CN105622679A - Preparation method of edible tannic acid - Google Patents
Preparation method of edible tannic acid Download PDFInfo
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- CN105622679A CN105622679A CN201410598169.1A CN201410598169A CN105622679A CN 105622679 A CN105622679 A CN 105622679A CN 201410598169 A CN201410598169 A CN 201410598169A CN 105622679 A CN105622679 A CN 105622679A
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- tannic acid
- ethyl acetate
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Abstract
The invention relates to a preparation method of edible tannic acid and belongs to the field of a food additive and a preparation method thereof. The preparation method comprises dissolving industrial tannic acid in distilled water of which the amount is 1-3 times that of the industrial tannic acid, adding ethyl acetate into the industrial tannic acid solution, carrying out extraction stirring in a heating water bath, pouring the extraction product into a separating funnel, carrying out standing layering at the room temperature, carrying out atmospheric distillation and then reduced pressure distillation on the ethyl acetate layer to remove the most of ethyl acetate, adding distilled water into the extraction product, wherein the amount of the used distilled water is 1/5 that of the extraction product, carrying out reduced pressure distillation to remove residual ethyl acetate, adding 4-6% of active carbon into the extraction product, carrying out backflow treatment at a temperature of 90-95 DEG C for 15-30min, carrying out hot filtration, washing residues through a small amount of water, carrying out vacuum concentration on the filtrate until the filtrate is dried, carrying out vacuum drying and carrying out crushing to obtain pale yellow amorphous powder which is edible tannic acid. The preparation method produces edible tannic acid with content of 94% or more from industrial tannic acid through ethyl acetate extraction and has a yield of 80.0%. The edible tannic acid has resin or dextrin test, resin substance test and ignition residue quality indexes satisfying the FAO/WHO related standards. The preparation method has simple processes and good operationality and is suitable for industrial production.
Description
Technical field
The preparation method that the present invention relates to a kind of Food-tannic acid, belongs to food additive and preparation method thereof field.
Background technology
Tannic acid can be widely used in food industry as clarifier, when medicated beer and drink manufacturing for removing the turbidity sediment caused because protein exists. Containing resin, protein, starch etc. in industrial tannic acid, in order to reach the requirement of Food-tannic acid, it is necessary to separate purification further, remove the impurity such as little molecular phenolics, improve its content. Conventional isolation and purification method has the sedimentation method, dialysis, solvent method, gel column chromatography etc.
Therefore it provides a kind of technique is simple, workable, it is adaptable to industrialized production and the high isolation and purification method that can be used for Food-tannic acid of product quality have certain necessity.
Summary of the invention
It is desirable to provide a kind of technique is simple, workable, it is adaptable to industrialized production and the high preparation method that can be used for Food-tannic acid of product quality.
The preparation method of described Food-tannic acid, comprises the following steps:
Industrial tannic acid is dissolved in the distilled water of 1-3 times amount, add ethyl acetate in heated water bath, extract stirring, it is poured in separatory funnel, it is layered in left at room temperature, after after ethyl acetate layer elder generation normal pressure, decompression steams major part ethyl acetate, the distilled water of about 1/5 amount of addition, decompression steams the ethyl acetate of remnants again, it is subsequently added the activated carbon of 4%-6%, in the 90-95 DEG C of 15-30min that refluxes, heat filtering, with a small amount of water washing residue, filter vacuum is concentrated into dry, then vacuum drying, obtains light yellow amorphous powder and namely obtain Food-tannic acid after pulverizing.
Preferably, ethyl acetate consumption of the present invention is 5-7 times of tannic acid weight.
It is furthermore preferred that extraction conditions of the present invention is bath temperature is 45-55 DEG C, extraction mixing time is 0.5-2h.
Tannic acid can be dissolved in ethanol, vinyl alcohol, methanol, acetone and other organic solvent, and in these several solvents, ethanol, methanol and acetone can be miscible with water, and acetic acid ethyl ester hydrophilic is poor, except on a small quantity by water saturation, can be layered well with water. Utilize this character, it is possible to be extracted with ethyl acetate tannin aqueous acid, will mostly divide tannic acid to transfer to ethyl acetate layer, and the water-solubility impurity of more amount is stayed water layer, thus playing the purpose purifying tannic acid.
The preparation method of Food-tannic acid of the present invention, industrial tannic acid is through extraction into ethyl acetate, content is up to more than 94%, and yield is up to 80.O%, the quality index such as resin or the test of dextrin class, resinous matter test and ignition residue are up to the relevant standard of FAO/WHO, and technique is simple, workable, it is adaptable to industrialized production.
Detailed description of the invention
Embodiment one:
Industrial tannic acid 100g is dissolved in the distilled water of 200mL, add ethyl acetate heated and stirred 1h in 45-55 DEG C of water-bath of 700mL, it is poured in separatory funnel, it is layered in left at room temperature, after after ethyl acetate layer elder generation normal pressure, decompression steams major part ethyl acetate, the distilled water of about 1/5 amount of addition, decompression steams the ethyl acetate of remnants again, it is subsequently added the activated carbon of 4%-6%, in the 90-95 DEG C of 15-30min that refluxes, heat filtering, with few most water washing residue, filter vacuum is concentrated into dry, vacuum drying again, obtain light yellow amorphous powder after pulverizing and namely obtain Food-tannic acid 81g, after measured, contents on dry basis reaches 95.3%, product yield is 81%. the quality index such as this product is tested through resin or dextrin class, resinous matter test and ignition residue are up to the relevant standard of FAO/WHO.
Embodiment two:
Industrial tannic acid 100g is dissolved in the distilled water of 300mL, add ethyl acetate heated and stirred 40min in 50 DEG C of water-baths of 500mL, it is poured in separatory funnel, it is layered in left at room temperature, after after ethyl acetate layer elder generation normal pressure, decompression steams major part ethyl acetate, the distilled water of about 1/5 amount of addition, decompression steams the ethyl acetate of remnants again, it is subsequently added the activated carbon of 4%-6%, in the 90-95 DEG C of 15-30min that refluxes, heat filtering, with few most water washing residue, filter vacuum is concentrated into dry, vacuum drying again, obtain light yellow amorphous powder after pulverizing and namely obtain Food-tannic acid 82.2g, after measured, contents on dry basis reaches 91.3%, product yield is 82.2%. the quality index such as this product is tested through resin or dextrin class, resinous matter test and ignition residue are up to the relevant standard of FAO/WHO.
Claims (3)
1. the preparation method of Food-tannic acid, comprises the following steps:
Industrial tannic acid is dissolved in the distilled water of 1-3 times amount, add ethyl acetate in heated water bath, extract stirring, it is poured in separatory funnel, it is layered in left at room temperature, after after ethyl acetate layer elder generation normal pressure, decompression steams major part ethyl acetate, the distilled water of about 1/5 amount of addition, decompression steams the ethyl acetate of remnants again, it is subsequently added the activated carbon of 4%-6%, in the 90-95 DEG C of 15-30min that refluxes, heat filtering, with a small amount of water washing residue, filter vacuum is concentrated into dry, then vacuum drying, obtains light yellow amorphous powder and namely obtain Food-tannic acid after pulverizing.
2. the preparation method of Food-tannic acid as claimed in claim 1, it is characterised in that described 5-7 times that ethyl acetate consumption is tannic acid weight.
3. the preparation method of Food-tannic acid as claimed in claim 1 or 2, it is characterised in that described extraction conditions is that bath temperature is 45-55 DEG C, and extraction mixing time is 0.5-2h.
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CN201410598169.1A CN105622679A (en) | 2014-10-31 | 2014-10-31 | Preparation method of edible tannic acid |
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CN201410598169.1A CN105622679A (en) | 2014-10-31 | 2014-10-31 | Preparation method of edible tannic acid |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111454307A (en) * | 2020-05-25 | 2020-07-28 | 贵州省中国科学院天然产物化学重点实验室(贵州医科大学天然产物化学重点实验室) | Preparation method of high-purity tannic acid with different crystal water |
CN111548377A (en) * | 2020-06-10 | 2020-08-18 | 贵阳单宁科技有限公司 | Novel method for purifying tannic acid |
-
2014
- 2014-10-31 CN CN201410598169.1A patent/CN105622679A/en active Pending
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111454307A (en) * | 2020-05-25 | 2020-07-28 | 贵州省中国科学院天然产物化学重点实验室(贵州医科大学天然产物化学重点实验室) | Preparation method of high-purity tannic acid with different crystal water |
CN111548377A (en) * | 2020-06-10 | 2020-08-18 | 贵阳单宁科技有限公司 | Novel method for purifying tannic acid |
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Application publication date: 20160601 |