CN107974131A - A kind of carbon dots ink and its preparation method and application - Google Patents
A kind of carbon dots ink and its preparation method and application Download PDFInfo
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- CN107974131A CN107974131A CN201711136053.6A CN201711136053A CN107974131A CN 107974131 A CN107974131 A CN 107974131A CN 201711136053 A CN201711136053 A CN 201711136053A CN 107974131 A CN107974131 A CN 107974131A
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- carbon dots
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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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/50—Sympathetic, colour changing or similar inks
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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
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/16—Writing inks
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- G—PHYSICS
- G06—COMPUTING; CALCULATING OR COUNTING
- G06F—ELECTRIC DIGITAL DATA PROCESSING
- G06F21/00—Security arrangements for protecting computers, components thereof, programs or data against unauthorised activity
- G06F21/60—Protecting data
- G06F21/602—Providing cryptographic facilities or services
Abstract
The invention discloses a kind of carbon dots ink and its preparation method and application, carbon dots is obtained as raw material using cation type polymer electrolyte and anionic polymer electrolyte, then carbon dots ink is prepared in a manner of self assembly, manufacturing cost is cheap, preparation process is simple, environmentally protective, compared to traditional fluorescent ink, the carbon dots ink that the present invention is prepared has the stability of higher, has great application prospect in the field such as data message encryption and typographical display.
Description
Technical field
The present invention relates to carbon nanomaterial field, more particularly, to a kind of carbon dots ink and its preparation method and application.
Background technology
Information security issue in economic, military, politics and daily life is increasingly valued by people.In recent years
Come, scientific research personnel develops a series of correlation techniques, and such as plasma-based safety label, magnetic response and luminescence imaging protect these heavy
Want, valuable data are not destroyed and forge.Wherein, fluorescence imaging has many significant advantages, including prepares easy, easy
In operation and high yield etc., it is widely used in data confidentiality.
Fluorescence imaging can become data record, secrecy and false proof powerful technique, be mostly derived from varied fluorescence
The appearance of material.It is reported that some fluorescent materials such as fluorescent crystal, transient metal complex, dyestuff etc. can by exterior machinery,
Heat and steam stimulation technology are applied to optical data recording, equipment protection, sensor matrices etc..But most of materials are potential
Bio-toxicity, low light resistance, high cost and low stability hinder its practical application.
As a kind of emerging nano material, fluorescent carbon point is because of its environmental protection, extensive chemical inertia, hypotoxicity, fabulous biology
The unique advantages such as compatibility, remarkable chemical photostability and excellent photoelectric properties, are urged in bio-imaging, light recently
Change, is of increased attention in terms of sensing, optoelectronic device and other application.Substantial amounts of research all concentrates on carbon dots at present
Preparation on.Wherein, the hydro-thermal reaction of carbon matrix precursor with its green, economic and easy to operate advantage by more and more extensive profit
With.All there is hydrophilic radical by most of carbon dots of Hydrothermal Synthesiss, so water can be dissolved in well, this characteristic has very much
Beneficial to the application such as such as bio-imaging, medical diagnosis and ink imaging.But this kind of carbon dots is typically due to carbon dots surface group and base
Weaker Van der Waals force and affinity cause serious unstability of the material to water or organic solvent between bottom, so that can not be wet
Practical application in the environment that degree, temperature change at any time.
The content of the invention
The technical problems to be solved by the invention are to provide a kind of preparation method of carbon dots ink, of low cost, prepare
Journey is simple, efficient, and the carbon dots ink being prepared is environmentally friendly, stability is high, can be applied to data message encryption and typographical display
Deng field.
The technical solution used in the present invention is：
The present invention provides a kind of preparation method of carbon dots ink, comprises the following steps：
Cation type polymer electrolyte is taken, solvent is added, is transferred in reaction kettle and is reacted to obtain solution one；
Take bag filter to dialyse solution one, collect the solution outside osmotic bag, be dried to obtain carbon dots one；
Anionic polymer electrolyte is taken, solvent is added, is transferred in reaction kettle and is reacted to obtain solution two；
Take bag filter to dialyse solution two, collect the solution outside osmotic bag, be dried to obtain carbon dots two；
Take carbon dots one to add solvent and be configured to solution three, take carbon dots two to add solvent and be configured to solvent four, mixed solution three
Carbon dots ink is prepared with solution four, ion institute's charge number of the solution three and the ion institute of the solution four are electrically charged
Number is identical.
Preferably, the cation type polymer electrolyte is polyallylamine hydrochloride, polyethyleneimine, polydiene propyl group
At least one of alkyl dimethyl ammonium chloride.
Preferably, the anionic polymer electrolyte is at least one of kayexalate, polyacrylic acid.
Preferably, the solvent is deionized water.
Preferably, molecular cut off≤3500 of the bag filter.
Preferably, the temperature reacted in a kettle is 150~250 DEG C.
Preferably, the reaction time is >=5h in a kettle.
Preferably, the time of dialysis is >=48h.
The present invention also provides a kind of carbon dots ink, is made by the preparation method of above-mentioned carbon dots ink.
Application of the above-mentioned carbon dots ink in data message encryption and typographical display field.
The beneficial effects of the invention are as follows：
The present invention provides a kind of preparation method of carbon dots ink, passes through certainly by raw material of the carbon dots solution with opposite charges
Prepared by main dress method, of low cost, reaction condition is gentle, environmentally protective, preparation process is simple, is obtained by preparation method of the present invention
For the carbon dots ink arrived in addition to the optical property with conventional fluorescent ink, the data write in paper have the stabilization of higher
Property, it can be applied to the fields such as data message encryption and typographical display.
Brief description of the drawings
Fig. 1 is that carbon dots ink prepares schematic diagram in embodiment 1；
Fig. 2 is the TEM shape appearance figures of carbon dots ink in embodiment 1；
Fig. 3 is fluorescence spectra of the carbon dots ink under different excitation wavelengths in embodiment 1；
Fig. 4 is the stability test of the carbon dots ink of the present invention.
Embodiment
Clearly and completely retouched below with reference to the technique effect of the design of embodiment and attached drawing to the present invention and generation
State, to be completely understood by the purpose of the present invention, feature and effect.Obviously, described embodiment is the part of the present invention
Embodiment, rather than whole embodiments, based on the embodiment of the present invention, those skilled in the art is not making the creative labor
On the premise of the other embodiment that is obtained, belong to the scope of protection of the invention.
Embodiment 1
Weigh 10g polyallylamine hydrochlorides (PAH) to be dissolved in 10mL deionized waters, 30mL poly- four is transferred to after ultrasonic dissolution
In the reaction kettle of vinyl fluoride liner, when reaction 5 is small in 200 DEG C of baking ovens.Using the bag filter that molecular cut off is 3500 to upper
State the solution that reaction obtains and carry out dialysis three days, to remove as reaction raw materials and intermediate product, collect the solution outside bag filter
It is freeze-dried, obtains powdered carbon dots one.
Weigh 10g kayexalates (PSS) to be dissolved in 10mL deionized waters, 30mL poly- four is transferred to after ultrasonic dissolution
In the reaction kettle of vinyl fluoride liner, when reaction 5 is small in 200 DEG C of baking ovens.Using the bag filter that molecular cut off is 3500 to upper
State the solution that reaction obtains and carry out dialysis three days, to remove as reaction raw materials and intermediate product, collect the solution outside bag filter
It is freeze-dried, obtains powdered carbon dots two.
Take carbon dots one to be dissolved in deionized water and obtain solution one, take carbon dots two to be dissolved in deionized water and obtain solution two, according to molten
Cationic charge number in the quality and solution one of liquid one in polyelectrolyte repetitive unit molecular weight calculation solution one, according to solution
Anionic charge number in two quality and solution two in polyelectrolyte repetitive unit molecular weight calculation solution two, according to working as gauge
Calculate the addition of control carbon dots one and carbon dots two so that solution one is suitable with the ionic charge number in solution two, mixed solution one
Carbon dots ink is obtained with solution two.
Embodiment 2
Weigh 10g polyallylamine hydrochlorides (PAH) to be dissolved in 10mL deionized waters, 30mL poly- four is transferred to after ultrasonic dissolution
In the reaction kettle of vinyl fluoride liner, when reaction 8 is small in 150 DEG C of baking ovens.Using the bag filter that molecular cut off is 2000 to upper
State the solution that reaction obtains and carry out dialysis four days, to remove as reaction raw materials and intermediate product, collect the solution outside bag filter
It is freeze-dried, obtains powdered carbon dots one.
Weigh 10g kayexalates (PSS) to be dissolved in 10mL deionized waters, 30mL poly- four is transferred to after ultrasonic dissolution
In the reaction kettle of vinyl fluoride liner, when reaction 8 is small in 150 DEG C of baking ovens.Using the bag filter that molecular cut off is 2000 to upper
State the solution that reaction obtains and carry out dialysis three days, to remove as reaction raw materials and intermediate product, collect the solution outside bag filter
It is freeze-dried, obtains powdered carbon dots two.
Take carbon dots one to be dissolved in deionized water and obtain solution one, take carbon dots two to be dissolved in deionized water and obtain solution two, control adds
The carbon dots one and the addition of carbon dots two entered causes the charge number of the ion institute band in solution one and the ion institute band in solution two
Charge number is identical, and mixed solution one and solution two obtain carbon dots ink.
Embodiment 3
Weigh 10g polyethyleneimines (PEI) to be dissolved in 10mL deionized waters, 30mL polytetrafluoroethyl-nes are transferred to after ultrasonic dissolution
In the reaction kettle of alkene liner, when reaction 10 is small in 250 DEG C of baking ovens.Using the bag filter that molecular cut off is 1000 to above-mentioned anti-
The solution that should be obtained carries out dialysis three days, to remove as reaction raw materials and intermediate product, collects the solution outside bag filter and carries out
Freeze-drying, obtains powdered carbon dots one.
Weigh 10g polyacrylic acid (PAA) to be dissolved in 10mL deionized waters, 30mL polytetrafluoroethylene (PTFE) is transferred to after ultrasonic dissolution
In the reaction kettle of liner, when reaction 10 is small in 250 DEG C of baking ovens.Using the bag filter that molecular cut off is 1000 to above-mentioned reaction
Obtained solution carries out dialysis 48h, to remove as reaction raw materials and intermediate product, collects the solution outside bag filter and is freezed
It is dry, obtain powdered carbon dots two.
Take carbon dots one to be dissolved in deionized water and obtain solution one, take carbon dots two to be dissolved in deionized water and obtain solution two, control adds
The carbon dots one and the addition of carbon dots two entered causes the charge number of the ion institute band in solution one and the ion institute band in solution two
Charge number is identical, and mixed solution one and solution two obtain carbon dots ink.
Embodiment 4
Weigh 10g diallyl dimethyl ammoniumchlorides (PDDA) to be dissolved in 10mL deionized waters, shifted after ultrasonic dissolution
Into the reaction kettle of 30mL polytetrafluoroethyllining linings, when reaction 5 is small in 180 DEG C of baking ovens.The use of molecular cut off is 3500
Bag filter carries out dialysis 60h to the solution that above-mentioned reaction obtains, and to remove as reaction raw materials and intermediate product, collects outside bag filter
The solution in portion is freeze-dried, and obtains powdered carbon dots one.
Weigh 10g kayexalates (PSS) to be dissolved in 10mL deionized waters, 30mL poly- four is transferred to after ultrasonic dissolution
In the reaction kettle of vinyl fluoride liner, when reaction 5 is small in 180 DEG C of baking ovens.Using the bag filter that molecular cut off is 3500 to upper
State the solution that reaction obtains and carry out dialysis three days, to remove as reaction raw materials and intermediate product, collect the solution outside bag filter
It is freeze-dried, obtains powdered carbon dots two.
Take carbon dots one to be dissolved in deionized water and obtain solution one, take carbon dots two to be dissolved in deionized water and obtain solution two, control adds
The carbon dots one and the addition of carbon dots two entered causes the charge number of the ion institute band in solution one and the ion institute band in solution two
Charge number is identical, and mixed solution one and solution two obtain carbon dots ink, its self assembling process is as shown in Figure 1.The TEM of carbon dots ink
Shape appearance figure is as shown in Fig. 2, it can be seen from the figure that carbon dots even size distribution, a diameter of 15~50 nanometers of carbon dots.
Above-mentioned carbon dots ink is taken, it is in excitation wavelength 310nm, 320nm, 330nm, 340nm, 350nm, 360nm, 370nm
With the fluorescence spectra under 380nm excitation wavelengths, as shown in figure 3, optimal excitation wavelength be 310 nanometers.
Embodiment 5：Stability test
Write respectively using the solution one (C-PAH) in embodiment 1, solution two (C-PSS) and carbon dots ink (SA-CDs)
Data air-dry paper, above-mentioned paper are respectively placed in water (H under ultraviolet light on paper2O), n-hexane, chloroform
(CHCl3) and dimethyl sulfoxide (DMSO) (DMSO) in, observe phenomenon after five minutes, as shown in Figure 4.It can be seen from the figure that with C-PAH
Relatively stablize in organic solvent for the writing data of fluorescent carbon point with C-PSS solution, it is extremely unstable in aqueous, and use this
It is excellent steady no matter the data of carbon dots ink SA-CDs writings prepared by invention show in aqueous solution or organic solvent
Qualitative, the carbon dots ink for showing to prepare based on self assembly not only has the fluorescence property of conventional fluorescent ink but also stability is high,
It can be applied to the fields such as data message encryption and typographical display.
Embodiment 6
The mixture for weighing 10g polyallylamine hydrochlorides (PAH) and polyethyleneimine (PEI) is dissolved in 10mL deionized waters
In, it is transferred to after ultrasonic dissolution in the reaction kettle of 30mL polytetrafluoroethyllining linings, when reaction 10 is small in 250 DEG C of baking ovens.Use
Molecular cut off be 1000 bag filter to the solution that above-mentioned reaction obtains carry out dialysis three days, with remove for reaction raw materials and in
Between product, collect bag filter outside solution be freeze-dried, obtain powdered carbon dots one.
Weigh 10g polyacrylic acid (PAA) to be dissolved in 10mL deionized waters, 30mL polytetrafluoroethylene (PTFE) is transferred to after ultrasonic dissolution
In the reaction kettle of liner, when reaction 10 is small in 250 DEG C of baking ovens.Using the bag filter that molecular cut off is 1000 to above-mentioned reaction
Obtained solution carries out dialysis 48h, to remove as reaction raw materials and intermediate product, collects the solution outside bag filter and is freezed
It is dry, obtain powdered carbon dots two.
Take carbon dots one to be dissolved in deionized water and obtain solution one, take carbon dots two to be dissolved in deionized water and obtain solution two, control adds
The carbon dots one and the addition of carbon dots two entered causes the charge number of the ion institute band in solution one and the ion institute band in solution two
Charge number is identical, and mixed solution one and solution two obtain carbon dots ink.
Embodiment 7
The mixture for weighing 10g polyethyleneimines (PEI) is dissolved in 10mL deionized waters, and 30mL is transferred to after ultrasonic dissolution
In the reaction kettle of polytetrafluoroethyllining lining, when reaction 10 is small in 250 DEG C of baking ovens.Use the bag filter that molecular cut off is 1000
Dialysis three days is carried out to the solution that above-mentioned reaction obtains, to remove as reaction raw materials and intermediate product, is collected outside bag filter
Solution is freeze-dried, and obtains powdered carbon dots one.
The mixture for weighing 10g kayexalates (PSS) and polyacrylic acid (PAA) is dissolved in 10mL deionized waters,
It is transferred to after ultrasonic dissolution in the reaction kettle of 30mL polytetrafluoroethyllining linings, when reaction 10 is small in 250 DEG C of baking ovens.Use retention
The bag filter that molecular weight is 1000 carries out dialysis 48h to the solution that above-mentioned reaction obtains, to remove as reaction raw materials and middle production
Thing, collects the solution outside bag filter and is freeze-dried, obtain powdered carbon dots two.
Take carbon dots one to be dissolved in deionized water and obtain solution one, take carbon dots two to be dissolved in deionized water and obtain solution two, control adds
The carbon dots one and the addition of carbon dots two entered causes the charge number of the ion institute band in solution one and the ion institute band in solution two
Charge number is identical, and mixed solution one and solution two obtain carbon dots ink.
Claims (10)
1. a kind of preparation method of carbon dots ink, it is characterised in that comprise the following steps：
Cation type polymer electrolyte is taken, solvent is added, is transferred in reaction kettle and is reacted to obtain solution one；
Take bag filter to dialyse solution one, collect the solution outside osmotic bag, be dried to obtain carbon dots one；
Anionic polymer electrolyte is taken, solvent is added, is transferred in reaction kettle and is reacted to obtain solution two；
Take bag filter to dialyse solution two, collect the solution outside osmotic bag, be dried to obtain carbon dots two；
Take carbon dots one to add solvent and be configured to solution three, take carbon dots two to add solvent and be configured to solvent four, mixed solution three and molten
Carbon dots ink, ion institute's charge number of the solution three and the ion institute charge number phase of the solution four is prepared in liquid four
Together.
2. the preparation method of carbon dots ink according to claim 1, it is characterised in that the cation type polymer electrolysis
Matter is at least one of polyallylamine hydrochloride, polyethyleneimine, diallyl dimethyl ammoniumchloride.
3. the preparation method of carbon dots ink according to claim 1, it is characterised in that the anionic polymer electrolysis
Matter is at least one of kayexalate, polyacrylic acid.
4. according to the preparation method of claim 1-3 any one of them carbon dots inks, it is characterised in that the solvent for go from
Sub- water.
5. according to the preparation method of claim 1-3 any one of them carbon dots inks, it is characterised in that the bag filter is cut
Stay molecular weight≤3500.
6. according to the preparation method of claim 1-3 any one of them carbon dots inks, it is characterised in that react in a kettle
Temperature be 150~250 DEG C.
7. according to the preparation method of claim 1-3 any one of them carbon dots inks, it is characterised in that react in a kettle
Time is >=5h.
8. according to the preparation method of claim 1-3 any one of them carbon dots inks, it is characterised in that the time of dialysis for >=
48h。
9. a kind of carbon dots ink, it is characterised in that by the preparation method system of claim 1-8 any one of them carbon dots inks
.
10. application of the carbon dots ink in data message encryption and typographical display field described in claim 9.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711136053.6A CN107974131B (en) | 2017-11-16 | 2017-11-16 | Carbon dot ink and preparation method and application thereof |
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| CN201711136053.6A CN107974131B (en) | 2017-11-16 | 2017-11-16 | Carbon dot ink and preparation method and application thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109535843A (en) * | 2018-11-06 | 2019-03-29 | 深圳市华星光电半导体显示技术有限公司 | A kind of ink-jet printing ink and preparation method thereof |
| CN109540857A (en) * | 2018-11-12 | 2019-03-29 | 安庆师范大学 | A kind of preparation method of the fluorescent test paper of quick detection barium ions |
| CN110294963A (en) * | 2019-08-12 | 2019-10-01 | 厦门欧化实业有限公司 | Aqueous UV exempts from processing table printing ink and its processing method, process equipment |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1826393A (en) * | 2003-06-17 | 2006-08-30 | 伊利诺斯大学理事会 | Polyelectrolyte ink |
| CN107099288A (en) * | 2017-04-01 | 2017-08-29 | 深圳市华星光电技术有限公司 | The preparation method and carbon point laminated film of carbon point laminated film |
-
2017
- 2017-11-16 CN CN201711136053.6A patent/CN107974131B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1826393A (en) * | 2003-06-17 | 2006-08-30 | 伊利诺斯大学理事会 | Polyelectrolyte ink |
| CN107099288A (en) * | 2017-04-01 | 2017-08-29 | 深圳市华星光电技术有限公司 | The preparation method and carbon point laminated film of carbon point laminated film |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109535843A (en) * | 2018-11-06 | 2019-03-29 | 深圳市华星光电半导体显示技术有限公司 | A kind of ink-jet printing ink and preparation method thereof |
| CN109540857A (en) * | 2018-11-12 | 2019-03-29 | 安庆师范大学 | A kind of preparation method of the fluorescent test paper of quick detection barium ions |
| CN110294963A (en) * | 2019-08-12 | 2019-10-01 | 厦门欧化实业有限公司 | Aqueous UV exempts from processing table printing ink and its processing method, process equipment |
| CN110294963B (en) * | 2019-08-12 | 2022-02-08 | 厦门欧化实业有限公司 | Water-based UV treatment-free surface printing ink and processing method and processing equipment thereof |
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| CN107974131B (en) | 2021-01-12 |
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