Novel process for preparing propylgallate directly from gallnuts
A technology for propyl gallate and gallnut, which is applied in the field of directly preparing propyl gallate from natural product gallnut, can solve the problems of long production method, high waste water treatment cost, serious environmental pollution, etc., and achieves avoiding high-concentration sewage discharge, Less impurities, good safety effect
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Embodiment 1
[0020] The raw material Galla chinensis is crushed and passed through a 40-mesh sieve. Take 100g of quince powder and 1000ml of n-propanol. Stir and extract at 50°C for 4 hours. minutes, followed by vacuum filtration. Add 25 ml of sulfuric acid with a catalyst concentration of 80% to the filtrate, react at 80°C for 5 hours, cool to 20°C and filter, evaporate and concentrate the filtrate under reduced pressure, recover the evaporated solvent n-propanol; dissolve the concentrated material in 500mL hot water at 80°C , stirred, cooled to 15°C, and centrifuged to filter the crystals to obtain 56.8g of wet crystals of gallic acid propanol. The crude product was heated and dissolved in 750ml of water, decolorized with 2g of activated carbon for 30 minutes, vacuum filtered, and the filtrate was cooled to 10°C to crystallize for 5 hours. Centrifuge and filter, wash the material until the pH is 6.0-7.0, take the filter cake, and vacuum-dry (60° C.) to obtain 32.6 g of propyl gallate fin...
Embodiment 2
[0022] Raw material gallic gall, powdered, passed through a 40 mesh sieve, 100g of gall powder and 1000ml of n-propanol were taken, stirred and extracted at 50°C for 4 hours, 5g of activated carbon and 10g of refined diatomite adsorbent were added to the feed liquid for decolorization for 30 minutes, followed by vacuum filtration. Add 25 ml of catalytic sulfuric acid to the filtrate, react at 80°C for 5 hours, cool to 20°C and filter, evaporate and concentrate the filtrate under reduced pressure, and recover the evaporated solvent n-propanol; the concentrated material is dissolved in 500mL hot water at 80°C, stirred, and cooled to At 15°C, crystallization was centrifugally filtered to obtain 61.2g wet crystals of gallic acid propanol. The crude product was heated and dissolved in 750ml of water, decolorized with 2g of activated carbon for 30 minutes, vacuum filtered, and the filtrate was cooled to 10°C to crystallize for 5 hours, centrifugally filtered, and the material was was...
Embodiment 3
[0024] The raw material Galla chinensis is crushed and passed through a 40-mesh sieve. Take 100g of quince powder and 600ml of n-propanol. Stir and extract at 50°C for 4 hours. minutes, followed by vacuum filtration. Add catalyst and 25 ml of sulfuric acid to the filtrate, react at 80°C for 5 hours, cool to 20°C and filter, evaporate and concentrate the filtrate under reduced pressure, recover the evaporated solvent n-propanol; dissolve the concentrated material in 500mL hot water at 80°C, stir, and cool down To 15°C, crystallize and filter by centrifugation to obtain 51.6g wet crystals of gallic acid propanol, heat and dissolve the crude product with 450ml of water, decolorize with 2g of activated carbon for 30 minutes, vacuum filter, cool the filtrate to 10°C to crystallize for 5 hours, centrifugally filter and wash The material was taken until the pH was 6.0-7.0, and the filter cake was taken and vacuum-dried (60° C.) to obtain 30.4 g of propyl gallate finished product, wit...
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