Preparation method of fullerene polyester
A fullerene polyester and fullerene technology, applied in the field of preparation of fullerene polyester, can solve the problems of low degree of polymerization, poor solubility, low polymer molecular weight, etc., and achieve good film-forming performance, clear structure, Effect of low refractive index
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[0023] A preparation method of fullerene polyester, comprising the following steps:
[0024] Step 1) Synthesis of fullerene bifunctional monomers containing flexible spacers of different lengths. The fullerene bifunctional monomers include fullerene diol monomers and fullerene diphenol monomers: the fullerene The diol monomer is synthesized by click reaction of fullerene alkynyl ester and diol azide under the catalyst of copper sulfate pentahydrate and sodium ascorbate. Wherein, the length of the flexible spacer can be regulated by the length of the alkyl chain on the alkyne ester and the diol; the fullerene diphenol monomer is synthesized by esterification of fullerene acetic acid and alcoholic hydroxyl-containing diphenol;
[0025] Step 2) Synthesis of fullerene polyester: use the fullerene diol or diphenol monomer and commonly used diacid chloride in pyridine (or dicarboxylic acid monomer in dicyclohexylcarbodiimide) as a catalyst , conduct condensation polymerization in a...
Embodiment 1
[0038] Embodiment one, with P (C 60 -C 9 -C 8 ) as an example:
[0039] (1) Synthesis and characterization of dimethyl 5-hydroxyisophthalate
[0040] In a 500mL round bottom flask, add 5.03 g of 5-hydroxyisophthalic acid, 50mL of 99.5% methanol, mix well, add a stirring bar, then install a condenser, heat to reflux, add 3mL of concentrated sulfuric acid, and reflux for 6 hours Afterwards, the reaction mixture was cooled to room temperature, and saturated NaHCO 3 Wash with deionized water until the solution is neutral, then filter to obtain a filter cake, dissolve the filter cake with a small amount of methanol and ethyl acetate, and perform column separation (eluent: petroleum ether: ethyl acetate = 1: 1), Dried in a vacuum oven for subsequent use, the final product obtained was 5.22 g of white solid (yield 90%). The above reaction process is as follows:
[0041]
[0042] Instrumental Analysis Data 1 H NMR (400 MHz, DMSO-d 6 ): δ 10.35(s, 1H), 7.92(s, 1H), 7.55(s,...
Embodiment 2
[0070] Embodiment two, with P (C 60 -C 12 -C 8 ) as an example:
[0071] In Example 2, the reactions of (1), (2), (3), and (4) are the same as in Example 1, please refer to Example 1.
[0072] (5)R 1 =12 fullerene acetylenic alcohol (C 60 -C 12 -alkyne) synthesis and characterization
[0073] In a 100 ml round bottom flask, add fullerene acetic acid (0.46 g), dissolve fullerene acetic acid with o-dichlorobenzene and a little DMF, then add DMAP (0.07 g), PTSA (0.11 g), DIPC (0.10 g), 12-hydroxydodecyl propiolate (0.10 g) was stirred at room temperature for 2 h, diluted with carbon disulfide, filtered, and spin-dried, and the crude product was subjected to column separation (eluent: toluene: petroleum ether = 5:2), the collected product was spin-dried, and precipitated with methanol. After standing for one day, the brown product was obtained by filtration and dried in a vacuum oven. The above reaction process is as follows:
[0074]
[0075] C 60 -C 12 -alkyne
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