Composite catalyst for esterification reaction and bisphenol F synthesis and preparation method
A composite catalyst, esterification technology, used in the preparation of organic compounds, chemical instruments and methods, physical/chemical process catalysts, etc.
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Embodiment 1
[0014] Embodiment one: a kind of composite catalyst and preparation method that are used for esterification reaction and bisphenol F synthesis comprise following processing steps:
[0015] Preparation steps of hydrotalcite-supported catalyst CuFeP@HT: Dissolve copper acetate (0.908g) and ferric chloride (0.811g) in 100mL of distilled water. Under the protection of nitrogen, disperse 25g of hydrotalcite in the above solution, stir it magnetically for 12 hours, and pay attention to controlling the rotation speed to ensure its uniform dispersion. Suction filtration, repeated washing with 400mL distilled water several times, and then freeze drying to remove all water. The above product was dissolved in 200 mL of absolute ethanol, and 40 mL of tert-butanol was added as a reducing agent and 0.8 g of binaphthol phosphate ligand. React at room temperature for 3 hours, remove a large amount of solvent by suction filtration, wash with ethanol and water (10:1) three times, and dry in va...
Embodiment 2
[0016] Example 2: Add the prepared hydrotalcite supported catalyst CuFeP@HT (2.0g), phenol (9.0g) and 10% concentrated hydrochloric acid (5.0g) into the reactor, add 100mL solvent, the solvent can be xylene and toluene. Stir at room temperature until evenly dispersed, slowly add 37% formaldehyde aqueous solution (10 mL) dropwise, and heat the oil bath to a suitable temperature. When the reaction temperature is lower, such as 125°C, toluene can also be used as a solvent for the reaction. After stirring at constant temperature for 8 h, the reaction solution was obtained. During the post-treatment, first filter to recover the loaded and solidified catalyst, and then separate the liquid to remove the water layer, and the obtained oil layer is the crude product of the reaction. A large amount of volatile solvent was removed by rotary evaporation, and the remaining phenol was recovered by distillation under reduced pressure to obtain bisphenol F with a small amount of impurities, ...
Embodiment 4
[0017] Example 4: Recycling of catalyst CuFeP@HT: In a 100mL round bottom flask, add 0.1mol glycerin, 0.6mol acetic acid and 40mL toluene, then add 0.3g recovered catalyst CuFeP@HT, and reflux at a reaction temperature of 130°C Water was separated and stirred for 5 hours. According to chromatographic analysis, the conversion rate of glycerol was 100%, the selectivity of diacetin was 54%, and the selectivity of triacetin was 41%.
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