CN107880201A - A kind of preparation and application of the compound photoswitch nano-particle for being adjustable to stable white light - Google Patents
A kind of preparation and application of the compound photoswitch nano-particle for being adjustable to stable white light Download PDFInfo
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- CN107880201A CN107880201A CN201711369704.6A CN201711369704A CN107880201A CN 107880201 A CN107880201 A CN 107880201A CN 201711369704 A CN201711369704 A CN 201711369704A CN 107880201 A CN107880201 A CN 107880201A
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F212/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring
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Abstract
Prepare and apply the invention discloses a kind of compound photoswitch nano-particle for being adjustable to stable white light.With styrene, double ((the 4 hexichol amido) phenyl) ketones of Isosorbide-5-Nitrae phenyl and the nitroindoline quinoline spiro-pyrans ester of 3,3 dimethyl of methacrylic acid ethyl 6 for raw material, two kinds of nano-particles are prepared for using a step miniemulsion polymerization.The nano-particle for being adjustable to stable white light is obtained by compound two kinds of nano-particles.The composite nanoparticle shows excellent photoswitch performance, and available for data encryption and false proof.Compared to existing photoswitch fluorescent nano particles, the compound photoswitch nano-particle that the present invention obtains is adjustable to stable white light, and input cost is relatively low, the advantages that synthetic route is simple, suitable for amplification synthesis and production application, there is huge application prospect in the technical field such as encryption, false proof, display, luminous, super-resolution imaging, life science.
Description
Technical field
The present invention relates to a kind of preparation and application of photoswitch fluorescent nano material, it particularly relates to be adjustable to stabilization
The compound photoswitch nano-particle of white light, belong to chemical material preparation.
Background technology
In past ten years, in the design and synthesis of various photoswitch fluorescent materials, have photochromic and can
The material of inverse fluorescent switch performance be considered as one kind can be applied to high-density optical storage, false proof, encryption, complex biological system into
The new material of picture.This photoswitch fluorescent material is generally by by the acceptor of a kind of donor fluorescent dye and corresponding level-density parameter
Photochromic compound (such as oxazine compound, spiro-pyrans class compound and azobenzene compound) is connected by covalent bond
Connect, the mode such as physical absorption is attached in nano-particle, excite the lower fluorescence property to particle to carry out not sharing the same light so as to realize
Reversible regulation and control.Compared with the traditional colour solid of photoswitch fluorescent organic molecule two or three colour solids, photoswitch nano-particle has following
Multiple advantages:(1) more preferable water dispersible and biocompatibility;(2) higher fluorescent brightness and photostability;(3) can apply
, can be by noise separation by warbled signal in complex system.These advantages cause photoswitch nano-particle in height
The every field such as density digital storage, encryption and biomedicine have very important application value.
At present, the material with white light emission is being shown, the field such as data encryption, storage shows its unique application valency
Value.But in the nano material based on white light developed at present, the nano material with white light emission based on photoswitch
It is still seldom.Existing two kinds of white-light nanometer material (Chem.Sci., 2016,7,5867-5871 based on diarylethene;
Nat.Commun., in work 2014,5,3799), the former can only obtain the white light of transition state, and what can not be stablized is white
Light.The latter is complicated three primary colors mixed system, more complicated, and still regulates and controls white light and disappear, and can not regulate and control white light
Produce.Diarylethene is simply quenched white fluorescent as sensitising agent in this work, is not the determined set of white fluorescent
Group, more it is worth noting that what is prepared in this work is conjugated polymer, base is synthesized in originally complicated diarylethene
On plinth building-up process is more complicated.It is well known that diarylethene is as a kind of sensitising agent, its synthesize be ultralow temperature (-
80 DEG C) under the conditions of (Nat.Commun., 2014,5,5079) that carries out, and synthesize and grown with syntheti c route, yield is low, in reality
It is very restricted in.Comparatively speaking, condition of ultralow temperature is not needed during spiro-pyrans class compound synthesis, prepared
Journey is simple, and total recovery is much larger than diarylethene, advantageously in practical application.
Therefore, a kind of simple, inexpensive, excellent water solubility is invented, bio-toxicity is low, is adjustable to the compound of stable white light
Photoswitch nano-particle has considerable realistic meaning and application prospect.
In view of this it is special to propose the present invention.
The content of the invention
The technical problem to be solved in the present invention is overcome the deficiencies in the prior art, there is provided a kind of stable white light of being adjustable to
The preparation and application of compound photoswitch nano-particle,
In order to solve the above technical problems, the present invention is using the basic conception of technical scheme:
It is an object of the invention to provide a kind of preparation of compound photoswitch nano-particle for being adjustable to stable white light and answer
With the compound photoswitch nano-particle for being adjustable to stable white light is prepared according to improved prior art (CN104151480B).
Further application study shows that the photoswitch nano-particle has multiple reversible fluorescence in the case where ultraviolet light and green light alternately irradiate
Switch performance, and compound photoswitch nano-particle is adjustable to stable white light.In addition the photoswitch nano-particle can also by with
In data encryption and false proof.
The purpose of the present invention is accomplished in the following manner:
A kind of preparation for the compound photoswitch nano-particle for being adjustable to stable white light, comprises the following steps:
A1:With styrene, divinylbenzene, 1,4- phenyl-bis- ((4- hexichol amido) phenyl) ketone (p-DTPACO), first
Base acrylic acid ethyl -3,3- dimethyl -6- nitroindoline quinoline spiro-pyrans ester, hexadecane, azodiisobutyronitrile, cetyl three
Ammonio methacrylate (CTAC) is raw material, and photoswitch nano-particle a is obtained by mini-emulsion polymerization;
A2:With styrene, divinylbenzene, 1,4- phenyl-bis- ((4- hexichol amido) phenyl) ketone, hexadecane, idol
Nitrogen bis-isobutyronitrile, hexadecyltrimethylammonium chloride are raw material, and nano-particle b is obtained by mini-emulsion polymerization;
A3:Nano-particle a and b be can obtain into a kind of compound photoswitch for being adjustable to stable white light by fixed proportion is compound
Nano-particle.
A kind of preparation for the compound photoswitch nano-particle for being adjustable to stable white light, comprises the following steps:
S1:By styrene, divinylbenzene, aggregation inducing enhancement effect of fluorescence dyestuff 1,4- phenyl-bis- ((4- hexichol
Amido) phenyl) ketone, methacrylic acid ethyl -3,3- dimethyl -6- nitroindoline quinoline spiro-pyrans ester, hexadecane, azo two
Isobutyronitrile is 1 in mass ratio:0.25:0.02:0.05:0.19:0.06 is mixed into solution;
S2:Hexadecyltrimethylammonium chloride reagent is made into the aqueous solution that concentration is 0.005~0.015g/mL;
S3:The solution prepared in S1 and S2 is mixed 10~15 minutes, forms pre-emulsion;
S4:The pre-emulsion formed in S3 is subjected to ultrasonic emulsification in Ultrasonic cell smash, the time is 10 minutes, complete
Into rear formation miniemulsion;
S5:Miniemulsion formed in S4 is placed in 75 DEG C of oil bath environment, reacts 3 hours, obtains photoswitch nanoparticle
Sub- a;
S6:By styrene, divinylbenzene, aggregation inducing enhancement effect of fluorescence dyestuff 1,4- phenyl-bis- ((4- hexichol
Amido) phenyl) ketone, hexadecane, azodiisobutyronitrile in mass ratio be 1:0.25:0.02:0.19:0.06 be mixed into it is molten
Liquid;
S7:Hexadecyltrimethylammonium chloride reagent is made into the aqueous solution that concentration is 0.005~0.015g/mL;
S8:The solution prepared in S6 and S7 is mixed 10~15 minutes, forms pre-emulsion;
S9:The pre-emulsion formed in S8 is subjected to ultrasonic emulsification in Ultrasonic cell smash, the time is 10 minutes, complete
Into rear formation miniemulsion;
S10:Miniemulsion formed in S9 is placed in 75 DEG C of oil bath environment, reacts 3 hours, obtains nano-particle b;
S11:By nano-particle resulting in S5 and S10 according to volume ratio 1:0.8~1:1 compound two kinds of nano-particles are molten
Liquid, you can obtain a kind of compound photoswitch nano-particle for being adjustable to stable white light.
In the present invention, bis- ((the 4- hexichol amido) phenyl) ketones of fluorescent dye Isosorbide-5-Nitrae-phenyl-in S1, its structure is as follows:
In the present invention, polymerizable type photoresponse group methacrylic acid ethyl -3,3- dimethyl -6- nitroindolines in S1
Quinoline spiro-pyrans ester, its structure are as follows:
In the present invention, bis- ((the 4- hexichol amido) phenyl) ketones of dyestuff Isosorbide-5-Nitrae-phenyl-of aggregation inducing enhancement effect of fluorescence
Mass ratio with methacrylic acid ethyl -3,3- dimethyl -6- nitroindoline quinoline spiro-pyrans esters is 1:2~1:4.
In the present invention, the ratio for being adjustable to stable white light of nano-particle a and the compound acquisitions of nano-particle b is 1:0.8~
1:1.
In the present invention, defined according to white light standard D65, this white light is close to the white light of daylight, and its cie color coordinate is
X=0.3090~0.3154, y=0.3260~0.3364.
A kind of application for the compound photoswitch nano-particle for being adjustable to stable white light, the complex light for being adjustable to stable white light are opened
Close nano-particle and be applied to light-operated three colors data encryption.
After adopting the above technical scheme, the present invention has the advantages that compared with prior art.
The present invention successfully prepares a kind of photoswitch fluorescent nano particles and another using a step miniemulsion polymerization
Kind of nano-particle, then by the compound compound photoswitch nano-particle for obtaining being adjustable to stable white light, and the composite nanoparticle
With stable dispersed and less particle diameter (70nm or so).
The present invention regulates and controls the generation of white light using spiro-pyrans as sensitising agent first, and can obtain the white of stabilization
Light, and synthesize simpler with preparation process.
The prepared compound photoswitch nano-particle for being adjustable to stable white light in the present invention, by regulating and controlling ultraviolet light and can
See the irradiation time of light, it is reversible being realized in the presence of ultraviolet light and visible ray from blue green light to the white light of stabilization
Conversion.
The prepared compound photoswitch nano-particle for being adjustable to stable white light in the present invention, can be in ultraviolet light and visible ray
Quick, reversible blue green light is shown under the irradiation of (green glow) to the switching mode of white light, in cell high-resolution imaging, is shown
Show, there is very important application prospect in the field such as data encryption.
The embodiment of the present invention is described in further detail below in conjunction with the accompanying drawings.
Brief description of the drawings
A part of the accompanying drawing as the application, for providing further understanding of the invention, of the invention is schematic
Embodiment and its illustrate to be used to explain the present invention, but do not form inappropriate limitation of the present invention.Obviously, drawings in the following description
Only some embodiments, to those skilled in the art, on the premise of not paying creative work, can be with
Other accompanying drawings are obtained according to these accompanying drawings.In the accompanying drawings:
Fig. 1 is the grain-size graph of the nano-particle prepared.
Fig. 2 be prepare nano-particle photoresponse schematic diagram (a is that the nano-particle a, b obtained in embodiment 1 is embodiment
The nano-particle b) obtained in 1.
Fig. 3 is the nano-particle prepared to ultraviolet light and the photoresponse figure of green glow.
Fig. 4 is the nano-particle prepared to ultraviolet light and the reversible response cycle figure of green glow.
Fig. 5 is spectrogram of the nano-particle prepared under ultraviolet light from blue green light to white light.
Fig. 6 is that (A is blue green light to CIE coordinate diagrams of the nano-particle prepared under ultraviolet light from blue green light to white light
CIE coordinates, B be white light CIE coordinates).
Fig. 7 be prepare nano-particle be used for three color data encryption figures (a is that the nano-particle a, b obtained in embodiment 1 is
The nano-particle b) obtained in embodiment 1.
It should be noted that these accompanying drawings and word description are not intended as the design model limiting the invention in any way
Enclose, but be that those skilled in the art illustrate idea of the invention by reference to specific embodiment.
Embodiment
To make the purpose, technical scheme and advantage of the embodiment of the present invention clearer, below in conjunction with the embodiment of the present invention,
Technical scheme in embodiment is clearly and completely described, following examples are used to illustrate the present invention, but are not limited to
The scope of the present invention.
Embodiment 1
A kind of preparation for the compound photoswitch nano-particle for being adjustable to stable white light, below specific steps:
(1) by styrene 0.40g, divinylbenzene 0.10g, p-DTPACO0.006g, methacrylic acid ethyl -3,3- two
Methyl -6- nitroindoline quinoline spiro-pyrans esters 0.020g, hexadecane 0.075g, azodiisobutyronitrile 0.025g are mixed evenly
It is dispersed in afterwards in the aqueous solution 10mL for the CTAC that concentration is 0.01g/mL, ultrasonic emulsification to the miniemulsion for forming stable and uniform, 75
Photoswitch nano-particle a is obtained after being reacted 3 hours at DEG C.
(2) by styrene 0.40g, divinylbenzene 0.10g, p-DTPACO0.006g, hexadecane 0.075g, azo two
Isobutyronitrile 0.025g is dispersed in after being mixed evenly in the aqueous solution 10mL for the CTAC that concentration is 0.01g/mL, and ultrasonic emulsification is extremely
The miniemulsion of stable and uniform is formed, nano-particle b is obtained after being reacted 3 hours at 75 DEG C.
(3) it is 1 according to volume ratio by a and b:The 0.87 compound two kinds of nano-particles of ratio, you can obtain one kind and be adjustable to
The compound photoswitch nano-particle of stable white light.
Embodiment 2
A kind of preparation for the compound photoswitch nano-particle for being adjustable to stable white light, below specific steps:
(1) by styrene 0.40g, divinylbenzene 0.10g, p-DTPACO0.004g, methacrylic acid ethyl -3,3- two
Methyl -6- nitroindoline quinoline spiro-pyrans esters 0.020g, hexadecane 0.075g, azodiisobutyronitrile 0.025g are mixed evenly
It is dispersed in afterwards in the aqueous solution 10mL for the CTAC that concentration is 0.005g/mL, ultrasonic emulsification to the miniemulsion for forming stable and uniform, 75
A kind of photoswitch nano-particle a is obtained after being reacted 3 hours at DEG C.
(2) by styrene 0.40g, divinylbenzene 0.10g, p-DTPACO0.004g, hexadecane 0.075g, azo two
Isobutyronitrile 0.025g is dispersed in after being mixed evenly in the aqueous solution 10mL for the CTAC that concentration is 0.005g/mL, ultrasonic emulsification
To the miniemulsion for forming stable and uniform, nano-particle b is obtained after being reacted 3 hours at 75 DEG C.
(3) it is 1 according to volume ratio by a and b:The 0.91 compound two kinds of nano-particles of ratio, you can obtain one kind and be adjustable to
The compound photoswitch nano-particle of stable white light.
Embodiment 3
A kind of compound photoswitch nano-particle for being adjustable to stable white light, below specific steps:
(1) by styrene 0.40g, divinylbenzene 0.10g, p-DTPACO0.008g, methacrylic acid ethyl -3,3- two
Methyl -6- nitroindoline quinoline spiro-pyrans esters 0.020g, hexadecane 0.075g, azodiisobutyronitrile 0.025g are mixed evenly
It is dispersed in afterwards in the aqueous solution 10mL for the CTAC that concentration is 0.015g/mL, ultrasonic emulsification to the miniemulsion for forming stable and uniform, 75
A kind of photoswitch nano-particle a is obtained after being reacted 3 hours at DEG C.
(2) by styrene 0.40g, divinylbenzene 0.10g, p-DTPACO0.008g, hexadecane 0.075g, azo two
Isobutyronitrile 0.025g is dispersed in after being mixed evenly in the aqueous solution 10mL for the CTAC that concentration is 0.015g/mL, ultrasonic emulsification
To the miniemulsion for forming stable and uniform, nano-particle b is obtained after being reacted 3 hours at 75 DEG C.
(3) it is 1 according to volume ratio by a and b:The 0.8 compound two kinds of nano-particles of ratio, you can obtain one kind and be adjustable to surely
The compound photoswitch nano-particle of ding white ware light.
Embodiment 4
Photoresponse is tested:
3mL sample a of the solid content for 0.18wt% is diluted into quartz colorimetric utensil specifically, taking, in 365nm uviol lamps
Irradiation under, its fluorescence emission curves is tested at regular intervals, until fluorescence does not continue to decline;Then in 525nm green glows
Irradiation under, test its fluorescence emission curves at regular intervals, then take the fluorescent value at 494nm to map, as a result such as Fig. 3 institutes
Show.From figure 3, it can be seen that the fluorescence intensity at 494nm can also produce with the extension of ultraviolet light or the irradiation time of green glow
Raw regular change, under ultraviolet light, it is only necessary to 2 minutes, its fluorescence intensity at 494nm just drop to it is minimum,
And under the irradiation of green glow, its fluorescence intensity at 494nm can be recovered substantially again after 10 minutes.As a result show, the nanometer
Particle has faster speed of photoresponse.
Embodiment 5
Replace the Reversible Cycle under irradiation with green glow in ultraviolet light to test:
Take and be diluted to 3mL sample a of the solid content for 0.18wt% into quartz colorimetric utensil, in 365nm ultraviolet lights and 525nm
Its fluorescence intensity at 494nm and 671nm can be tested respectively after the multiple alternately irradiation of green glow, as a result as shown in figure 4, Fig. 4
Show that the nano-particle still has good Two Colour Fluorescence invertible switch performance after ten photoswitch loop tests.
In ultraviolet light and visible ray regulation and control white light:
The compound photoswitch for being adjustable to stable white light that solid content is 0.18wt% that is diluted to obtained in Example 1 is received
Grain of rice subsample respectively after 525nm visible lamp and 365nm ultra violet lamp, is tested respectively into quartz colorimetric utensil
Its spectrum, as a result as shown in figure 5, further entered chromatic diagram can be calculated the CIE of this white light for (0.0.3104,
0.3304), as shown in Figure 6 (A is glaucous CIE coordinates, and B is the CIE coordinates of white light), defined according to white light standard (D65)
White light CIE understands that this white light is the white light close to day light standard for (0.3129,0.3293).
Embodiment 6
Data encryption is tested:
Take compound photoswitch nano-particle sample, a and the b that are adjustable to stable white light for being diluted to that solid content is 0.18wt%
It is added in ceramic reaction plate, according to regularly arranged shown by template.The uviol lamp after 525nm visible lamp irradiation 5min
Clapped under irradiation in Fig. 7 A scheme.Then using 365nm ultra violet lamp 2min after, clap in Fig. 7 B scheme, and A and B figures
Between can 365nm uviol lamp and 525nm visible lamp alternating irradiation under reversible transformation.
Described above is only presently preferred embodiments of the present invention, not makees any formal limitation to the present invention, though
So the present invention is disclosed above with preferred embodiment, but is not limited to the present invention, any technology people for being familiar with this patent
Member without departing from the scope of the present invention, when the technology contents using above-mentioned prompting make it is a little change or be modified to
The equivalent embodiment of equivalent variations, as long as being the content without departing from technical solution of the present invention, the technical spirit pair according to the present invention
Any simple modification, equivalent change and modification that above example is made, in the range of still falling within the present invention program.
Claims (8)
1. a kind of preparation for the compound photoswitch nano-particle for being adjustable to stable white light, it is characterised in that comprise the following steps:
A1:With styrene, divinylbenzene, 1,4- phenyl-bis- ((4- hexichol amido) phenyl) ketone, methacrylic acid ethyl-
3,3- dimethyl -6- nitroindoline quinoline spiro-pyrans ester, hexadecane, azodiisobutyronitrile, hexadecyltrimethylammonium chloride are
Raw material, photoswitch nano-particle a is obtained by mini-emulsion polymerization;
A2:With styrene, divinylbenzene, 1,4- phenyl-bis- ((4- hexichol amido) phenyl) ketone, hexadecane, azo two
Isobutyronitrile, hexadecyltrimethylammonium chloride are raw material, and nano-particle b is obtained by mini-emulsion polymerization;
A3:Nano-particle a and b be can obtain into a kind of compound photoswitch nanometer for being adjustable to stable white light by fixed proportion is compound
Particle.
2. a kind of preparation of compound photoswitch nano-particle for being adjustable to stable white light according to claim 1, its feature
It is, comprises the following steps:
S1:By styrene, divinylbenzene, aggregation inducing enhancement effect of fluorescence dyestuff 1,4- phenyl-bis- ((4- hexichol amidos)
Phenyl) ketone, methacrylic acid ethyl -3,3- dimethyl -6- nitroindoline quinoline spiro-pyrans ester, hexadecane, the isobutyl of azo two
Nitrile is 1 in mass ratio:0.25:0.02:0.05:0.19:0.06 is mixed into solution;
S2:Hexadecyltrimethylammonium chloride reagent is made into the aqueous solution that concentration is 0.005~0.015g/mL;
S3:The solution prepared in S1 and S2 is mixed 10~15 minutes, forms pre-emulsion;
S4:The pre-emulsion formed in S3 is subjected to ultrasonic emulsification in Ultrasonic cell smash, the time is 10 minutes, after the completion of
Form miniemulsion;
S5:Miniemulsion formed in S4 is placed in 75 DEG C of oil bath environment, reacts 3 hours, obtains photoswitch nano-particle a;
S6:By styrene, divinylbenzene, aggregation inducing enhancement effect of fluorescence dyestuff 1,4- phenyl-bis- ((4- hexichol amidos)
Phenyl) ketone, hexadecane, azodiisobutyronitrile in mass ratio be 1:0.25:0.02:0.19:0.06 is mixed into solution;
S7:Hexadecyltrimethylammonium chloride reagent is made into the aqueous solution that concentration is 0.005~0.015g/mL;
S8:The solution prepared in S6 and S7 is mixed 10~15 minutes, forms pre-emulsion;
S9:The pre-emulsion formed in S8 is subjected to ultrasonic emulsification in Ultrasonic cell smash, the time is 10 minutes, after the completion of
Form miniemulsion;
S10:Miniemulsion formed in S9 is placed in 75 DEG C of oil bath environment, reacts 3 hours, obtains nano-particle b;
S11:By nano-particle resulting in S5 and S10 according to volume ratio 1:0.8~1:1 compound two kinds of nano-particle solutions,
It can obtain a kind of compound photoswitch nano-particle for being adjustable to stable white light.
3. a kind of preparation of compound photoswitch nano-particle for being adjustable to stable white light according to claim 2, its feature
It is, bis- ((the 4- hexichol amido) phenyl) ketones of the fluorescent dye Isosorbide-5-Nitrae-phenyl-in S1, its structure is as follows:
4. a kind of preparation of compound photoswitch nano-particle for being adjustable to stable white light according to claim 2, its feature
It is, polymerizable type photoresponse group methacrylic acid ethyl -3,3- dimethyl -6- nitroindoline quinoline spiro-pyrans esters in S1,
Its structure is as follows:
5. prepared by a kind of compound photoswitch nano-particle for being adjustable to stable white light according to claim 1, its feature exists
In bis- ((the 4- hexichol amido) phenyl) ketones of dyestuff Isosorbide-5-Nitrae-phenyl-and methacrylic acid second of aggregation inducing enhancement effect of fluorescence
The mass ratio of base -3,3- dimethyl -6- nitroindoline quinoline spiro-pyrans esters is 1:2~1:4.
6. prepared by a kind of compound photoswitch nano-particle for being adjustable to stable white light according to claim 1, its feature exists
In the ratio for being adjustable to stable white light of nano-particle a and the compound acquisitions of nano-particle b is 1:0.8~1:1.
7. prepared by a kind of compound photoswitch nano-particle for being adjustable to stable white light according to claim 1, its feature exists
In, defined according to white light standard D65, this white light is close to the white light of daylight, its cie color coordinate be x=0.3090~
0.3154, y=0.3260~0.3364.
8. a kind of application for the compound photoswitch nano-particle for being adjustable to stable white light, it is characterised in that be adjustable to stable white light
Compound photoswitch nano-particle be applied to light-operated three colors data encryption.
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Cited By (4)
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CN109081784A (en) * | 2018-10-09 | 2018-12-25 | 浙江工业大学 | A kind of triphenylamine derivative and its preparation method and application |
CN109721919A (en) * | 2019-01-10 | 2019-05-07 | 湖南科技大学 | Photoswitch red fluorescence polymer nano-particle is applied to the method for data encryption |
CN109942603A (en) * | 2019-05-06 | 2019-06-28 | 湖南科技大学 | Photoswitch spiro-pyrans-imide compound preparation and its application |
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