Rare earth fluorescent microsphere preparation method
A technology of rare earth fluorescent microspheres, which is applied in the field of preparation of rare earth fluorescent microspheres, can solve the problems of rare earth fluorescent microspheres such as less dyeing amount, high toxicity in the preparation process, and low preparation efficiency, and achieve large dyeing amount, short production time, The effect of high production efficiency
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[0028] In this embodiment, the preparation method of rare earth fluorescent microspheres includes the following steps:
[0029] (1) Synthetic polymer microspheres
[0030] Using the emulsion polymerization method, add a certain ratio of A, B and C monomers into a three-necked flask filled with nitrogen. Wherein, the mass ratio of the monomers A, B, and C is 70-100:0-20:0-10. Add pure water and emulsifier into the three-necked flask, stir and homogenize at room temperature at 200-800 rpm for 10-60 minutes, then raise the temperature in the water bath to 60-80°C, and add an initiator to initiate polymerization. Wherein, the mass ratio of total monomer, pure water, emulsifier and initiator is 1:10-100:0-0.1:0-0.1. The reaction is continued for 12-24 hours at 60-80° C. and a stirring speed of 200-800 rpm, and polymer microspheres are obtained after the reaction is completed. The diameter of polymer microspheres is generally the minimum of 10-30nm and the maximum of 500-1000μm. ...
Embodiment 1
[0040] Example 1: Preparation of 400nm polystyrene rare earth fluorescent microspheres
[0041] (1) Synthetic polymer microspheres
[0042] Add 10 g of purified styrene monomer into a three-necked flask filled with nitrogen, then add 100 mL of pure water and 0.02 g of sodium lauryl sulfate, and stir and homogenize at room temperature at 500 rpm for 20 minutes. Then the temperature of the water bath was raised to 70° C., and 0.1 g of ammonium persulfate was added to initiate polymerization. Continue to react for 18 hours at 70°C and 500 rpm at a stirring speed. After the reaction is over, obtain a polystyrene microsphere emulsion with a diameter of 400nm, wash it with pure water for 3-5 times by centrifugation, and dry it in a vacuum oven to constant weight. , to obtain polystyrene microspheres with a diameter of 400 nm.
[0043] (2) Complex synthesis
[0044] Dissolve 1mmol of europium chloride in 100mL of absolute ethanol and set aside; add 3mmol of benzoyltrifluoroacetone...
Embodiment 2
[0047] Example 2: Preparation of 200nm carboxypolymethyl methacrylate rare earth fluorescent microspheres
[0048] (1) Synthetic polymer microspheres
[0049] Add 9.5g of purified methyl methacrylate and 0.5g of purified methyl methacrylate into a three-necked flask filled with nitrogen, then add 100mL of pure water and 0.2g of polyvinylpyrrolidone, at room temperature 400 rpm Homogenize under stirring for 20 minutes. Then the temperature of the water bath was raised to 70° C., and 0.15 g of potassium persulfate was added to initiate polymerization. Continue to react for 15 hours at 70°C and 400 rpm at a stirring speed. After the reaction is over, obtain a carboxy polymethyl methacrylate microsphere emulsion with a diameter of 200 nm, centrifuge and wash with pure water for 3-5 times, and place in a vacuum oven Dry to constant weight to obtain carboxypolymethyl methacrylate microspheres with a diameter of 200 nm.
[0050] (2) Synthesis of rare earth fluorescent complexes
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