CN103204972A - Thermo-sensitive fluorescent carbon nano composite material and preparation method thereof - Google Patents
Thermo-sensitive fluorescent carbon nano composite material and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the field of a composite intelligent fluorescent material, and in particular relates to a thermo-sensitive fluorescent carbon nano composite material and a preparation method thereof. The fluorescent material is prepared by the steps of adding N,N-methylene bisacrylamide in an acrylamide water solution, and mixing; adding 0.3-3wt% of a carbon quantum dot solution, 0.5-2.5wt% of a poly N-isopropyl acrylamide solution and tetraethylethylenediamine in mixing liquid, adding an initiator after dissolving, and standing by for 3-8 hours to obtain the fluorescent material. The initiator is either thiosulfate or persulfate. According to the fluorescent material disclosed by the invention, with the addition of the carbon quantum dot, the fluorescence of the composite material is guaranteed, by introducing the N-isopropyl acrylamide, the composite material is thermo-sensitive, and by adding the acrylamide, the mechanical strength of the semi-interpenetrating network structure of the composite material is enhanced; and the composite is free from toxicity, environment-friendly and good in stability; and the thermo-sensitive fluorescent carbon nano composite material is simple in preparation process, low in raw material price, and free from toxicity and pollution in a synthesis process.
Description
Technical field
The invention belongs to composite intelligent fluorescent material field, particularly a kind of temperature-sensitive fluorescent carbon nano-composite material and preparation method thereof.
Background technology
In recent years, intelligent material is a kind of rising high tech tip materials, is a class produces response and has the function executive capability to environment sensing type material.Temperature sensitive intelligent material in the intelligent material is paid attention to by people because of subtle change or stimulation that it can the perception ambient temperature.Tanaka in 1984 has reported that poly N-isopropyl acrylamide (PNIPAM) hydrogel has the temperature-sensing property feature, contain clear water group and hydrophobic group in its side chain simultaneously, and receive between this wetting ability and the hydrophobic group that there is the hydrophilic/hydrophobic balance in Temperature Influence, the PNIPAM hydrogel has a lower Kraft point (LCST) about 32 ℃.When temperature was lower than its LCST, the PNIPAM hydrogel is the suction height swelling in water, and when temperature was higher than LCST, the PNIPAM hydrogel acutely shrank dehydration, was separated.Because the intelligent characteristic that this sensitive aquagel shows, make aspects such as its separation purification at drug release, protein, memory cell switch that wide application prospect be arranged, but the mechanics intensity difference of this hydrogel own, especially lost self holding capacity by water-soluble substantially after bloated, so limited its application.
Along with optical detective technology in the further research aspect the biosensor, people are to having the temperature sensitive fluorescent material of optical tag and temperature response, cause more and more people's concern, exist certain cognation between the fluorescence intensity of this matrix material and the envrionment temperature, and has a reversible cycle characteristic, in this material, fluorescent characteristic is generally provided by fluorescence quantum.But, the shortcoming that the present main fluorescence quantum that adopts exists some can not be ignored, as semiconductor-quantum-point (CdSe, CdTe, CdS etc.), contain the toxic metal ion, environment and HUMAN HEALTH are caused potential threat and limited its application in fields such as biological medicine and food safeties.And a kind of novel carbon nanomaterial that the carbon quantum dot is the scientist of U.S. Clemson University to be produced first is similar with various metal quantum points, has superior luminescent properties, and the carbon quantum dot can emit a brilliant light under the situation of illumination.Relative metal quantum point, carbon quantum dot toxicological harmless effect, very little to the harm of environment, preparation cost is cheap; Compare with semiconductor-quantum-point, the carbon quantum dot light emitting is more stable, be easy to functionalization and industrialization, nontoxic, preparation cheap and simple, and expection will bring new development space to fields such as luminescent material, environmental protection, biomedicines.
Summary of the invention
The purpose of this invention is to provide a kind of temperature-sensitive fluorescent carbon nano-composite material, this matrix material has the dual responsiveness of fluorescence and temperature sensitive property, and stable, nontoxic, safety.
Another object of the present invention provides a kind of method for preparing above-mentioned temperature-sensitive fluorescent carbon nano-composite material, and this method synthesis technique is simple, reaction conditions is gentle, operational safety, environmental protection.
Purpose of the present invention can be achieved through the following technical solutions:
A kind of preparation method of temperature-sensitive fluorescent carbon nano-composite material, its step comprises: add N,N methylene bis acrylamide in acrylamide solution, mix; The carbon quantum dot solution of adding 0.3-3wt%, the poly N-isopropyl acrylamide aqueous solution and the tetraethylethylenediamine of 0.5-2.5wt% in mixed solution are waited to dissolve the back and are added initiator, leave standstill to get final product in 3-8 hour.Preferably, the concentration of described carbon quantum dot solution is 0.9-2wt%, and the concentration of the described poly N-isopropyl acrylamide aqueous solution is 0.6-1.5wt%.
Described initiator is a kind of in thiosulphate or the persulphate.
The weight ratio of described acrylamide and N,N methylene bis acrylamide is 2-30:1; The concentration of described acrylamide solution is 0.01-1.5g/mL.Preferably, the weight ratio of described acrylamide and N,N methylene bis acrylamide is 3-15:1.
The weight ratio of described N,N methylene bis acrylamide, carbon quantum dot, poly N-isopropyl acrylamide, tetraethylethylenediamine is 1-6:1:50-200:0.1-2.
The amount ratio of the element sulphur in described carbon quantum dot and the initiator is 1g:2-10mmol.
The preparation method of described carbon quantum dot solution is,
A kind of with in Ovum Gallus domesticus album or the egg yolk is warming up to 220 ℃-280 ℃ and be incubated 1-3 hour under nitrogen atmosphere, after the cooling product is dissolved in the solvent, stirs to get supernatant liquid filtering behind 0.1-1 hour, centrifugation and get final product; Described solvent is deionized water, dehydrated alcohol, acetone, a kind of in dimethyl formamide or the chloroform.
The preparation method of described poly N-isopropyl acrylamide is,
N-N-isopropylacrylamide monomer, N,N methylene bis acrylamide are dissolved in the deionized water, feed nitrogen and stirring, add the persulfate solution post-heating to 60-80 ℃ and be incubated 3-5 hour, cooling, with the reaction solution centrifugation, taking precipitate is dry to get final product.
The weight ratio of described N-N-isopropylacrylamide monomer, N,N methylene bis acrylamide and persulphate is 1:0.005-0.03:0.01-0.07.
Can obtain the temperature-sensitive fluorescent carbon nano-composite material by above-mentioned preparation method.
The present invention is in acrylamide solution, add poly N-isopropyl acrylamide (PNIPAM) dispersion liquid that is mixed with the carbon quantum dot, with N, the N-methylene-bisacrylamide is linking agent, be accelerator with the Tetramethyl Ethylene Diamine, be initiator with thiosulphate or persulphate, at room temperature form the plural gel of half interpenetrating network structure.The carbon quantum dot makes gel have fluorescence, and the introducing of PNIPAM makes gel have temperature sensitive property, has increased the physical strength of half interpenetrating network structure behind the adding acrylamide.
Compared with prior art, beneficial effect of the present invention is:
(1) described temperature-sensitive fluorescent carbon nano-composite material adopts the carbon quantum dot as fluorescence source, has good fluorescence and temperature sensitive double-response performance, and nontoxic, environmental protection, good stability.
(2) described temperature-sensitive fluorescent carbon nano-composite material is the plural gel that has the half interpenetrating network structure of fluorescence and temperature sensitive property concurrently, and added acrylamide, make the physical strength of hydrogel obviously increase, and coating is relatively good, can be by applying or the printing film forming, can be used for weaving, chemical reaction control, the drug release hierarchy of control etc., the scope of application is wider.
(3) preparation technology of described temperature-sensitive fluorescent carbon nano-composite material is simple, and cost of material is cheap, and building-up process is nontoxic, pollution-free.
Description of drawings
Fig. 1 is that the fluorescence intensity of the temperature-sensitive fluorescent carbon nano-composite material that makes among the embodiment 1 is with variation of temperature figure.
Fig. 2 is that the temperature-sensitive fluorescent carbon nano-composite material that makes among the embodiment 1 is coated in the comparison diagram on the quartz substrate, and wherein Fig. 2 a is the picture under 20 ℃ sun exposure, and Fig. 2 b is the picture under UV-irradiation.
Embodiment
Below in conjunction with embodiment, the invention will be further described:
Embodiment 1
1, the preparation of carbon quantum dot solution:
Get 1g Ovum Gallus domesticus album heat-up rate with 10 ℃/min under nitrogen atmosphere and be warming up to 250 ℃, and be incubated 2 hours, naturally cool to room temperature, obtain black powder.The 0.1g black powder is dissolved in the deionized water of 10g, and the centrifugal 20min of 10000rpm behind the magnetic agitation 30min gets centrifuged supernatant with 200nm ultrafiltration membrance filter three times, and concentration is the carbon quantum dot solution of 1wt%, and is standby.
2, the preparation of poly N-isopropyl acrylamide (PNIPAM) solution:
Get 1.5g PNIPAM monomer and 0.0225g MBA is dissolved in the 150ml deionized water, feed nitrogen then, stir 30min under the room temperature.With K
2S
2O
8Solution (0.068g K
2S
2O
8Be dissolved in the 30ml deionized water) add above solution, be warming up to 70 ℃ and be incubated 4 hours under the nitrogen atmosphere.Solution after the polymerization is cooled to room temperature, is dispersed in deionized water, triplicate after 18000rpm is centrifugal.The polymerisate that obtains is made into the PNIPAM solution of 0.98wt%, standby.
3, the preparation of temperature-sensitive fluorescent carbon nano-composite material:
Get the deionized water that 0.76g acrylamide (AAm) is dissolved in 30mL, the N that adds 138mg, N-methylene-bisacrylamide (MBA), mixing back adding concentration is that 1wt% carbon quantum dot solution 3mL and concentration are the PNIPAM solution 3mL of 0.98wt%, drip the tetraethylethylenediamine (TEMED) of 13mg then, after treating to dissolve fully, add the hypo solution 4mL of 28mmol/L at last, left standstill under the room temperature condition 7 hours, and can obtain the temperature-sensitive fluorescent carbon nano-composite material.
With the temperature-sensitive fluorescent carbon nano-composite material in the present embodiment, under 20 ℃ of daylight, be the homogeneous transparent shape, place under the ultraviolet lamp, send stronger blue-fluorescence; During with its heating in water bath to 40 ℃, be creamy white, place under the ultraviolet lamp, the blue-fluorescence that sends obviously weakens, and illustrates that matrix material has good temperature sensitive fluorescent characteristic.
Fig. 1 for the fluorescence intensity of the temperature-sensitive fluorescent carbon nano-composite material that makes in the present embodiment with variation of temperature figure, as can be seen from Figure, the matrix material that makes has fluorescence, and along with the rising of temperature, the fluorescence intensity of matrix material reduces gradually, illustrates that the matrix material that makes has responsiveness to temperature.
Fig. 2 is for to be coated in the temperature-sensitive fluorescent carbon nano-composite material that makes in the present embodiment on the quartz substrate, respectively 20 ℃ daylight (specifically see Fig. 2 a) and UV-light (specifically seeing Fig. 2 b) under comparison diagram, as can be seen from Figure, under the daylight, matrix material is transparence, under the irradiation of UV-light, sends fluorescence, and can be coated on the quartz substrate well, but illustrate that the matrix material that makes has coating.
The viscosity of the temperature-sensitive fluorescent carbon nano-composite material that makes in the test present embodiment, its viscosity number is 380cP, has both had certain mechanical strength, has and has good coating.
Embodiment 2
1, the preparation of carbon quantum dot solution:
Get 1g egg yolk heat-up rate with 10 ℃/min under nitrogen atmosphere and be warming up to 250 ℃, and be incubated 2 hours, naturally cool to room temperature, obtain black powder.The 0.1g black powder is dissolved in the dehydrated alcohol of 10g, the centrifugal 20min of 10000rpm behind the magnetic agitation 30min gets centrifuged supernatant 200nm ultrafiltration membrance filter three times, and concentration is the carbon quantum dot solution of 1wt%, and is standby.
2, the preparation method of poly N-isopropyl acrylamide (PNIPAM) solution is with embodiment 1.
3, the preparation of temperature-sensitive fluorescent carbon nano-composite material:
Get the deionized water that 0.89g acrylamide (AAm) is dissolved in 30mL, the N that adds 138mg, N-methylene-bisacrylamide (MBA), mixing back adding concentration is that 1wt% carbon quantum dot solution 3mL and concentration are the PNIPAM solution 3mL of 0.98wt%, drip the tetraethylethylenediamine (TEMED) of 12mg then, after treating to dissolve fully, add the hypo solution 4mL of 28mmol/L at last, left standstill under the room temperature condition 7 hours, and can obtain the temperature-sensitive fluorescent carbon nano-composite material.
Embodiment 3
1, the preparation method of carbon quantum dot solution is with embodiment 1:
2, the preparation method of poly N-isopropyl acrylamide (PNIPAM) solution is with embodiment 1.
3, the preparation of temperature-sensitive fluorescent carbon nano-composite material:
Get the deionized water that 0.94g acrylamide (AAm) is dissolved in 30mL, the N that adds 138mg, N-methylene-bisacrylamide (MBA), mixing back adding concentration is that 1wt% carbon quantum dot solution 5mL and concentration are the PNIPAM solution 3mL of 0.98wt%, drip the tetraethylethylenediamine (TEMED) of 13mg then, after treating to dissolve fully, add the thiosulfuric acid potassium solution 4mL of 28mmol/L at last, left standstill under the room temperature condition 6 hours, and can obtain the temperature-sensitive fluorescent carbon nano-composite material.
Embodiment 4
1, the preparation method of carbon quantum dot solution is with embodiment 1:
2, the preparation method of poly N-isopropyl acrylamide (PNIPAM) solution is with embodiment 1.
3, the preparation of temperature-sensitive fluorescent carbon nano-composite material:
Get the deionized water that 0.42g acrylamide (AAm) is dissolved in 30mL, the N that adds 138mg, N-methylene-bisacrylamide (MBA), mixing back adding concentration is that 1wt% carbon quantum dot solution 5mL and concentration are the PNIPAM solution 3mL of 0.98wt%, drip the tetraethylethylenediamine (TEMED) of 13mg then, after treating to dissolve fully, add the ammonium persulfate solution 4mL of 28mmol/L at last, left standstill under the room temperature condition 7 hours, and can obtain the temperature-sensitive fluorescent carbon nano-composite material.
The above is preferred embodiment of the present invention, but the present invention should not be confined to the disclosed content of this embodiment.So everyly do not break away from the equivalence of finishing under the spirit disclosed in this invention or revise, all fall into the scope of protection of the invention.
Claims (10)
1. the preparation method of a temperature-sensitive fluorescent carbon nano-composite material, its step comprises: add N,N methylene bis acrylamide in acrylamide solution, mix; In mixed solution, add the carbon quantum dot solution of 0.3-3wt%, the poly N-isopropyl acrylamide aqueous solution and the tetraethylethylenediamine of 0.5-2.5wt%, wait to dissolve the back and add initiator, left standstill 3-8 hour.
2. the preparation method of temperature-sensitive fluorescent carbon nano-composite material according to claim 1 is characterized in that: described initiator is a kind of in thiosulphate or the persulphate.
3. the preparation method of temperature-sensitive fluorescent carbon nano-composite material according to claim 1, it is characterized in that: the weight ratio of described acrylamide and N,N methylene bis acrylamide is 2-30:1; The concentration of described acrylamide solution is 0.01-1.5g/mL.
4. the preparation method of temperature-sensitive fluorescent carbon nano-composite material according to claim 1, it is characterized in that: the weight ratio of described N,N methylene bis acrylamide, carbon quantum dot, poly N-isopropyl acrylamide, tetraethylethylenediamine is 1-6:1:50-200:0.1-2.
5. the preparation method of temperature-sensitive fluorescent carbon nano-composite material according to claim 2, it is characterized in that: the amount ratio of the element sulphur in described carbon quantum dot and the initiator is 1g:2-10mmol.
6. the preparation method of temperature-sensitive fluorescent carbon nano-composite material according to claim 1, it is characterized in that: the concentration of described carbon quantum dot solution is 0.9-2wt%, the concentration of the described poly N-isopropyl acrylamide aqueous solution is 0.6-1.5wt%.
7. the preparation method of temperature-sensitive fluorescent carbon nano-composite material according to claim 1 is characterized in that: the preparation method of described carbon quantum dot solution is,
A kind of with in Ovum Gallus domesticus album or the egg yolk is warming up to 220 ℃-280 ℃ and be incubated 1-3 hour under nitrogen atmosphere, after the cooling product is dissolved in the solvent, gets supernatant liquid filtering after stirring 0.1-1 hour, centrifugation; Described solvent is a kind of in deionized water, dehydrated alcohol, acetone, dimethyl formamide or the chloroform.
8. the preparation method of temperature-sensitive fluorescent carbon nano-composite material according to claim 1 is characterized in that: the preparation method of described poly N-isopropyl acrylamide is,
N-N-isopropylacrylamide monomer, N,N methylene bis acrylamide are dissolved in the deionized water, feed nitrogen and stirring, add the persulfate solution post-heating to 60-80 ℃ and be incubated 3-5 hour, cooling, with the reaction solution centrifugation, the taking precipitate drying.
9. the preparation method of temperature-sensitive fluorescent carbon nano-composite material according to claim 8, it is characterized in that: the weight ratio of described N-N-isopropylacrylamide monomer, N,N methylene bis acrylamide and persulphate is 1:0.005-0.03:0.01-0.07.
10. a temperature-sensitive fluorescent carbon nano-composite material is characterized in that: by each described method preparation among the claim 1-9.
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| CN105131207A (en) * | 2015-07-16 | 2015-12-09 | 复旦大学 | Core halo/core-shell halo structure fluorescent microgel having double responsiveness and preparation method thereof |
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Application publication date: 20130717 |