Method for efficient catalytic synthesis of epoxy bisphenol fluorene

Abstract

The invention relates to the technical field of chemical engineering chemistry, in particular to a method for efficient catalytic synthesis of epoxy bisphenol fluorene. The method can effectively shorten the reaction time, simplify the reaction steps, conveniently control the reaction temperature and effectively improve the product yield, and the product is easy to purify and good in chromaticity.The method comprises the following steps: S1, mixing and dissolving; S2, catalytic reaction: adding a catalyst into the reaction solution obtained in the step S1, adjusting the temperature of the reaction solution to 50-100 DEG C, and reacting for 3-6 hours; S3, adding alkali for reaction: adjusting the temperature of the reaction solution to 30-70 DEG C, adding alkali into the reaction solution,adjusting the temperature of the reaction solution to 50-80 DEG C, and continuing to react for 1-3 hours; S4, filtering and separating; S5, water washing treatment; S6, distillation treatment; S7, recrystallization: adding a recrystallization solvent into the white solid product obtained in the step S6, fully dissolving to obtain a recrystallization mixed solution, lowering the temperature of themixed solution to-5 DEG C, and cooling to separate out; S8, performing centrifugal separation; and S9, performing drying treatment.

Description

technical field [0001] The invention relates to the technical field of chemical engineering, in particular to a method for efficiently catalytically synthesizing epoxy bisphenol fluorene. Background technique [0002] Epoxy bisphenol fluorene, namely epoxy bisphenol fluorene, is a white crystal or white powder, which can be used as a solvent, a catalyst for alkylation esterification and polymerization, and is mainly used in the field of medicine and electroplating industry. As an important thermosetting epoxy resin containing polyphenylene ring fluorene structure, bisphenol fluorene has good mechanical properties, good heat resistance, chemical resistance, abrasion resistance, strong adhesion and other characteristics. The introduction of the structure can reduce the crosslinking density of the resin after curing, and the increase in the number of benzene rings can not only increase the rigidity of the molecular chain, increase the glass transition temperature of the resin, ...

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Problems solved by technology

[0003] The existing patent No. CN106519187A discloses a preparation method of epoxy resin, which is to inject epichlorohydrin and bisphenol A into a reaction kettle with a stirrer and a reflux condenser, open the stirrer, and the reaction kettle Heat in a water bath; dissolve sodium hydroxide with distilled water, slowly add it to the reaction kettle, stir continuously, and react for 60 minutes until the liquid is all milky yellow, stop the reaction, and cool naturally to room temperature; add distilled water and benzene to the reaction kettle , fully stirred and placed in a liquid separation device to stand still, heated the separated organic layer with a water bath to remove benzene, and recovered the distilled benzene with a reflux condensing device, and then distilled under reduced pressure to remove water and unreacted epoxy Chloropropane, the remaining light yellow viscous liquid is bisphenol A epoxy resin, for the above method, the chromaticity of the product obtained at last needs to be processed after many times, thereby causing its production cost to increase, and at the same time the Organic waste liquid will increase, which will affect the environment

[0004] In the document "Thermosetting Resin" (Volume 27, No. 3, 2012, 23-26), it is reported that a preparation method of epoxy bisphenol fluorene resin is disclosed, which is to mix bisphenol fluorene and epichlorohydrin evenly. Hexaalkyltrimethylammonium bromide and sodium hydroxide solution carry out step-by-step catalytic reaction, but the process has problems such as high reaction temperature in the later stage during operation, and more high polymers are produced, and it is also mentioned in the literature The yield of epoxy bisphenol fluorene resin is not reported

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