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Tetraphenolic hydroxyfluorene compound and preparation method thereof
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A technology of tetraphenol hydroxyfluorene and compound, which is applied in the field of organic synthetic materials and can solve the problems of low crosslinking density of polymers
Inactive Publication Date: 2014-08-20
HARBIN ENG UNIV
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At present, the raw materials used in the synthesis of fluorenyl resins are mainly bisphenol compounds, that is, 9,9-bis-(4-hydroxyphenyl) fluorene and its derivatives, and fluorenyl epoxy resins synthesized with bisphenol monomers , polycarbonate, etc. can only have 2 functional groups, and the crosslinking density of the polymer is low
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Embodiment 1
[0018] Add 2.12g (0.01mol) of 2,7-dihydroxy-9-fluorenone, 11.3g (0.12mol) of phenol, 0.2mL of 3-mercaptopropionic acid, and 1mL of methanesulfonic acid into a three-port vessel with a stirrer and a thermometer In the flask, start stirring, the reaction temperature is 55°C, and the reaction time is 3 hours. The reactant is washed with water and filtered to obtain a white crude product, which is then recrystallized, filtered, and vacuum-dried to finally obtain white 2,7-dihydroxy-9. 3.13 g of 9-bis-(4-hydroxyphenyl)fluorene, melting point 325-326°C, yield 81.9%.
[0019] Proton NMR spectrum test results (DMSO-d 6 , ppm): 9.31 (2H, fluorene ring-OH) and 9.30 (2H, benzene ring-OH), 6.63~7.49 (14H, Ar-H); infrared spectrum test results (KBr, cm -1 ): 3370 (-OH stretching vibration peak), 1609, 1508 and 1451 (skeleton vibration of benzene ring), 1241 and 1073 (C-O asymmetric and symmetric stretching vibration), 861 (1,2,4-trisubstituted benzene ring), 791 (para-disubstituted benze...
Embodiment 2
[0021] Except that concentrated sulfuric acid was used as the catalyst, other conditions were the same as in Example 1, and finally 3.05 g of white 2,7-dihydroxy-9,9-bis-(4-hydroxyphenyl)fluorene was obtained with a yield of 79.8%.
Embodiment 3
[0023] Except that the catalyst is changed to p-toluenesulfonic acid, the dosage is 1.5g, and the reaction temperature is 60°C, other conditions are the same as in Example 1, and finally white 2,7-dihydroxy-9,9-bis-(4-hydroxyphenyl ) fluorene 2.94g, yield 78.0%.
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Abstract
The invention provides a preparation method of a tetraphenolic hydroxyfluorene compound. The preparation method comprises the following steps: adding a phenol, 2,7-dihydroxyfluorenone, an acid catalyst and mercapto carboxylic acid to a container provided with a stirrer, a condenser tube and a thermometer, wherein the molar ratio of the phenol to the 2,7-dihydroxyfluorenone is 8-16:1, the mass ratio of the acid catalyst to the 2,7-dihydroxyfluorenone is 0.2-1:1, and the mass ratio of the mercapto carboxylic acid to the 2,7-dihydroxyfluorenone is 0.05-0.30:1; reacting for 1-8h at 40-80DEG C; and washing with water, recrystallizing, filtering, and carrying out vacuum drying to obtain the tetraphenolic hydroxyfluorene compound. The main chain and the side chain of the fluorine of the invention respectively have two phenolic hydroxy groups, and a tetra-functional resin can be synthesized with the fluorine as a raw material, so the polymer crosslinking density is improved, and performances of the polymer are greatly improved. The compound of the invention can be used for preparing high-performance matrix resins, epoxy resins, benzoxazine resins, polycarbonate, polyester resins and the like.
Description
technical field [0001] The invention relates to an organic synthetic material, and the invention relates to a preparation method of the organic synthetic material. Specifically relates to a fluorenyl compound containing a tetraphenolic hydroxyl structure and a preparation method thereof. Background technique [0002] Fluorene is a white flaky crystal, affected by two benzene rings, the 9-position of fluorene is an active methylene group, and the 2 hydrogens have certain acidity, and a series of reactions can occur at the 9-position. The mass fraction of fluorene in coal tar is 1%-2%, and it is the main component of coal tar. In recent years, the deep processing of fluorene as raw material to produce high value-added chemical products is a relatively popular research topic, for example: the production of 9-fluorenone, 9-fluorenylmethanol, bisphenol fluorene and 2,7 -Downstream products such as dihydroxyfluorenone, which are used as raw materials to further apply to the synt...
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