CN107938321A - A kind of fiber solid support method of fluorescence carbon nanomaterial - Google Patents
A kind of fiber solid support method of fluorescence carbon nanomaterial Download PDFInfo
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- CN107938321A CN107938321A CN201711233493.3A CN201711233493A CN107938321A CN 107938321 A CN107938321 A CN 107938321A CN 201711233493 A CN201711233493 A CN 201711233493A CN 107938321 A CN107938321 A CN 107938321A
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
- D06M11/74—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/02—Use of particular materials as binders, particle coatings or suspension media therefor
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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
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/65—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing carbon
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Abstract
The invention discloses a kind of fiber solid support method of fluorescence carbon nanomaterial.Functional fibre is added in solvent orange 2 A first and is swollen, the functional fibre after being swollen；Fluorescence carbon nanomaterial is scattered in solvent B, the functional fibre then added after swelling stirs evenly；Mixing material heating reaction after stirring evenly, reaction postcooling to room temperature；Product washing after cooling, is dried in vacuo after washing, the immobilized fluorescence carbon nanomaterial of fiber is obtained after dry.Technical solution of the present invention can effectively overcome separation of the fluorescence carbon nanomaterial in the application process of the field such as fluorescence probe, photocatalysis and recycle problem, solve the problems, such as that fluorescence carbon nanomaterial is immobilized after fluorescent quenching.
Description
First, technical field：
The present invention relates to a kind of solid support method of fluorescence carbon nanomaterial, more particularly to a kind of fluorescence carbon nanomaterial
Fiber solid support method.
2nd, background technology：
Compared with traditional semiconductor-quantum-point and fluorescent dye, fluorescence carbon nanomaterial has nontoxic, inexpensive, anti-light
Drift, excellent chemical stability and the advantages that biocompatibility, in fluorescence probe, bio-imaging, fluorescent ink, semiconductor hair
Light, solar cell and photocatalysis field have certain application prospect, particularly in photocatalysis field, fluorescence carbon nanomaterial
Photoresponse scope is wider (from ultraviolet to near-infrared), and available sunlight is more.Therefore, it is catalyzed in visible ray and near infrared light
Aspect has wide application value and prospect.
It is difficult recycling and repetition in use although fluorescence carbon nanomaterial has excellent photocatalysis performance
Utilize, and difficulty is separated with product, so as to seriously limit the practical application of fluorescence carbon nanomaterial in the industry.Will catalysis
Agent is immobilized to being effective way for solving the problems, such as catalyst recycling and recycling on segregative porous material or fibrous material
Footpath；But serious fluorescent quenching phenomenon occurs in fluorescence carbon nanomaterial under solid conditions, urged so as to substantially reduce its light
Change activity.Therefore, common inorganic catalyst support can not efficiently solve practical problem.Patent CN105713607A is disclosed
The preparation and application of the mesoporous silicon oxide polypropylene cyanogen core-shell nano tunica fibrosa of load carbon quantum dot, the method belong to physics
Load, easily comes off and fluorescent quenching.The immobilized starting stage also in research at present of fluorescence carbon nanomaterial is, it is necessary to solve
Two key issues be influence less carrier and fluorescence carbon nanomaterial of the selection to fluorescence carbon nanomaterial optical property
With the combination of carrier.
3rd, the content of the invention：
The technical problem to be solved in the present invention is：In order to overcome fluorescence carbon nanomaterial to be led in fluorescence probe, photocatalysis etc.
In the application process of domain separate and recycle problem, solves the problems, such as fluorescence carbon nanomaterial it is immobilized after fluorescent quenching technology,
Invention provides a kind of fiber solid support method of new fluorescence carbon nanomaterial.Technical solution of the present invention utilizes the mode effectively heated
Fluorescence carbon nanomaterial is immobilized on functional fibre by chemical bond, so as to efficiently solve fluorescence carbon nanomaterial in fluorescence
The fluorescence using problem and fluorescence carbon nanomaterial after immobilized for separating and circulating in the application process of the field such as probe, photocatalysis
Quenching technique problem.
To solve the above-mentioned problems, the present invention adopts the technical scheme that：
The present invention provides a kind of fiber solid support method of fluorescence carbon nanomaterial, and the solid support method comprises the following steps：
A, functional fibre is added in solvent orange 2 A first and is swollen, swelling time is 1~48h, filters solvent orange 2 A after swelling
Go out, the functional fibre after being swollen；The mass volume ratio (g/ml) of the functional fibre and solvent orange 2 A is 1：10~100；
B, by fluorescence carbon nanomaterial ultrasonic disperse in solvent B, the functional fibre stirring after step a swellings is then added
Uniformly；Mass ratio between functional fibre and the fluorescence carbon nanomaterial is 1：0.01~1；
C, the step b mixing materials stirred evenly are heated to 40~180 DEG C, under this temperature conditions react 1~
48h, is cooled to room temperature after reaction；
D, step c products after cooling are fully washed, is dried in vacuo after washing, obtaining fiber after dry consolidates
The fluorescence carbon nanomaterial of load.
According to the fiber solid support method of above-mentioned fluorescence carbon nanomaterial, solvent orange 2 A described in step a is water, ethanol, dichloro
At least one of ethane, n,N-Dimethylformamide, dimethyl sulfoxide (DMSO) and nitrobenzene.
According to the fiber solid support method of above-mentioned fluorescence carbon nanomaterial, functional fibre described in step a for faintly acid from
Sub- exchange fiber or Weak-alkaline ion exchange fibre.
The weak acid ion exchange fiber that the present invention uses is according to 200410060275.0 (proprietary term of Patent No. CN
Referred to as：The preparation method of ion-exchange fibre and its fabric) patent of invention specification in embodiment 1-10 prepare Hydrogen from
Sub- exchange fiber.
The Weak-alkaline ion exchange fibre that the present invention uses is (patent name is according to Patent No. CN 95116025.7：
Acid-gas adsorbing fibre and its preparation process and device) patent of invention specification in embodiment 1-3 prepare adsorbing fiber
Or according to document the preparation of Weak-alkaline ion exchange fibre " and to salicylic absorption property " (polymer material science and work
Journey, 2015,31 (1)：78-87) the adsorbing fiber prepared.
According to the fiber solid support method of above-mentioned fluorescence carbon nanomaterial, swelling time described in step a is 6~24h.
According to the fiber solid support method of above-mentioned fluorescence carbon nanomaterial, fluorescence carbon nanomaterial described in step b is carbon
Quantum dot, graphene oxide quantum dot, graphene quantum dot or carbon dots.
According to the fiber solid support method of above-mentioned fluorescence carbon nanomaterial, solvent B described in step b is water, ethanol, first
At least one of alcohol, dichloroethanes, n,N-Dimethylformamide, dimethyl sulfoxide (DMSO) and nitrobenzene.
According to the fiber solid support method of above-mentioned fluorescence carbon nanomaterial, the reaction time is 6~24h in step c.
According to the fiber solid support method of above-mentioned fluorescence carbon nanomaterial, the mode of heat temperature raising adds for oil bath in step c
Heat, hydrothermal reaction kettle heating, Microwave-assisted firing or ultrasonic wave added heating.
According to the fiber solid support method of above-mentioned fluorescence carbon nanomaterial, used solvent when fully being washed in step d
For at least one of water, methanol, ethanol and acetone.
According to the fiber solid support method of above-mentioned fluorescence carbon nanomaterial, vacuum is when being dried in vacuo described in step d
0.08Mpa, drying temperature are 40~100 DEG C, and drying time is 4~48h.
The positive beneficial effect of the present invention：
1st, the present invention is first matrix using functional fibre, is received using the amino on functional fibre or carboxyl with fluorescent carbon
The reaction of rice material surface carboxyl or amido functional group is effectively immobilized by fluorescence carbon nanomaterial, and keeps fluorescent carbon nanometer
The original fluorescence of material and catalytic performance.The fluorescence carbon nanomaterial obtained after immobilized in use, fluorescent carbon nanometer material
Material be able to can be efficiently separated by simply filtering or centrifuging, and the fluorescence carbon nanomaterial after separation can be further
Regeneration cycle uses.Therefore, technical solution of the present invention can effectively overcome fluorescence carbon nanomaterial in fluorescence probe, photocatalysis
Deng the separation in the application process of field and recycle problem, solve the problems, such as fluorescence carbon nanomaterial it is immobilized after fluorescent quenching.
2nd, the present invention can use multiple heating mode, effective combination of fluorescence carbon nanomaterial be realized, by heating side
Formula and time can regulate and control supported quantity of the fluorescence carbon nanomaterial on functional fibre.
3rd, technical solution of the present invention passes through verification experimental verification, and mature and stable, reaction process is simple and convenient to operate, the time is short, energy
Consume it is low, be easily handled, pollute it is small.Functional fibre after immobilized fluorescence carbon nanomaterial can not only keep fluorescence carbon nanomaterial
Fluorescence property, the pattern of functional fibre shape, structurally and mechanically performance can also be kept.
4th, illustrate：
The scanning electron microscopic picture of the gained load fluorescence carbon nanomaterial of Fig. 1 embodiment of the present invention 1；
In Fig. 1：A) scanning electron microscopic picture under 500 and 5000 times, b and c) for Weak-alkaline ion exchange fibre are amplified) and
D) scanning electron microscopic picture under 500 and 5000 times is amplified for the immobilized fluorescent carbon quantum dot of the fiber prepared.Can from Fig. 1
Go out：Fibre diameter loads the fiber entirety pattern after fluorescent carbon quantum dot and form does not change significantly, say at 20 μm or so
The stability and satisfactory mechanical property of light fibers.
1 fluorescence carbon nanomaterial (i.e. carbon quantum dot) of Fig. 2 embodiment of the present invention and fiber-loaded rear fluorescence carbon nanomaterial
The excitation spectrum (em=460nm) of (i.e. the immobilized carbon quantum dot of fiber)；
The fiber (i.e. the immobilized carbon quantum dot of gained fiber) that Fig. 3 embodiment of the present invention 1 loads fluorescence carbon nanomaterial exists
Emission spectrum under different wave length excitation.
It can be illustrated by Fig. 3：Fluorescence is nanometer carbon material supported have been arrived on fiber, and keeps fluorescence property.
Fluorescence spectrum of Fig. 4 functional fibre load fluorescence carbon nanomaterials of the present invention to various concentrations Cr VI.
Figure 4, it is seen that with the increase of hexavalent chromium concentration, the fluorescence for loading the fiber of fluorescence carbon nanomaterial is strong
Degree is gradually reduced.
5th, embodiment：
The present invention is further explained with reference to embodiments, but is not intended to limit the technology contents that the present invention is protected.
Embodiment 1：
The fiber solid support method of fluorescence carbon nanomaterial of the present invention, the detailed step of the solid support method are as follows：
A, by 5g Weak-alkaline ion exchange fibres, (Weak-alkaline ion exchange fibre is according to Patent No. CN first
The adsorbing fiber that embodiment 1 is prepared in 95116025.7 patent of invention specification) add 100ml water in be swollen,
Swelling time is 1h, filters out solvent after swelling, the Weak-alkaline ion exchange fibre after being swollen；
B, by 0.05g carbon quantum dots ultrasonic disperse in 50mL water, the weakbase ion then added after step a swellings is handed over
Fiber is changed to stir evenly；
C, the mixing material oil bath heating that step b is stirred evenly is warming up to 40 DEG C, reacts 48h under this temperature conditions,
It is cooled to room temperature after reaction；
D, step c products after cooling are fully washed with water and ethanol successively, (vacuum is dried in vacuo after washing
For 0.08Mpa, drying temperature is 40 DEG C, drying time 48h), obtain the immobilized fluorescent carbon quantum dot of fiber after dry.
Embodiment 2：
The fiber solid support method of fluorescence carbon nanomaterial of the present invention, the detailed step of the solid support method are as follows：
A, by 0.1g weak acid ions exchange fiber, (the weak acid ion exchange fiber is according to Patent No. CN first
The form ion exchange fiber that embodiment 3 is prepared in 200410060275.0 patent of invention specification) add 20ml bis-
It is swollen in chloroethanes, swelling time 48h, filters out solvent after swelling, and the weak acid ion after being swollen exchanges fine
Dimension；
B, by 0.1g graphene oxide quantum dots ultrasonic disperse in the mixed solution of 10mL water and ethanol, step is then added
Weak acid ion exchange fiber after rapid a swellings stirs evenly；
C, the step b mixing materials stirred evenly are transferred in 50ml hydrothermal reaction kettles, are heated to 180 DEG C, herein
1h is reacted under temperature conditionss, is cooled to room temperature after reaction；
D, step c products after cooling are fully washed using water, methanol, ethanol and acetone successively, washing is laggard
Row vacuum drying (vacuum 0.08Mpa, drying temperature are 60 DEG C, drying time 40h), it is immobilized to obtain fiber after dry
Graphene oxide quantum dot.
Embodiment 3：
The fiber solid support method of fluorescence carbon nanomaterial of the present invention, the detailed step of the solid support method are as follows：
A, by 1g weak acid ions exchange fiber, (the weak acid ion exchange fiber is according to Patent No. CN first
The form ion exchange fiber that embodiment 1 is prepared in 200410060275.0 patent of invention specification) add 50ml nitre
It is swollen in base benzene, swelling time 24h, filters out solvent after swelling, the weak acid ion exchange fiber after being swollen；
B, by 0.2g graphene quantum dots ultrasonic disperse in the mixing of 30mL n,N-Dimethylformamide and dimethyl sulfoxide (DMSO)
In solution, the weak acid ion exchange fiber then added after step a swellings stirs evenly；
C, the step b mixing materials stirred evenly are placed in microwave reactor, are heated to 140 DEG C, in this temperature
Under the conditions of react 2h, be cooled to room temperature after reaction；
D, step c products after cooling are fully washed using water, ethanol and acetone successively, vacuum is carried out after washing
Dry (vacuum 0.08Mpa, drying temperature are 80 DEG C, drying time 12h), the immobilized graphene of fiber is obtained after dry
Quantum dot.
Embodiment 4：
The fiber solid support method of fluorescence carbon nanomaterial of the present invention, the detailed step of the solid support method are as follows：
A, by 2g Weak-alkaline ion exchange fibres, (Weak-alkaline ion exchange fibre is according to special document " alkalescent first
The preparation of ion-exchange fibre and to salicylic absorption property " (polymer material science and engineering, 2015,31 (1)：78-
87) adsorbing fiber being prepared) add 100ml n,N-Dimethylformamide and dimethyl sulfoxide (DMSO) mixed solution (the two
Volume ratio is 1:1) it is swollen in, swelling time 15h, filters out solvent after swelling, the weakbase ion after being swollen
Exchange fiber；
B, by 1g carbon dotss ultrasonic disperse in the mixed solution of 50mL ethanol and methanol, after then adding step a swellings
Weak-alkaline ion exchange fibre stirs evenly；
C, the step b mixing materials stirred evenly are placed in microwave reactor, are heated to 80 DEG C, in this temperature strip
4h is reacted under part, is cooled to room temperature after reaction；
D, step c products after cooling are fully washed using water, ethanol and acetone successively, vacuum is carried out after washing
Dry (vacuum 0.08Mpa, drying temperature are 100 DEG C, drying time 4h), the immobilized carbon dots of fiber is obtained after dry.
Embodiment 5：
The fiber solid support method of fluorescence carbon nanomaterial of the present invention, the detailed step of the solid support method are as follows：
A, by 3g Weak-alkaline ion exchange fibres, (Weak-alkaline ion exchange fibre is according to Patent No. CN first
The adsorbing fiber that embodiment 3 is prepared in 95116025.7 patent of invention specification) add 150ml ethanol in carry out it is molten
Swollen, swelling time 24h, filters out solvent after swelling, the Weak-alkaline ion exchange fibre after being swollen；
B, by 0.5g carbon dotss ultrasonic disperse in 50mL ethanol, the weakbase ion then added after step a swellings exchanges
Fiber stirs evenly；
C, the step b mixing materials stirred evenly are placed in ultrasonic reactor, are heated to 80 DEG C, in this temperature strip
8h is reacted under part, is cooled to room temperature after reaction；
D, step c products after cooling are fully washed using water, ethanol and acetone successively, vacuum is carried out after washing
Dry (vacuum 0.08Mpa, drying temperature are 40 DEG C, drying time 48h), the immobilized carbon dots of fiber is obtained after dry.
Embodiment 6：
The fiber solid support method of fluorescence carbon nanomaterial of the present invention, the detailed step of the solid support method are as follows：
A, by 2g weak acid ions exchange fiber, (the weak acid ion exchange fiber is according to Patent No. CN first
The form ion exchange fiber that embodiment 5 is prepared in 200410060275.0 patent of invention specification) add 80ml bis-
It is swollen in chloroethanes, swelling time 25h, filters out solvent after swelling, and the weak acid ion after being swollen exchanges fine
Dimension；
B, by 0.3g graphene oxide quantum dots ultrasonic disperse in 70mL n,N-Dimethylformamide, step is then added
Weak acid ion exchange fiber after rapid a swellings stirs evenly；
C, the step b mixing materials stirred evenly are transferred in 100ml hydrothermal reaction kettles, are heated to 140 DEG C,
10h is reacted under this temperature conditions, is cooled to room temperature after reaction；
D, step c products after cooling are fully washed using water, ethanol and acetone successively, vacuum is carried out after washing
Dry (vacuum 0.08Mpa, drying temperature are 40 DEG C, drying time 48h), the immobilized oxidation stone of fiber is obtained after dry
Black alkene quantum dot.
Embodiment 7
The immobilized fluorescent carbon quantum dot of fiber prepared by 0.05g embodiments 1 is weighed in the different Cr VI of 20ml concentration
In solution, 25 DEG C of constant temperature oscillation 4h, filter out fiber, are washed with water to and can't detect Cr VI, 80 DEG C of vacuum drying 5h (vacuum
Spend for 0.08Mpa)；Dried sample is used into the FLSP920 type modular fluorometer service lifes using Edinburgh, Britain Instrument Corporation
Fluorescence analysis is carried out with steady-state fluorescence spectrometer, as shown in figure 4, with the increase of hexavalent chromium concentration, loads fluorescent carbon nanometer material
The fluorescence intensity of the fiber of material is gradually reduced.
Claims (10)
1. a kind of fiber solid support method of fluorescence carbon nanomaterial, it is characterised in that the solid support method comprises the following steps：
A, functional fibre is added in solvent orange 2 A first and is swollen, swelling time is 1~48h, filters out solvent orange 2 A after swelling, obtains
Functional fibre after to swelling；The mass volume ratio of the functional fibre and solvent orange 2 A is 1：10~100；
B, by fluorescence carbon nanomaterial ultrasonic disperse in solvent B, it is equal then to add the functional fibre stirring after step a swellings
It is even；Mass ratio between functional fibre and the fluorescence carbon nanomaterial is 1：0.01~1；
C, the step b mixing materials stirred evenly are heated to 40~180 DEG C, 1~48h are reacted under this temperature conditions,
It is cooled to room temperature after reaction；
D, step c products after cooling are fully washed, is dried in vacuo after washing, it is immobilized to obtain fiber after dry
Fluorescence carbon nanomaterial.
2. the fiber solid support method of fluorescence carbon nanomaterial according to claim 1, it is characterised in that：Described in step a
Solvent orange 2 A is at least one of water, ethanol, dichloroethanes, n,N-Dimethylformamide, dimethyl sulfoxide (DMSO) and nitrobenzene.
3. the fiber solid support method of fluorescence carbon nanomaterial according to claim 1, it is characterised in that：Described in step a
Functional fibre is weak acid ion exchange fiber or Weak-alkaline ion exchange fibre.
4. the fiber solid support method of fluorescence carbon nanomaterial according to claim 1, it is characterised in that：Described in step a
Swelling time is 6~24h.
5. the fiber solid support method of fluorescence carbon nanomaterial according to claim 1, it is characterised in that：Described in step b
Fluorescence carbon nanomaterial is carbon quantum dot, graphene oxide quantum dot, graphene quantum dot or carbon dots.
6. the fiber solid support method of fluorescence carbon nanomaterial according to claim 1, it is characterised in that：Described in step b
Solvent B is at least one of water, ethanol, methanol, dichloroethanes, n,N-Dimethylformamide, dimethyl sulfoxide (DMSO) and nitrobenzene.
7. the fiber solid support method of fluorescence carbon nanomaterial according to claim 1, it is characterised in that：Reacted in step c
Time is 6~24h.
8. the fiber solid support method of fluorescence carbon nanomaterial according to claim 1, it is characterised in that：Heated in step c
The mode of heating is oil bath heating, hydrothermal reaction kettle heats, Microwave-assisted firing or ultrasonic wave added heat.
9. the fiber solid support method of fluorescence carbon nanomaterial according to claim 1, it is characterised in that：In step d fully
Used solvent is at least one of water, methanol, ethanol and acetone during washing.
10. the fiber solid support method of fluorescence carbon nanomaterial according to claim 1, it is characterised in that：Described in step d
Vacuum is 0.08Mpa during vacuum drying, and drying temperature is 40~100 DEG C, and drying time is 4~48h.
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