Crystallization method for improving stability of trichlorosucrose
A technology for sucralose and stability, applied in the field of crystallization for improving the stability of sucralose, can solve the problems of low yield, not taking into account the problem of crystallization mother liquor recovery, product waste, etc., and achieves simple equipment, easy operation, improved Yield effect
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Embodiment 1
[0019] Using 50g of sucralose-6-ethyl ester with a content of 98.2% as a raw material, a methanol solution of sucralose was obtained after deacetylation reaction, and the filtrate was concentrated to dryness to obtain 41g of sucralose concentrate, which was added to 95% Add 40g of ethanol, and add the previous batch of mother liquor that is 5% by weight of the sucralose concentrate after concentration, then add 0.005g of sodium acetate, heat to 75°C, stir until completely dissolved, add 1g of activated carbon, stir for 20 minutes, filter, The filtrate was cooled to 0° C., stirred at 0° C. for 2 hours, filtered, and vacuum-dried to obtain 40.8 g of sucralose finished product. The content detected by HPLC was 99.2%. The filtered mother liquor is recovered for the next batch of crystallization.
Embodiment 2
[0021] Using 50 g of sucralose-6-ethyl ester with a content of 98.2% as a raw material, a methanol solution of sucralose was obtained after deacetylation reaction, and the filtrate was concentrated to dryness to obtain 41.5 g of sucralose concentrate, and 95 % ethanol: water = 40g of the solution of 1:0.1, and add the previous batch of mother liquor which is concentrated and accounts for 5% of the weight of the sucralose concentrate, then add 0.01g of sodium acetate, heat to 70°C, stir until completely dissolved, add Activated carbon 1g, stirred for 20 minutes, filtered, the filtrate was cooled to 0°C, stirred at 0°C for 2 hours, filtered, and vacuum-dried to obtain 40.4g of sucralose finished product. The content detected by HPLC was 98.8%. The filtered mother liquor is recovered for the next batch of crystallization.
Embodiment 3
[0023] Using 50 g of sucralose-6-ethyl ester with a content of 98.2% as a raw material, a methanol solution of sucralose was obtained after deacetylation reaction, and the filtrate was concentrated to dryness to obtain 40.9 g of sucralose concentrate, and 95 % ethanol: water = 20g of the solution of 1:0.4, and add the previous batch of mother liquor which is 10% by weight of the sucralose concentrate after concentration, then add 0.02g of sodium acetate, heat to 75°C, stir until completely dissolved, add Activated carbon 1g, stirred for 20 minutes, filtered, the filtrate was cooled to -5°C, stirred at -5°C for 2 hours, filtered, and vacuum-dried to obtain 40.1g of sucralose finished product. The content detected by HPLC was 98.6%. The filtered mother liquor is recovered for the next batch of crystallization.
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