multistep and time-consuming material preparation process.The SiNPs of this method preparation has good thermal stability, and excellent is anti-
Photobleaching ability and salt tolerance, quantum yield 7.1%.The fluorescence of SiNPs is quenched after TNP is added, and mechanism is quenched and is
Interior filtering effect (IFE).On this basis, the present invention establishes a kind of detection TNP highly sensitive and highly selective in water phase
New method.It is also prepared for a kind of fluorescence SiNPs test paper for detecting TNP simultaneously.
Detailed description of the invention
The infrared spectrogram of Fig. 1 SiNPs.
The x-ray photoelectron spectroscopy figure of Fig. 2 SiNPs.
Influence of Fig. 3 temperature to SiNPs normalization fluorescence intensity.
The influence of Fig. 4 inorganic ions (A) and nitryl aromatic explosive (B) to detection TNP.
Influence of Fig. 5 (a) TNP concentration to SiNPs test paper fluorescence intensity；(b) other nitryl aromatic explosive mixtures are dense
Spend the influence to SiNPs test paper fluorescence intensity；(c) TNP and other nitryl aromatic explosive mixture concentrations are glimmering to SiNPs test paper
The influence of luminous intensity；Concentration is from left to right followed successively by 0,0.01,0.05,0.1,0.5,1.0mg/mL.
The measurement result of TNP in Fig. 6 nitryl aromatic explosive.The concentration of TNP is 1mg/L；Nitryl aromatic explosive DNB,
The concentration of DNBA, DNT, NB, NT and TNT are 5mg/L (NAE represents nitryl aromatic explosive mixture in figure).
Specific embodiment
Embodiment 1
50mL deionized water is added in 100mL round-bottomed flask, 5mL DAMO is added in whipping process, is then added
25mg catechol after 1min is sufficiently stirred, said mixture solution is transferred in polytetrafluoroethylene (PTFE) autoclave, 200
DEG C when react 4h, cooled to room temperature.Then by the SiNPs solution prepared 1000Da (molecular weight cutoff) bag filter
Middle dialysis 6h.Finally, by the SiNPs solution storage dialysed to be used for subsequent detection in 4 DEG C of refrigerator.N- (2- ammonia second
Base) -3- aminopropyl trimethoxysilane and catechol optimum molar ratio are as follows: 9.3:100.
Embodiment 2
50mL deionized water is added in 100mL round-bottomed flask, 2mL DAMO is added in whipping process, is then added
11mg catechol after 1min is sufficiently stirred, said mixture solution is transferred in polytetrafluoroethylene (PTFE) autoclave, 200
DEG C when react 4h, cooled to room temperature.Then by the SiNPs solution prepared 1000Da (molecular weight cutoff) bag filter
Middle dialysis 6h.Finally, by the SiNPs solution storage dialysed to be used for subsequent detection in 4 DEG C of refrigerator.
Embodiment 3
30mL deionized water is added in 50mL round-bottomed flask, 5mL DAMO is added in whipping process, is then added
20mg catechol after 1min is sufficiently stirred, said mixture solution is transferred in polytetrafluoroethylene (PTFE) autoclave, 200
DEG C when react 4h, cooled to room temperature.Then by the SiNPs solution prepared 1000Da (molecular weight cutoff) bag filter
Middle dialysis 6h.Finally, by the SiNPs solution storage dialysed to be used for subsequent detection in 4 DEG C of refrigerator.
Embodiment 4
10mL deionized water is added in 25mL round-bottomed flask, 5mL DAMO is added in whipping process, is then added
20mg catechol after 1min is sufficiently stirred, said mixture solution is transferred in polytetrafluoroethylene (PTFE) autoclave, 200
DEG C when react 4h, cooled to room temperature.Then by the SiNPs solution prepared 1000Da (molecular weight cutoff) bag filter
Middle dialysis 6h.Finally, by the SiNPs solution storage dialysed to be used for subsequent detection in 4 DEG C of refrigerator.
Embodiment 5
(1) synthesis of SiNPs
10mL deionized water is added in 25mL round-bottomed flask, 2mL DAMO is added in whipping process, is then added
11mg catechol after 1min is sufficiently stirred, said mixture solution is transferred in polytetrafluoroethylene (PTFE) autoclave, 200
DEG C when react 4h, cooled to room temperature.Then by the SiNPs solution prepared 1000Da (molecular weight cutoff) bag filter
Middle dialysis 6h.Finally, by the SiNPs solution storage dialysed to be used for subsequent detection in 4 DEG C of refrigerator.
(2) it is characterized with the structure of the methods of XPS, FT-IR to SiNPs.
(3) to the thermal stability of SiNPs, anti-light Bleachability, salt tolerance and different pH value fluorescence intensity when is examined
It examines.It determines determination condition, establishes the fluorescence SiNPs test paper of the method for measuring TNP in water phase, preparation detection TNP.
(4) in water phase TNP measurement
(a) SiNPs solution 10mM PBS (pH=7.4) buffer solution prepared is diluted 1000 times；In 3.0mL
The TNP solution of various concentration is added in SiNPs weak solution, places 1min；It is 430nm, launch wavelength 512nm in excitation wavelength
When survey fluorescence intensity；The slit width of excitation wavelength and launch wavelength is 5nm.
(b) SiNPs measures the selectivity of TNP as follows: a certain concentration is added in 3mL SiNPs weak solution
Inorganic ionic solution or nitryl aromatic explosive solution；According to the parametric measurement fluorescence intensity set in (a).All experiments are equal
It carries out at room temperature.
(5) preparation of fluorescent test paper strip and the Visual retrieval to TNP
(a) quantitative filter paper is immersed in the SiNPs solution for diluting 2.5 times with 10mM PBS (pH=7.4) buffer solution；
After impregnating 20min, by filter paper from pipetting out dry 20min in the baking oven for be placed in 50 DEG C in solution；It is naturally cooled to filter paper
After room temperature, filter paper is cut into test strips.
(b) the TNP solution that 10 μ L various concentrations are instilled in the test strips prepared will try after solvent natural evaporation
The color change that paper slip is placed in observation filter paper item under the ultraviolet lamp of 365nm determines that TNP whether there is.Above-mentioned experiment is at room temperature
It carries out.
The measurement result of TNP in 1 water sample of table
From Fig. 4,5 as can be seen that fluorescent nano particle synthesized by the present invention has fabulous selectivity, for various interference
Object is excellent in, and can be used as environmental testing and safety check test uses.
Embodiment 6
Detection mode when safety check is tested
TNP is yellow powdery solid, similar to other nitro explosive appearance, has extremely strong explosivity.On airport
Or it when the discovery suspicious item of other public arenas, can be tested by the test paper mentioned in embodiment 5, in the examination prepared
10 μ L suspicious item solution are instilled on paper slip to be placed in test strips under the ultraviolet lamp of 365nm after solvent natural evaporation and observe filter paper
The color change of item determines that TNP whether there is.If fluorescence intensity change shown in fig. 5 occurs, then illustrate there is pole in suspicious item
Big possibility is mixed with TNP, should handle in time, avoid danger.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto,
Anyone skilled in the art in the technical scope disclosed by the present invention, according to the technique and scheme of the present invention and its
Inventive concept is subject to equivalent substitution or change, should be covered by the protection scope of the present invention.
Claims (2)
1. a kind of water soluble fluorescence nano silicon particles preparation method for measuring trace TNP, which is characterized in that the preparation method comprises the following steps:
A, deionized water is added in round-bottomed flask, DAMO is added in whipping process, catechol is then added, sufficiently stirs
It mixes；
B, said mixture solution is transferred in polytetrafluoroethylene (PTFE) autoclave, 200 DEG C of whens react 4h, naturally cool to room
Temperature；
C, the SiNPs solution prepared is dialysed 6h in the bag filter of 1000Da；
D, by the SiNPs solution storage dialysed in 4 DEG C of refrigerator to be used for subsequent detection；
In preparation method, N- (2- aminoethyl) -3- aminopropyl trimethoxysilane and catechol molar ratio are as follows: 9.3:100；
In preparation method, this method can be used for making test paper or reagent, when preparing test paper, quantitative filter paper is immersed in and uses pH=
7.4 PBS buffer solution dilutes in 2.5 times of SiNPs solution；After impregnating 20min, filter paper is pipetted out from solution it is placed in
Dry 20min in 50 DEG C of baking oven；After filter paper cooled to room temperature, filter paper is cut into test paper.
2. a kind of water soluble fluorescence nano silicon particles preparation method for measuring trace TNP according to claim 1, feature
It is, the detection of trace TNP in detection and water sample of the test paper for TNP in trace explosive is made.
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| CN108410449B (en) * | 2018-01-31 | 2022-03-11 | 兰州大学 | Preparation and application of water-soluble fluorescent silicon nanoparticles for detecting alkaline phosphatase |
| CN112467137B (en) * | 2020-09-09 | 2022-07-12 | 珠海中科兆盈丰新材料科技有限公司 | Silicon-based graphene composite material |
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| KR20120066349A (en) * | 2010-12-14 | 2012-06-22 | 한양대학교 산학협력단 | Carbon/silicon nano-particle complex and method for preparing same |
| CN104181135A (en) * | 2014-08-19 | 2014-12-03 | 东南大学 | Application of water-soluble silicon quantum dot to dopamine detection |
| CN105802611A (en) * | 2016-04-20 | 2016-07-27 | 复旦大学 | Ratio-type nano silicon quantum dot fluorescence probe and preparation method and application thereof |
| CN105969344A (en) * | 2016-06-06 | 2016-09-28 | 中南民族大学 | Silicon quantum dot aqueous phase preparation method |
| CN106350061A (en) * | 2016-08-29 | 2017-01-25 | 北京化工大学 | Silicon quantum dot as well as preparation method and application thereof |
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| KR20120066349A (en) * | 2010-12-14 | 2012-06-22 | 한양대학교 산학협력단 | Carbon/silicon nano-particle complex and method for preparing same |
| CN104181135A (en) * | 2014-08-19 | 2014-12-03 | 东南大学 | Application of water-soluble silicon quantum dot to dopamine detection |
| CN105802611A (en) * | 2016-04-20 | 2016-07-27 | 复旦大学 | Ratio-type nano silicon quantum dot fluorescence probe and preparation method and application thereof |
| CN105969344A (en) * | 2016-06-06 | 2016-09-28 | 中南民族大学 | Silicon quantum dot aqueous phase preparation method |
| CN106350061A (en) * | 2016-08-29 | 2017-01-25 | 北京化工大学 | Silicon quantum dot as well as preparation method and application thereof |
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