Fluorescent composite, preparation method and application thereof
A composite material and fluorescent technology, which is applied in the direction of luminescent materials, material analysis through optical means, and analytical materials, etc., can solve the problems of high price, inability to realize real-time dynamic monitoring of organisms and cells, complex instruments and operations, etc., and achieve low / Non-toxic, avoid biological autofluorescence, high selective recognition effect
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[0055] In another aspect, the present invention provides a method for preparing the above-mentioned optical composite material, comprising the following steps:
[0056] 1) 4-bromoacenaphthenequinone reacts with compounds a, b, and c at a molar ratio of 1:1-1:7 to prepare compound i, compound ii, and compound iii;
[0057]
[0058] The reaction temperature is 0-200°C, the reaction time is 1-32 hours, and the reaction solvent is selected from ethanol, glacial acetic acid, ethylene glycol monomethyl ether, methanol, dichloromethane, acetone, glycerol, ethyl acetate or mixtures thereof ;
[0059] In a specific embodiment, the reaction temperature in step 1) is preferably 30-180°C, more preferably 50-180°C, most preferably 60-160°C; the reaction time is preferably 1-24h, more preferably 1-20h, most preferably Preferably 1-18h; The preferred ethanol, glacial acetic acid, ethylene glycol monomethyl ether, methyl alcohol, dichloromethane, acetone, glycerol, ethyl acetate or mixtur...
Embodiment 1
[0080] Fluorescent Composite Material A 1 The synthetic route of is as follows:
[0081]
[0082] (1) Compound A 1 Synthesis of -1
[0083] Add 20 mmol of 4-bromoacenaphthenequinone and 80 mmol of diaminomaleonitrile into a round bottom flask containing 10 mL of glacial acetic acid solution. The reaction was heated to reflux at 110°C for 8 hours and then stopped. The solvent was distilled off under reduced pressure, and treated with column chromatography (dichloromethane:petroleum ether, 3:1, v / v) to obtain yellow compound A 1 -1,
[0084] Yield 80%.
[0085] (2) Compound A 1 Synthesis of -2
[0086] 20mmol compound A 1 -1 and 120mmol of N,N-dimethylethylenediamine were added to a round-bottomed flask containing 20mL of ethylene glycol monomethyl ether solution, and the reaction was heated at 125°C under reflux for 6h and then stopped. The mixture was poured into ice water, precipitated out, and suction filtered to obtain a brick red crude product, which was treate...
Embodiment 2
[0095] Embodiment 2: Absorption spectrum detection test of material A1
[0096] Weigh the material A synthesized above 1 Add 0.0002g into a four-way cuvette containing 3mL of high-purity water, measure its absorption spectrum, collect the absorbance value at a wavelength of 200-800nm, and the wavelength corresponding to the maximum absorbance value is its absorption wavelength. The result is as image 3 shown.
[0097] The instruments used in this example are Agilent 8453 UV spectrophotometers.
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