CN107099036A - Fluorescence chemical sensor material suitable for the liquid different scale molecule of explosive containing nitro and its preparation method and application - Google Patents
Fluorescence chemical sensor material suitable for the liquid different scale molecule of explosive containing nitro and its preparation method and application Download PDFInfo
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- CN107099036A CN107099036A CN201710144053.4A CN201710144053A CN107099036A CN 107099036 A CN107099036 A CN 107099036A CN 201710144053 A CN201710144053 A CN 201710144053A CN 107099036 A CN107099036 A CN 107099036A
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- 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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- 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
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Abstract
The present invention relates to a kind of suitable for fluorescence chemical sensor material of the liquid different scale molecule of explosive containing nitro and its preparation method and application, belong to chemical sensor material technical field.Solve the technical problem that existing fluorescence explosive detection sensor adsorptive selectivity is poor, reception fluorescence intensity is unstable.The fluorescence chemical sensor material that the present invention is provided, it is different from the physisorption between conventional explosive Molecular Detection material and adsorbed explosive molecule, adsorbate is to be present in by chemisorption in the fluorescence chemical sensor material duct, and the material is used as metal ion by magnesium metal, can it is a certain degree of reduce material quality, more conducively practical application, it is strong with the molecular action of explosive containing nitro, detection explosive molecule can be carried out by the method for fluorescent quenching, so as to improve the stability and accuracy of test.The preparation method step is simple, low raw-material cost, repeatability is strong, can realize prepared by batch, can be to be applicable.
Description
Technical field
The present invention relates to chemical sensor material technical field, and in particular to one kind is applied to liquid different scale and contains nitro
Fluorescence chemical sensor material of explosive molecule and its preparation method and application.
Background technology
The sensing technology of principle of fluorescent quenching is fast to the detection speed of explosive, sensitivity is high, stability good, sensor body
The small, cost of product is low, it is easy to operate the advantages of, it is considered to be one of best technology in terms of current explosive detection.Fluorescent quenching
Mechanism be that an electronics on the electronic transfer process based on photoinduction, (HOMO) of fluorogen highest occupied molecular orbital is excited
Lowest unoccupied molecular orbital (LUMO) is transitted to, a room is left on HOMO, now, will be provided containing electron donors such as nitro, cyano group
One electro transfer is to room on HOMO, the fluorescent emission process for as a result returning to the electronics suppressed on LUMO on HOMO, so that
Generation fluorescent quenching.In view of the explosive sensing device of principle of fluorescent quenching has many advantages, such as, external many research institutions are just
Stepping up to be studied.The Swager groups design of Massachusetts Institute Technology, which has been synthesized, carries many yuan of rings of Three-dimensional Rigidity in skeleton
Polyparaphenylene's ethynylene (PPE) of shape pentiptycene groups, detects that solid nitro-aromatic class is exploded using Fluorimetric Quenching Method
Thing TNT and DNT, in TNT (10ppb) and DNT (180ppb) saturated vapor, the fluorescent quenching efficiency of detectable substance is in 10s
30% and 70% are respectively reached, high sensitivity is shown.The country, Zhang Zhongping groups etc., which have also carried out, utilizes quantum dot nano
Material carries out the research in terms of detection explosive fluorescent material synthesis.The Li Jing group of Rutgers university of the U.S. utilizes MOFs micropores
Material is (such as：[Zn2(bpdc)2(bpee)] (bpdc=4,4 '-biphenyldicarboxylate；Bpee=1,2-
Bipyridylethene)) as solid 2,4- dinitrotoluene (DNT)s (DNT) and DMNB (DMNB)
The sensor of nitro explosive quick detection, its principle is similar with being formerly mentioned conjugated polymer, is organic by metal
Framework compound MOFs adsorption realizes the quick detection to solid explosive.
At present the fluorescence explosives sensor majority developed both at home and abroad be based on conjugated polymer (CPs,
ConjugatedPolymer) fluorescence intensity is detected to adsorb explosive.This method depends on and prepares high ratio surface
Polymer sensor simultaneously further improves their surface adsorption property by the method for chemical modification.But because absorption is with thing
Manage what the mode adsorbed was carried out, the adhesion between adsorbent and adsorbed explosive steam is weaker, and (Van der Waals force is quiet
Electrical affinity), the selectivity of absorption it is poor, unstable, fluorescence indicator photobleaching when light source and detector, light path vibration
When, it can all cause and receive the unstable of fluorescence intensity, and then cause measurement error.
The content of the invention
The invention solves the problems that fluorescence explosive detection sensor adsorptive selectivity is poor in the prior art, receive fluorescence intensity
There is provided a kind of fluorescence chemical sensor material suitable for the liquid different scale molecule of explosive containing nitro for unstable technical problem
Material and its preparation method and application.
In order to solve the above-mentioned technical problem, technical scheme is specific as follows：
A kind of fluorescence chemical sensor material suitable for the liquid different scale molecule of explosive containing nitro, the fluorescence chemical
Sensor material is the metal-organic framework materials using magnesium as metal center, and its chemical composition is：Mg2(BDC)2(BPNO), formula
In：BDC is that 1,4- phthalic acids (1,4-benzene dicarboxylate), BPNO are 4,4 '-bipyridyl-N, N '-titanium dioxide
Thing (4,4 '-dipyridyl-N, N '-dioxide).
A kind of preparation method of fluorescence chemical sensor material suitable for the liquid different scale molecule of explosive containing nitro,
Comprise the following steps：
By 0.1282g Mg (NO3)2·6H2O、0.0330g H2The anhydrous second of BDC, 0.0565g BPNO, 2mL DMF, 3mL
Alcohol is placed in the stainless steel cauldron of teflon lined, is heated 24 hours under conditions of 120 DEG C of spontaneous pressure, naturally cold
But to after room temperature, carry out separation of solid and liquid, then by solid crude product using DMF cleaning filterings after, obtain the production of yellow bulk crystals
Thing；Finally the yellow bulk crystals product is put into and is connected with the round-bottomed flask that oil pump is vacuumized, is heated in 150 DEG C of oil bath
8 hours, that is, obtain the fluorescence chemical sensor material suitable for the liquid different scale molecule of explosive containing nitro.
Suitable for the application of the fluorescence chemical sensor material of the liquid different scale molecule of explosive containing nitro, this is Fluoresceinated
Learning sensor material is used to detect nitrobenzene, nitromethane or nitroethane.
The beneficial effects of the invention are as follows：
The fluorescence chemical sensor material suitable for the liquid different scale molecule of explosive containing nitro that the present invention is provided is
Using alkaline-earth metal magnesium as the metal-organic framework materials of metal center, and utilize the absorption inside material molecule duct and the work of separation
Can, by the method for fluorescent quenching, the explosive molecule containing nitro of different scale in liquid phase is detected, is realized quick-fried to liquid nitro
The selective absorption of fried thing with separate and quick detection fluorescence chemical sensor.
The fluorescence chemical sensor material suitable for the liquid different scale molecule of explosive containing nitro that the present invention is provided, area
Physisorption not between conventional explosive Molecular Detection material and adsorbed explosive molecule, adsorbate is logical
Chemisorption is crossed to be present in the fluorescence chemical sensor material duct, and the material by magnesium metal as metal ion,
Can a certain degree of quality for reducing material, more conducively practical application is strong with the molecular action of explosive containing nitro, can pass through fluorescence
The method being quenched carries out detection explosive molecule, so as to improve the stability and accuracy of test.
The fluorescence chemical sensor material suitable for the liquid different scale molecule of explosive containing nitro that the present invention is provided
Preparation method utilizes solvent-thermal process method, by the control of the ratio of temperature, solvent, alkaline earth ion and organic ligand, obtains good
Good alkaline-earth metal organic framework compounds, the preparation method step is simple, low raw-material cost, repeatable strong, Ke Yishi
Now prepared by batch, can be to be applicable.
The fluorescence chemical sensor material suitable for the liquid different scale molecule of explosive containing nitro that the present invention is provided is used
In detection nitrobenzene, nitromethane and nitroethane, three kinds of adsorbates are to be present in sensory device by chemisorption
In the duct of material, so as to improve the stability and accuracy of measurement.
Brief description of the drawings
The present invention is described in further detail with reference to the accompanying drawings and detailed description.
Fig. 1 is that the fluorescence chemical sensing suitable for the liquid different scale molecule of explosive containing nitro is prepared by the present invention
Device material crystal structure figure；
Fig. 2 is that the fluorescence chemical sensing suitable for the liquid different scale molecule of explosive containing nitro is prepared by the present invention
Equipment material adsorbs the molecular schematic diagram of explosive containing nitro of different scale；
Fig. 3 is the fluorescence chemical sensor suitable for the liquid different scale molecule of explosive containing nitro prepared by the present invention
Material carries out Dynamic Fluorescence spectrum under room temperature 305nm shooting conditions in the nitro explosive molecular vapor of three kinds of different scales
Test analysis figure；
Fig. 4 is that the fluorescence chemical sensing suitable for the liquid different scale molecule of explosive containing nitro is prepared by the present invention
The molecule of explosive containing nitro that equipment material adsorbs three kinds of different scales recycles fluorescent quenching efficiency chart.
Embodiment
The present invention is described in detail below in conjunction with the accompanying drawings.
Raw material used in the present invention is Mg (NO3)3·6H2O, H2BDC, BPNO, DMF and absolute ethyl alcohol.
Prepare embodiment [Mg2(BDC)2(BPNO)]
By Mg (NO3)2·6H2O (0.1282g, 0.5mmol), H2BDC (0.0330g, 0.2mmol), BPNO (0.0565g,
0.3mmol), DMF (2mL), absolute ethyl alcohol (3mL) is positioned in the stainless steel cauldron of 15mL teflon lineds, 120
Heat 24 hours, naturally cooled to after room temperature under conditions of DEG C spontaneous pressure, carry out separation of solid and liquid, then make solid crude product
Cleaned with DMF after filtering, obtain yellow bulk crystals product (product 1), finally the yellow bulk crystals product is put into and is connected with
In the round-bottomed flask that oil pump is vacuumized, heated 8 hours in 150 DEG C of oil bath, you can prepare final product (product 1a).
Using the homoorganicity of above-mentioned metal organic framework compound, different metal ions is synthesized this in different proportions
Material, can be achieved the metal-organic framework materials of the explosive containing nitro of absorption and separation different scale.It is also an option that different
The isostructural metal-organic framework materials of organic ligand materials synthesis.
Application Example
The fluorescence chemical sensor material suitable for the liquid different scale molecule of explosive containing nitro that the present invention is provided
In the saturated vapor for being respectively exposed to nitrobenzene (NB), nitromethane (NM) and nitroethane (NE) three kinds of nitro compounds,
Under room temperature 305nm shooting conditions, Dynamic Fluorescence spectrum test is carried out, fluorescent quenching effect occurs in same time, quenches
Efficiency of going out is respectively 94.7%, 92.1% and 83.3%.By different quenching effects, so as to reach the work of separation and detection
With.Fluorescence chemical sensor material of the present invention is soaked in and is respectively provided with the container of NB, NM and NE liquid, passes through suction-operated
Three kinds of new products will be obtained, are [Mg respectively2(BDC)2(BPNO)] 2NB (product 2), [Mg2(BDC)2(BPNO)]·2NM
(product 3) and [Mg2(BDC)2(BPNO)] 2NE (product 4).Analyzed by X-ray single crystal diffraction, three kinds of adsorbates are
It is present in by chemisorption in the duct of sensor material, so as to improve the stability and accuracy of measurement.This
Outside, it can be reprocessed by the way that three kinds have been adsorbed with the material of nitro explosive molecule, the present invention is obtained again is applied to liquid
The fluorescence chemical sensor material of different scale explosive containing nitro molecule, so as to carry out Reusability.
Fig. 1 is that the fluorescence chemical sensing suitable for the liquid different scale molecule of explosive containing nitro is prepared by the present invention
In device material crystal structure figure, figure：Bead is oxygen element, and big ball is magnesium elements, and other elements such as icon is noted；The figure can directly divide
Analyse its molecular structure.
Fig. 2 is that the fluorescence chemical sensing suitable for the liquid different scale molecule of explosive containing nitro is prepared by the present invention
Equipment material adsorbs the molecular schematic diagram of explosive containing nitro of different scale；Product 1 under heating and vacuumized conditions by removing
DMF molecules in duct, obtain product 1a, and product 1a can be used for absorption explosive molecule NB, NM, NE, obtain containing NB, NM,
NE three kinds of products 2,3,4, three kinds of products in DMF solution by soaking, and the molecule in commutative duct retrieves product
1.The purpose of reuse is can reach by above procedure.
Fig. 3 is the fluorescence chemical sensor suitable for the liquid different scale molecule of explosive containing nitro prepared by the present invention
Material (product 1a), under room temperature 305nm shooting conditions, inspires stronger blue 421nm fluorescence, in three kinds of different scales
In nitro explosive molecular vapor, quick fluorescent quenching phenomenon can be observed.Tracing analysis is quenched by analysis of fluorescence, found
In three kinds of atmosphere, it is NB that efficiency order, which is quenched,>NM>NE.
Fig. 4 is that the fluorescence chemical sensing suitable for the liquid different scale molecule of explosive containing nitro is prepared by the present invention
The molecule of explosive containing nitro that equipment material adsorbs three kinds of different scales recycles fluorescent quenching efficiency chart.Abscissa is attached most importance in figure
Multiple access times, ordinate is emissive porwer, in each Test Drawing, and left side is product 1a emissive porwer, and right side is absorption
Emissive porwer after explosive molecule.From figure it was found from data, by three reuses, product 1a is remained to by fluorescence
Detection is identified to three kinds of explosive molecules in quenching method.
Table 1：Product 1, the crystal structure refined parameters of 1a, 2,3,4,2 ', 3 ' and 4 '
Upper table explanation：The crystal structure of product 2 ', 3 ' and 4 ' essence that product 2,3,4 is obtained again after being handled except adsorbate
Parameter is repaiied, shows that the fluorescence chemical sensor material in the present invention suitable for the liquid different scale molecule of explosive containing nitro can be weighed
It is multiple to utilize.
Obviously, above-described embodiment is only intended to clearly illustrate example, and the not restriction to embodiment.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of change or
Change.There is no necessity and possibility to exhaust all the enbodiments.And the obvious change thus extended out or
Among changing still in the protection domain of the invention.
Claims (3)
1. a kind of fluorescence chemical sensor material suitable for the liquid different scale molecule of explosive containing nitro, it is characterised in that
The fluorescence chemical sensor material is the metal-organic framework materials using magnesium as metal center, and its chemical composition is：Mg2(BDC)2
(BPNO), in formula：BDC is that 1,4- phthalic acids, BPNO are 4,4 '-bipyridyl-N, N '-dioxide.
2. the fluorescence chemical sensor material suitable for the liquid different scale molecule of explosive containing nitro described in claim 1
Preparation method, it is characterised in that comprise the following steps：
By 0.1282g Mg (NO3)2·6H2O、0.0330g H2BDC, 0.0565g BPNO, 2mL DMF, 3mL absolute ethyl alcohol are placed in
In the stainless steel cauldron of teflon lined, heated 24 hours under conditions of 120 DEG C of spontaneous pressure, naturally cool to room
Wen Hou, carries out separation of solid and liquid, after then solid crude product is filtered using DMF cleanings, obtains yellow bulk crystals product；Finally
The yellow bulk crystals product is put into and is connected with the round-bottomed flask that oil pump is vacuumized, is heated 8 hours in 150 DEG C of oil bath,
Obtain the fluorescence chemical sensor material suitable for the liquid different scale molecule of explosive containing nitro.
3. the fluorescence chemical sensor material suitable for the liquid different scale molecule of explosive containing nitro described in claim 1
Using, it is characterised in that the fluorescence chemical sensor material is used to detect nitrobenzene, nitromethane or nitroethane.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108414490A (en) * | 2018-03-22 | 2018-08-17 | 中国工程物理研究院化工材料研究所 | Fluorescence gel test paper and fluorescence colloidal sol, and preparation method and application |
| CN111825851A (en) * | 2020-08-11 | 2020-10-27 | 盐城工学院 | Light-emitting metal-organic framework material based on PBP and polycarboxylic acid ligand and preparation method and application thereof |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108414490A (en) * | 2018-03-22 | 2018-08-17 | 中国工程物理研究院化工材料研究所 | Fluorescence gel test paper and fluorescence colloidal sol, and preparation method and application |
| CN108414490B (en) * | 2018-03-22 | 2021-03-16 | 中国工程物理研究院化工材料研究所 | Fluorescent gel test paper, fluorescent sol, preparation method and application thereof |
| CN111825851A (en) * | 2020-08-11 | 2020-10-27 | 盐城工学院 | Light-emitting metal-organic framework material based on PBP and polycarboxylic acid ligand and preparation method and application thereof |
| CN111825851B (en) * | 2020-08-11 | 2022-04-05 | 盐城工学院 | Light-emitting metal-organic framework material based on PBP and polycarboxylic acid ligand and preparation method and application thereof |
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Application publication date: 20170829 |