Preparation method of mono-ammonium glycyrrhizinate
A technology of glycyrrhizic acid monoammonium salt and glycyrrhizic acid is applied in the preparation of sugar derivatives, chemical instruments and methods, steroid compounds, etc., and can solve the problems of low industrialization degree of the preparation process and insufficient purity of the finished product, and achieves excellent color and luster. The effect of good quality and high product purity
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Embodiment 1
[0024] 1) Test steps:
[0025] (1) Extract glycyrrhizic acid with 3 times its volume, 2 times its volume, and 1 times its volume of acidic ethanol with a concentration of 90% and a pH of 4.5 at 60°C-70°C, the extraction time is 2 hours, and filter separately after extraction , to obtain three parts of extracts, and mix the three parts of extracts evenly;
[0026] (2) Concentrate the uniformly mixed extract above at 80°C until the concentration of acidic ethanol is 82%, and the concentration is controlled by calculating the volume of water to be concentrated, adding ammonia water to adjust the pH to 5.0, and centrifuging statically to obtain licorice Acid monoammonium salt crude product;
[0027] (3) Add 75% acidic ethanol substance and activated carbon to the crude product of glycyrrhizinate monoammonium salt obtained above, stir, heat and reflux at 60°C for decolorization, settle and filter to obtain a wet product of glycyrrhizinate monoammonium salt;
[0028] (4) Dissolve ...
Embodiment 2
[0035] 1) Test steps:
[0036] (1) Extract glycyrrhizic acid with 3 times volume, 2 times volume, and 1 times volume of acidic ethanol with a concentration of 90%-95% and a pH of 5.0 at 70°C for 2 hours, and filter separately after extraction , to obtain three parts of extracts, and mix the three parts of extracts evenly;
[0037] (2) Concentrate the uniformly mixed extract at 80°C in vacuum until the concentration of acidic alcohols is 86%, add ammonia water to adjust the pH to 5.5, and centrifuge statically to obtain the crude product of monoammonium glycyrrhizinate;
[0038] (3) Add 80% acidic ethanol substance and activated carbon to the crude product of monoammonium glycyrrhizinate obtained above, stir, heat and reflux at 70°C for decolorization, settle and filter to obtain a wet product of monoammonium glycyrrhizinate;
[0039] (4) Dissolve the wet product of monoammonium glycyrrhizinate obtained above into purified water of 3 times its volume, mix the purified water wi...
Embodiment 3
[0046] 1) Test steps:
[0047] (1) Extract glycyrrhizic acid with 3 times volume, 2 times volume, and 1 times volume of acidic ethanol with a concentration of 90%-95% and a pH of 4.8 at 65°C for 2 hours, and filter separately after extraction , to obtain three parts of extracts, and mix the three parts of extracts evenly;
[0048] (2) Concentrate the homogeneously mixed extract above at 80°C until the concentration of acidic alcohols is 84%, and the concentration is controlled by calculating the volume of water to be concentrated, adding ammonia water to adjust the pH to 5.3, and centrifuging statically Obtain the crude product of monoammonium glycyrrhizinate;
[0049] (3) Add 78% acidic ethanol substance and activated carbon to the crude product of glycyrrhizinate monoammonium salt obtained above, stir, heat and reflux at 65°C for decolorization, settle and filter to obtain a wet product of glycyrrhizinate monoammonium salt;
[0050] (4) Dissolve the wet product of monoammo...
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