CN108426865A - A kind of preparation method and application of surface bond single fluorescent molecular gel glass - Google Patents
A kind of preparation method and application of surface bond single fluorescent molecular gel glass Download PDFInfo
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- CN108426865A CN108426865A CN201810318857.6A CN201810318857A CN108426865A CN 108426865 A CN108426865 A CN 108426865A CN 201810318857 A CN201810318857 A CN 201810318857A CN 108426865 A CN108426865 A CN 108426865A
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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
- G01N21/6402—Atomic fluorescence; Laser induced fluorescence
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/16—Preparation of silica xerogels
- C01B33/163—Preparation of silica xerogels by hydrolysis of organosilicon compounds, e.g. ethyl orthosilicate
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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Abstract
The present invention provides a kind of preparation method and application of surface bond single fluorescent molecular gel glass.It is characterized in that following steps：(1) use sol-gal process with ethyl orthosilicate (TEOS) and amino silane collectively as silicon source synthesizing amino functionalized SiO 2 microballoon, it is well dispersed in absolute ethyl alcohol after washes clean, is subsequently placed in baking oven and is formed by curing surface amination gel glass；(2) lemon acyl chlorides is synthesized by chloride method using citric acid as raw material；(3) react with the acyl chlorides synthetic surface that links together of the amino of glass surface is bonded the gel glass of single fluorescent molecule, places it in thermal-stable in baking oven.The gel glass homogeneous transparent of surface bond list fluorescent molecular prepared by the method for the present invention, with good thermal stability and easily processed into type, it is suitble to industrial production, can be applied to the qualitative detection of iron ion, also have broad application prospects in photovoltaic cell or lighting area.
Description
Technical field
The invention belongs to fluorescent molecular composite luminescent material technical fields, and in particular to a kind of surface bond single fluorescent point
The preparation method and application of sub- gel glass.
Background technology
Hybrid inorganic-organic solid fluorescence sensing is made in recent years, organic fluorescence molecule is fixed on solid matrix
The method of device becomes the new method of ion sensor and identification, and has attracted great research interest.These solid matrixs generally wrap
Include SiO2、TiO2、Al2O3、Fe3O4With thin polymer film etc..Using the methods of sol-gel or hydro-thermal by organic fluorescence molecule
Fixed in inorganic or organic/inorganic matrix become a selectable approach.Wherein, using amino oxygen alkane as presoma via
Gel glass prepared by sol-gel process is a kind of good hybrid inorganic-organic materials matrix, has flexibility, Yi Jia
The advantages that work, optical transparence, thermal stability.Currently, the mode that organic fluorescence molecule introduces gel glass is with physical doping
The problems such as master, this mode is although simple and practicable, but uneven there is bulk phase concentration, influence luminosity.
Heavy metal ion is the pollutant very harmful to environment, because they are widely distributed in air, water and soil
In, and have prodigious harm to human health.The analysis method of the detection iron ion of exploitation sensibility and selectivity evokes
Broad interest, common qualitative and quantitative detection Fe3+Method have：Atomic absorption, colorimetric method, spectrophotometry, cyclic voltammetry,
Fluorescence probe method etc..Fe is detected currently with fluorescence probe method3+Patent have very much, but still there are many aspect deficiency,
For example fluorescence probe preparation process is relatively cumbersome, cannot carry out Quantitative detection etc..Therefore, overcome the above deficiency, prepare
A kind of easy to use, strong antijamming capability can carry out the Fe of fast qualitative detection simultaneously3+Probe has important practical significance.
Invention content
In view of the deficiencies of the prior art, it is solidifying to be to provide a kind of surface bond single fluorescent molecule for one of present disclosure
The preparation method and application of glue glass, the fluorescent glass are to deposit the gel to be formed by amination silicon dioxide microsphere self assembly
Glass, surface only graft one layer of fluorescent molecular and are uniformly dispersed and with the ability for efficiently detecting iron ion in water body in real time.
A kind of preparation method and application of surface bond single fluorescent molecular gel glass provided by the present invention, including with
Lower step：
（1）Prepare amination silicon dioxide microsphere
By ethyl orthosilicate, amino silane, deionized water, ammonium hydroxide with mass ratio 1：(0~1)：(5~15)：(2 ~ 4) are added to alcohols
In solvent, it is stirred to react at 3 ~ 12 hours, after centrifuge washing is clean, 0 ~ 100 DEG C drying and grinding at room temperature into powder, it is made 120 ~
250 nm amination silicon dioxide microspheres；
（2）Prepare amination gel glass
It in amination silicon dioxide microsphere ultrasonic disperse to alcohols solvent, will be placed in baking oven and heat a period of time, remove solvent
Form amination gel glass；
（3）The preparation of lemon acyl chlorides
By anhydrous citric acid and thionyl chloride according to molar ratio 1:(2 ~ 4) are added in reaction dissolvent, -20 DEG C ~ 30 DEG C conditions
Lower reaction 6 ~ 18 hours.Three times with the azeotropic of n-hexane and tetrahydrofuran purification rotary-cleaning, excessive thionyl chloride is removed, is obtained
To pure product；
（4）Prepare the gel glass of surface bond single fluorescent molecule
Amination gel glass obtained is placed in the tetrahydrofuran solution of lemon acyl chlorides, is sealed with polyethylene film, centainly
At a temperature of react the gel glass of 4 ~ 12 hours obtained surface bond single fluorescent molecules.Then it places it in baking oven and heats surely
Fixed a period of time.
As optimal technical scheme, during synthesizing fluorescence gel glass, the alcohols solvent is methanol, ethyl alcohol
Or butanol, preferred absolute ethyl alcohol.
As optimal technical scheme, during synthesizing fluorescence gel glass, the grain of the fluorescent silicon dioxide microballoon
Diameter is 120 ~ 250 nm, preferably 200 nm.
As optimal technical scheme, during synthesizing fluorescence gel glass, the ethyl orthosilicate, amino silane,
Deionized water, ammonium hydroxide are by certain mass than 1：(0~1)：(5~15)：(2 ~ 4), preferably 1:0.1:10:3.
As optimal technical scheme, during synthesizing fluorescence gel glass, the amino silane is 3- aminopropans
Ethyl triethoxy silicane alkane, aminoethylaminopropyl methyl dimethoxysilane, 3- TSL 8330s etc., preferably ammonia second
Base aminopropyltriethoxy dimethoxysilane.
As optimal technical scheme, during synthesizing fluorescence gel glass, the amination silica
Microballoon heats 12 hours in baking oven at 50 DEG C ~ 100 DEG C heating 6 ~ 24 hours, preferably 60 DEG C.
As optimal technical scheme, during synthesizing fluorescent silicon dioxide microballoon, the fluorescence gel glass needs
It to be heated 20 hours at 6 ~ 24 hours, preferably 80 DEG C 50 DEG C ~ 100 DEG C thermal-stables in an oven.
As optimal technical scheme, during synthesizing fluorescent silicon dioxide microballoon, the amination glass and lemon
Lemon acyl chloride reaction solvent is acetonitrile, toluene, the solvent stabilities such as tetrahydrofuran, preferably tetrahydrofuran.
It is an advantage of the invention that：
The preparation method is simple for process, reaction condition is mild and environmentally protective；The fluorescence gel glass homogeneous transparent of preparation, has
Good thermal stability, surface only connect one layer of fluorescent molecular, the efficient qualitative detection of iron ion are can be applied to, in photovoltaic
It has broad application prospects in battery or lighting area.
Description of the drawings
Fig. 1 is the scanning electron microscopic picture of amination silicon dioxide microsphere prepared by embodiment 1.
Fig. 2 is the infrared spectrogram of surface bond single fluorescent molecular gel glass prepared by embodiment 1.
Fig. 3 is the fluorescence spectra of surface bond single fluorescent molecular gel glass prepared by embodiment 1.
Specific implementation mode
The present invention is described in more detail with reference to the accompanying drawings and examples, but the present invention is not limited only to these implementations
Example.
Embodiment 1：
（1）Prepare amination silicon dioxide microsphere
By ethyl orthosilicate, amino silane, deionized water, ammonium hydroxide with mass ratio 1：0.1：10：3 are added in alcohols solvent, room
It is stirred to react drying and grinding at 6 hours, after centrifuge washing is clean, 60 DEG C under temperature, 200 nm or so amination two is made at powder
Silicon oxide microsphere；
（2）Prepare amination gel glass
It in amination silicon dioxide microsphere ultrasonic disperse to absolute ethyl alcohol, will be placed in baking oven and heat 12 hours for 60 DEG C, removal is molten
Dosage form is at amination gel glass；
（3）The preparation of lemon acyl chlorides
By anhydrous citric acid and thionyl chloride according to molar ratio 1:3 are added in reaction dissolvent, are reacted 12 hours under the conditions of 0 DEG C.
Three times with the azeotropic of n-hexane and tetrahydrofuran purification rotary-cleaning, excessive thionyl chloride is removed, pure product is obtained；
（4）Prepare the gel glass of surface bond single fluorescent molecule
Amination gel glass obtained is placed in the tetrahydrofuran solution of lemon acyl chlorides, is sealed with polyethylene film, 25 DEG C
The gel glass of 6 hours obtained surface bond single fluorescent molecules of lower reaction.Then 80 DEG C of thermal-stables in baking oven are placed it in
20 hours.
Embodiment 2：
（1）Prepare amination silicon dioxide microsphere
By ethyl orthosilicate, amino silane, deionized water, ammonium hydroxide with mass ratio 1：0.2：8：2 are added in alcohols solvent, room temperature
Under be stirred to react at 6 hours, after centrifuge washing is clean, 60 DEG C drying and grinding into powder, 220 nm or so amination dioxy is made
SiClx microballoon；
（2）Prepare amination gel glass
It in amination silicon dioxide microsphere ultrasonic disperse to absolute ethyl alcohol, will be placed in baking oven and heat 10 hours for 70 DEG C, removal is molten
Dosage form is at amination gel glass；
（3）The preparation of lemon acyl chlorides
By anhydrous citric acid and thionyl chloride according to molar ratio 1:3 are added in reaction dissolvent, are reacted 12 hours under the conditions of 0 DEG C.
Three times with the azeotropic of n-hexane and tetrahydrofuran purification rotary-cleaning, excessive thionyl chloride is removed, pure product is obtained；
（4）Prepare the gel glass of surface bond single fluorescent molecule
Amination gel glass obtained is placed in the tetrahydrofuran solution of lemon acyl chlorides, is sealed with polyethylene film, 25 DEG C
The gel glass of 4 hours obtained surface bond single fluorescent molecules of lower reaction.Then 90 DEG C of thermal-stables in baking oven are placed it in
24 hours.
Embodiment 3：
（1）Prepare amination silicon dioxide microsphere
By ethyl orthosilicate, amino silane, deionized water, ammonium hydroxide with mass ratio 1：0.05：10：2 are added in alcohols solvent, room
It is stirred to react drying and grinding at 6 hours, after centrifuge washing is clean, 60 DEG C under temperature, 180 nm or so amination two is made at powder
Silicon oxide microsphere；
（2）Prepare amination gel glass
It in amination silicon dioxide microsphere ultrasonic disperse to absolute ethyl alcohol, will be placed in baking oven and heat 8 hours for 60 DEG C, removal is molten
Dosage form is at amination gel glass；
（3）The preparation of lemon acyl chlorides
By anhydrous citric acid and thionyl chloride according to molar ratio 1:3 are added in reaction dissolvent, are reacted 12 hours under the conditions of 0 DEG C.
Three times with the azeotropic of n-hexane and tetrahydrofuran purification rotary-cleaning, excessive thionyl chloride is removed, pure product is obtained；
（4）Prepare the gel glass of surface bond single fluorescent molecule
Amination gel glass obtained is placed in the tetrahydrofuran solution of lemon acyl chlorides, is sealed with polyethylene film, 25 DEG C
The gel glass of 6 hours obtained surface bond single fluorescent molecules of lower reaction.Then 60 DEG C of thermal-stables in baking oven are placed it in
24 hours.
Embodiment 4：
（1）Prepare amination silicon dioxide microsphere
By ethyl orthosilicate, amino silane, deionized water, ammonium hydroxide with mass ratio 1：0.2：6：3 are added in alcohols solvent, room temperature
Under be stirred to react at 8 hours, after centrifuge washing is clean, 60 DEG C drying and grinding into powder, 230 nm or so amination dioxy is made
SiClx microballoon；
（2）Prepare amination gel glass
It in amination silicon dioxide microsphere ultrasonic disperse to absolute ethyl alcohol, will be placed in baking oven and heat 15 hours for 50 DEG C, removal is molten
Dosage form is at amination gel glass；
（3）The preparation of lemon acyl chlorides
By anhydrous citric acid and thionyl chloride according to molar ratio 1:3 are added in reaction dissolvent, and it is small that 10 are reacted under the conditions of -5 DEG C
When.Three times with the azeotropic of n-hexane and tetrahydrofuran purification rotary-cleaning, excessive thionyl chloride is removed, pure product is obtained；
（4）Prepare the gel glass of surface bond single fluorescent molecule
Amination gel glass obtained is placed in the tetrahydrofuran solution of lemon acyl chlorides, is sealed with polyethylene film, 25 DEG C
The gel glass of 10 hours obtained surface bond single fluorescent molecules of lower reaction.Then 70 DEG C of thermal-stables in baking oven are placed it in
18 hours.
The above-mentioned description to embodiment can be understood and applied the invention for ease of those skilled in the art.
Person skilled in the art obviously readily can make various modifications to these embodiments, and described herein general
Principle be applied in other embodiment without into cross creative work.Therefore, the present invention is not limited to embodiment here, abilities
Field technique personnel announcement according to the present invention, the improvement and modification made for the present invention all should be in protection scope of the present invention
Within.
Claims (9)
1. a kind of preparation method and application of surface bond single fluorescent molecular gel glass, it is characterised in that it is by following step
Composition：
（1）Prepare amination silicon dioxide microsphere
By ethyl orthosilicate, amino silane, deionized water, ammonium hydroxide with mass ratio 1：(0~1)：(5~15)：(2 ~ 4) are added to alcohols
In solvent, it is stirred to react at 3 ~ 12 hours, after centrifuge washing is clean, 0 ~ 100 DEG C drying and grinding at room temperature into powder, it is made 120 ~
250 nm amination silicon dioxide microspheres；
（2）Prepare amination gel glass
It in amination silicon dioxide microsphere ultrasonic disperse to alcohols solvent, will be placed in baking oven and heat a period of time, remove solvent
Form amination gel glass；
（3）The preparation of lemon acyl chlorides
By anhydrous citric acid and thionyl chloride according to molar ratio 1:(2 ~ 4) are added in reaction dissolvent, -20 DEG C ~ 30 DEG C conditions
Lower reaction 6 ~ 18 hours three times with the azeotropic of n-hexane and tetrahydrofuran purification rotary-cleaning removes excessive thionyl chloride, obtains
To pure product；
（4）Prepare the gel glass of surface bond single fluorescent molecule
Amination gel glass obtained is placed in the tetrahydrofuran solution of lemon acyl chlorides, is sealed with polyethylene film, centainly
At a temperature of react the gel glass of 4 ~ 12 hours obtained surface bond single fluorescent molecules, then place it in baking oven heat it is steady
Fixed a period of time.
2. a kind of preparation method and application of surface bond single fluorescent molecular gel glass as described in claim 1, special
Sign is step（1）（2）The alcohols solvent is methanol, ethyl alcohol or butanol, alcohols solvent etc..
3. a kind of preparation method and application of surface bond single fluorescent molecular gel glass as described in claim 1, special
Sign is step（1）The grain size of the amination silicon dioxide microsphere is 120 ~ 250 nm.
4. a kind of preparation method and application of surface bond single fluorescent molecular gel glass as described in claim 1, special
Sign is step（1）The ethyl orthosilicate and amino silane are according to mass ratio 1:(0~1).
5. a kind of preparation method and application of surface bond single fluorescent molecular gel glass as described in claim 1, special
Sign is step（1）The amino silane be 3-aminopropyltriethoxysilane, aminoethylaminopropyl methyl dimethoxysilane,
3- TSL 8330s etc..
6. a kind of preparation method and application of surface bond single fluorescent molecular gel glass as described in claim 1, special
Sign is step（2）The amination silicon dioxide microsphere heats 6 ~ 24 hours for 50 DEG C ~ 100 DEG C in baking oven.
7. a kind of preparation method and application of surface bond single fluorescent molecular gel glass as described in claim 1, special
Sign is step（3）The reaction dissolvent is acetonitrile, toluene, the solvent stabilities such as tetrahydrofuran.
8. a kind of preparation method and application of surface bond single fluorescent molecular gel glass as described in claim 1, special
Sign is step（4）50 DEG C in an oven ~ 100 DEG C of needs thermal-stable 6 ~ 24 hours.
9. a kind of preparation method and application of surface bond single fluorescent molecular gel glass, which is characterized in that wanted according to right
Any one of 1 ~ 8 the method is asked to be made.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109399647A (en) * | 2018-11-01 | 2019-03-01 | 湖南工业大学 | Hollow multistage mesoporous silicon dioxide micro-sphere of a kind of amino functional and preparation method thereof |
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| CN104371732A (en) * | 2014-11-14 | 2015-02-25 | 天津理工大学 | Method for preparing fluorescent gel glass by adopting hydrophobic semiconductor quantum dots |
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2018
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| CN104371732A (en) * | 2014-11-14 | 2015-02-25 | 天津理工大学 | Method for preparing fluorescent gel glass by adopting hydrophobic semiconductor quantum dots |
| CN105349150A (en) * | 2015-05-26 | 2016-02-24 | 大连工业大学 | Fluorescent film sensing composite material as well as preparation method and application thereof |
| CN106929001A (en) * | 2017-04-12 | 2017-07-07 | 中国农业科学院蔬菜花卉研究所 | A kind of fluorescence SiO2The preparation method of Nano microsphere |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109399647A (en) * | 2018-11-01 | 2019-03-01 | 湖南工业大学 | Hollow multistage mesoporous silicon dioxide micro-sphere of a kind of amino functional and preparation method thereof |
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Application publication date: 20180821 |