Production process for preparing high-purity synephrine by crystallization method
A production process and crystallization technology, which are applied in the production process field of preparing high-purity synephrine by crystallization, can solve the problems of high energy consumption cost, insufficient purity, complicated process, etc., and achieve a high degree of continuous production and high extraction efficiency. Simple method and high solvent utilization effect
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example 1
[0045] Take 100kg of Citrus aurantium raw material, pulverize and moisten it, percolate and extract with dilute hydrochloric acid with a concentration of 0.02mol / L and a volume of 500L to obtain an extract; after adsorbing the extract with a 732 cation exchange resin with a volume of 100L, use the mass concentration Analyze 5% of dilute ammonia water with a volume of 500L to obtain synephrine analytical solution; concentrate the analytical solution at room temperature under vacuum under reduced pressure to obtain synephrine crude extract, and at the same time recover ammonia; use water as a solvent to refine the crude extract and add Adjust the pH to 1 with dilute hydrochloric acid, and then add 8kg of activated carbon to decolorize and filter to obtain a decolorizing liquid; add 3% sodium hydroxide to pH=7 by mass concentration to the decolorizing liquid, leave to crystallize, filter, wash, and dry to obtain a purity of 98.2 % Synephrine product; the filtrate is then adsorbed b...
example 2
[0047] Take 100kg of Citrus aurantium raw material, crush and moisten it, percolate and extract with dilute hydrochloric acid with a concentration of 0.01mol / L and a volume of 700L to obtain an extract; after adsorbing the extract with a 732 cation exchange resin with a volume of 240L, use the mass concentration Analyze 4% dilute ammonia water with a volume of 700L to obtain synephrine analytical solution; concentrate the analytical solution at room temperature under vacuum under reduced pressure to obtain synephrine crude extract, while recovering ammonia water; refine the crude extract with water as a solvent and add Adjust the pH to 5 with dilute hydrochloric acid, and then add 5kg of activated carbon to decolorize and filter to obtain a decolorizing solution; add 6% by mass sodium hydroxide to the decolorizing solution to pH=9, stand for crystallization, filter, wash, and dry to obtain a purity of 97.9 % Synephrine product; the filtrate is then adsorbed by 732 cation exchang...
example 3
[0049] Take 100kg of Citrus aurantium raw material, pulverize and moisten it, percolate and extract with dilute hydrochloric acid with a concentration of 0.05mol / L and a volume of 600L to obtain an extract; after adsorbing the extract with a 732 cation exchange resin with a volume of 200L, use the mass concentration Dilute ammonia water with a volume of 9% and a volume of 600L was analyzed to obtain synephrine analytical solution; the analytical solution was concentrated under vacuum and reduced pressure at room temperature to obtain crude synephrine extract, while ammonia water was recovered; the crude extract was refined with water as a solvent and added Adjust the pH to 5 with dilute hydrochloric acid, and then add 5kg of activated carbon to decolorize and filter to obtain a decolorizing solution; add 5% by mass sodium hydroxide to the decolorizing solution to pH=9, stand for crystallization, filter, wash, and dry to obtain a purity of 97.7 % Synephrine product; the filtrate ...
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