A kind of green synthesis technology of 2,4-dihydroxybenzophenone
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A technology of dihydroxybenzophenone and synthesis process, which is applied in the direction of condensation preparation of carbonyl compounds, physical/chemical process catalysts, organic chemistry, etc., and can solve the problems of HCl acid mist, waste water and exhaust gas discharge, equipment corrosion, etc.
Active Publication Date: 2021-06-11
优普生物科技湖北有限公司
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In order to eliminate its influence, water and AlCl are often used 3 Hydrolysis reaction occurs, but this will generate HCl acid mist, waste water and exhaust gas discharge, equipment corrosion and other problems
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Embodiment 1
[0037] Weigh 1.76g resorcinol, 2.26g benzoic anhydride, 0.16gBiCl 3 . Dissolve resorcinol in ethanol at room temperature to form 60°C saturated solution a, and dissolve benzoic anhydride in ethanol to form 60°C saturated solution b. BiCl 3 Put the saturated solution a in the reactor, stir and add the saturated solution b dropwise to it, and fully react at 73°C for 4 hours. After the reaction, cool to 5°C, filter, recrystallize and refine the filter residue with an organic solvent of ethanol:water=4:1 (volume ratio, the same below), weigh 3.23g after drying, and detect 2,4- The content of dihydroxybenzophenone is 99.45%, and the yield is 94.42%.
Embodiment 2
[0039] Weigh 2.03g resorcinol, 2.26g benzoic anhydride, 0.17gBiCl 3 . Dissolve resorcinol in ethanol at room temperature to form 60°C saturated solution a, and dissolve benzoic anhydride in ethanol to form 60°C saturated solution b. BiCl 3 and saturated solution a are placed in a reactor, stirred, and saturated solution b is added dropwise thereinto, and fully reacted at 73° C. for 4 hours. After the reaction, cool to 5°C, filter, recrystallize and refine the filter residue with an organic solvent of ethanol:water=4:1, then dry it and weigh 3.75g, and detect 2,4-dihydroxybenzophenone by HPLC The content of ketone is 99.38%, and the yield is 94.63%.
Embodiment 3
[0041] Weigh 2.20g resorcinol, 2.260g benzoic anhydride, 0.22gBiCl 3 . Dissolve resorcinol in ethanol at 60°C to form a saturated solution a, and dissolve benzoic anhydride in ethanol to form a 60°C saturated solution b. BiCl 3 Put the saturated solution a in the reactor, stir and add the saturated solution b dropwise to it, and fully react at 73°C for 4 hours. After the reaction, cool to 5°C, filter, recrystallize and refine the filter residue with an organic solvent of ethanol:water=4:1, weigh 4.03g after drying, and detect 2,4-dihydroxybenzophenone by HPLC The content of ketone is 99.20%, and the yield is 94.22%.
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Abstract
The invention belongs to the field of fine chemical industry and discloses a new process for synthesizing 2,4-dihydroxybenzophenone ultraviolet absorber. The steps are as follows: drop into the ethanol saturated solution of resorcinol and a certain amount of catalyst BiCl in the reaction vessel 3 or doped with 5% (w / w) CeO 2 Composite HZSM‑5 zeolite catalyst, add the saturated ethanol solution of benzoic anhydride drop by drop under good stirring, reflux at 60~80°C for a certain period of time, stop heating, and precipitate solid matter. Follow-up treatment is carried out according to the selected catalyst, the catalyst and the crude product are separated, and the crude product is recrystallized with a mixture of ethanol and water to obtain the finished product 2,4-dihydroxybenzophenone. The invention uses low-toxicity and low-hazard raw materials and reagents, and the novel catalyst adopted has the characteristics of easy separation and recovery, simple process in the whole reaction process and little environmental pollution, and the synthesized 2,4-dihydroxybenzophenone The purity can reach more than 99%, and the yield can reach more than 94%. It is suitable as a light stabilizer for polyvinyl chloride, polystyrene, epoxy resin, cellulose resin, unsaturated resin, paint, and synthetic rubber.
Description
technical field [0001] The invention belongs to the field of fine organic chemical industry, and specifically relates to a new process for synthesizing 2,4-dihydroxybenzophenone ultraviolet absorber. Background technique [0002] Ultraviolet absorbers can absorb the ultraviolet rays in sunlight and fluorescent light sources, and solve the problem of product surface fading. The research and development of new electronic chemicals such as ultraviolet absorbers and photoresists has become a hot spot in the fine chemical industry at home and abroad recently. 2,4-dihydroxybenzophenone is a high-efficiency ultraviolet absorber, also known as UV-O, which belongs to the series of benzophenone ultraviolet absorbers. Due to its good comprehensive performance, low price and wide application range, It occupies an important position in ultraviolet absorbers and is widely used in polymer materials, coatings (automobile spray paint, building finish), printing ink, post-treatment of dyed / p...
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