Preparation method of efficient blue-light polyfluorene spherocrystal material
A technology of spherulite and blue light, which is applied in the field of preparation of high-efficiency blue light polyfluorene spherulite materials, can solve problems affecting device luminescence stability and device service life, and achieve good thermal stability
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[0032] see Figure 1-3 , the present invention provides a technical solution: a method for preparing a high-efficiency blue-light polyfluorene spherulite material. The specific preparation steps of the high-efficiency blue-light polyfluorene spherulite material are as follows:
[0033] S1: Preparation of polymerized monomers:
[0034] a: Preparation of lactone from 2,7-dibromo-9-fluorenone by Bayer-Villiger rearrangement;
[0035] b: Lactone is prepared by Grignard reaction to 2,7-dibromodiol;
[0036] c: Alkyl substitution reaction of the 4th alcohol group of 2,7-dibromodiol;
[0037] d: The product of the previous step is produced by the Friedel-Crafts reaction as the main polymer monomer;
[0038] S2: Preparation of polymer: take equal amounts of bipyridine and nickel catalyst Ni(COD) 2 to fill N 2 In a two-necked flask, activate it in a DMF solution at 75°C for 20min, then add the polymerized monomer solution dissolved in toluene, reflux at 85°C for 3 days, then end-c...
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[0049] The specific preparation steps of the preparation method of the high-efficiency blue light polyfluorene spherulite material are as follows:
[0050] S1: Preparation of polymerized monomers:
[0051] a: Prepare lactone from 2,7-dibromo-9-fluorenone by Bayer-Villiger rearrangement reaction, take 2.8g (8.28mmol) of 2,7-dibromofluorenone and dissolve it in 30ml of dry dichloromethane In, then add 25ml trifluoroacetic acid. Under ice bath conditions, add sodium percarbonate Na every 15min 2 CO 4 1g, 5 times in total. Then return to room temperature and stir for 72h, after the reaction is complete, use sodium bicarbonate NaHCO 4 The remaining trifluoroacetic acid was removed, extracted with dichloromethane and then purified with petroleum ether:dichloromethane (5:1) silica gel column to obtain a light yellow powdery solid (yield 85%);
[0052] b: 2,7-dibromodiol was prepared from lactone by Grignard reaction. First, take 12ml of bromobenzene and magnesium chips (1.76g, 72...
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