Preparation method of composite fluorescent micelle with dual wavelength detection and full spectrum modulation and its application in water-based anti-counterfeiting ink
A composite fluorescence, full spectrum technology, applied in the field of water-based anti-counterfeiting ink materials, can solve the problems of easy leakage of dye molecules, single detection wavelength, and large pollution.
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[0071] According to the fourth aspect of the present invention, the present invention provides a method for preparing a composite fluorescent micelle capable of dual-wavelength detection and full-spectrum adjustment, preferably including preparing the above-mentioned blue fluorescent micelles and red fluorescent micelles As well as the micelles that emit green fluorescence, the preparation method comprises the following steps:
[0072] Step 1, respectively preparing blue fluorescent micelles, red fluorescent micelles, and green fluorescent micelles;
[0073] Step 2, according to the three kinds of micelles prepared in step 1, it can be adjusted into a full-spectrum color material according to a certain mass ratio;
[0074] Preferably, in step 1,
[0075] Preparation of blue fluorescent micelles Including: adding L1 and block polymers to water according to the set ratio and sequence, optionally adding inorganic salts, vortexing evenly, and then obtaining blue fluorescent mic...
Embodiment 1
[0113] Preparation and characterization of embodiment 1 L1 (containing tetraphenylethylene compound)
[0114] With R=O(CH 2 CH 2 O) n , n=4 as an example, the preparation steps of L1 and the characterization of the product, the NMR spectrum of the characterization is shown in figure 1 , 1 HNMR, the solvent is heavy water.
[0115] The preparation reaction equation is as follows:
[0116]
[0117] Reaction preparation steps:
[0118] 1→3: compound 1 (3.3g), compound 2 (6.9g), K 2 CO 3 (4.97g) was refluxed in acetonitrile (250mL) solution, and N 2 Protected and reacted overnight. The product was subjected to column separation, using petroleum ether and ethyl acetate (volume ratio 3:1) as a developing solvent to obtain compound 3.
[0119] 3→5: Compound 3 (3.5 g), TsCl (1 g), triethylamine (0.67 g) were dissolved in dichloromethane (100 mL), and stirred overnight at room temperature. After the solvent was evaporated to dryness, compound 4 (1.8 g) and K were added 2...
Embodiment 2
[0121] Preparation and Characterization of Example 2 Blue Fluorescent Micelles
[0122] Preparation of fluorescent micellar systems that fluoresce blue. The specific preparation method is as follows, and the block polymer PMVP-b-PEO is taken as an example for illustration.
[0123] (1) Blu-ray micelles I: L1 (0.1019g) was first mixed with block polymer PMVP-b-PEO (0.1226g), then zinc salt (0.0297g zinc nitrate), water (100mL) was added, and mixed evenly; Get the product.
[0124] Fluorescence spectrum, TEM electron microscope, and dynamic light scattering test results of the product are shown in figure 2 , image 3 , Figure 4 .
[0125] (2) Blu-ray micelles II: L1 (0.1019g) and block polymer PMVP-b-PEO (0.2452g) were evenly mixed. The fluorescence spectrum and TEM electron microscope characterization of the product blue micelle II are shown in figure 2' , image 3 .
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