CN111454307A - Preparation method of high-purity tannic acid with different crystal water - Google Patents
Preparation method of high-purity tannic acid with different crystal water Download PDFInfo
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- CN111454307A CN111454307A CN202010450075.5A CN202010450075A CN111454307A CN 111454307 A CN111454307 A CN 111454307A CN 202010450075 A CN202010450075 A CN 202010450075A CN 111454307 A CN111454307 A CN 111454307A
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- C07H13/00—Compounds containing saccharide radicals esterified by carbonic acid or derivatives thereof, or by organic acids, e.g. phosphonic acids
- C07H13/02—Compounds containing saccharide radicals esterified by carbonic acid or derivatives thereof, or by organic acids, e.g. phosphonic acids by carboxylic acids
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Abstract
The invention discloses a preparation method of tannic acid with different crystal water in high purity, which comprises the steps of dissolving a tannic acid sample by using water as a solvent to form a tannic acid water solution, wherein the amount of the water is 0.5-10 times of that of the tannic acid sample by mass; drying to obtain the tannic acid solid with the crystal water content of 4-9%, wherein the drying temperature is set to-20-200 ℃, and the vacuum degree is set to-0.05-0.1 Mpa. The invention can obtain high-quality tannic acid solid and tannic acid solid containing different contents of crystal water by strictly controlling the drying temperature and vacuum degree of the tannic acid, and meets the high requirements of food-grade and medical-grade tannic acid on the purity of the tannic acid.
Description
Technical Field
The invention belongs to the field of food and medicine, relates to the research on a drying process of tannic acid, and particularly relates to a preparation method of tannic acid with different crystal water in high purity. The tannic acid solid prepared by the method can ensure that the residue and the quality of the organic solvent reach the national standards of food grade and medicine grade.
Tannic acid, also known as Tannic acid or Tannic acid, having an english name of Tannic acid, is in a form of amorphous powder or flake from light yellow to brown at normal temperature, and the crystal form of Tannic acid is closely related to the color and purification process. The tannin is mainly extracted from plant bark and fruit, such as Chinese gall, Turkey gall, tara fruit pod, pomegranate, sumac leaves, cotinus coggygria, hamamelis trees and the like, and is also a main component in insect galls (galls) generated by insect attack on the trees, and the content of the tannin is 50-70%. In addition, more than 70% of the herbs such as sanguisorba officinalis, rheum officinale, myrobalan, cinnamon, mango, agrimony and the like contain a large amount of tannic acid.
The tannic acid is widely applied to the fields of medicine, wine brewing, beverages, tanning, metallurgy, daily chemical industry and the like, and particularly, the high-purity tannic acid product has larger market demand. At present, the domestic tannin production process research focuses on the purification of tannin, such as activated carbon adsorption, macroporous resin adsorption, membrane separation technology, ion exchange technology, molecular distillation technology, freeze clarification, solvent extraction and other single purification methods and multi-component combined purification methods, but few reports are made on tannin drying methods. Document "use of an air-flow spray drying apparatus in tannic acid production" discloses a spray drying method which can rapidly obtain powdery tannic acid, but the method has the disadvantage that the polyhydroxy chemical group of the heat-sensitive tannic acid is easily oxidized under the high temperature condition of spray drying. Therefore, it is difficult to prepare high-purity tannic acid under conventional conditions, and it is difficult to satisfy market demand of high-purity tannic acid products.
Disclosure of Invention
The technical problems to be solved by the invention are the removal of residual organic solvent in the tannic acid product and the preparation of tannic acid with different crystal water in high purity. In order to solve the technical problem, the invention provides a preparation method of tannic acid with different crystal water in high purity. The tannic acid prepared by the method has stable quality, can effectively remove organic solvent residues in the tannic acid purification process and reaches the national food-grade and medicine-grade standards.
Specifically, the invention relates to a method for preparing high-purity different crystal water tannic acid, which comprises the following steps,
dissolving a tannic acid sample by using water as a solvent to form a tannic acid aqueous solution, wherein the amount of the water is 0.5-10 times of that of the tannic acid sample by mass;
drying to obtain the tannic acid solid with the crystal water content of 4-9%, wherein the drying temperature is set to-20-200 ℃, and the vacuum degree is set to-0.05-0.1 Mpa.
As the preferable preparation method of the tannic acid with different crystal water of high purity, when the dried tannic acid has a mass of less than 100 g and is dried in vacuum, the drying temperature is-20 to 60 ℃ under stirring, the vacuum degree is-0.08 to 0.095Mpa, and the drying time is 15 to 20 hours. When the dried tannic acid has a mass of 100 g or more and vacuum drying is adopted, the drying time is suitably prolonged, usually more than 20 hours.
As the method for preparing the tannic acid with different crystal water of high purity, the drying temperature is set to 100 to 200 ℃ and the vacuum degree is set to-0.05 to-0.1 MPa after the water in the tannic acid aqueous solution is removed and the tannic acid is solid.
As the optimization of the preparation method of the high-purity tannic acid with different crystal water, the tannic acid aqueous solution is dried by adopting a gradient heating way, wherein the gradient heating way is to heat 10 ℃ per hour so as to obtain tannic acid solids with different crystal forms and tannic acid solids with different crystal water contents.
As the optimization of the preparation method of the high-purity tannic acid with different crystal water, when the vacuum degree is controlled to be-0.05 to-0.1 Mpa, the drying temperature is set to be 65 ℃, and the stirring is carried out for 1 hour; cooling to solidify the tannic acid aqueous solution; freeze drying in a freeze drier with freezing parameter set at-40-80 deg.c and vacuum degree not higher than-0.09 MPa; after freeze drying, putting the solid into a vacuum drying oven, setting the vacuum degree to be-0.085 to-0.1 Mpa, setting the temperature to be 70 to 200 ℃, and controlling the drying time to obtain the tannic acid solid containing 4 to 9 percent of crystal water.
Compared with the prior art, the preparation method of the high-purity tannic acid with different crystal waters has the advantages or beneficial effects.
Most of tannin products prepared by the existing tannin production process have organic solvents with boiling points lower than 100 ℃, such as ethyl acetate, methyl acetate, acetone, ethanol, petroleum ether, dichloromethane, chloroform, tetrahydrofuran and the like. In order to optimize the drying condition of the tannic acid product, ensure that the quality of the tannic acid before and after drying is not changed and obtain the high-purity tannic acid with different contents of crystal water, the invention provides a preparation method of the tannic acid with different high-purity crystal water. The tannic acid prepared by the method has stable quality, can effectively remove organic solvent residues in the purification process of the tannic acid, and can reach the national food grade and pharmaceutical grade standards. The method for preparing the tannic acid has the advantages of simple process, convenient operation and low cost.
The invention researches the quality difference of the dried tannic acid under different vacuum degrees and different temperature conditions. Firstly, dissolving a proper amount of tannic acid in a certain amount of water (preferably deionized water) (the mass ratio of the water to the tannic acid is 0.5:1 to 10: 1), reducing the pressure by using a water pump or an oil pump or other instruments capable of vacuumizing (the vacuum degree is controlled to be-0.05 Mpa to-0.1 Mpa), and heating and stirring the tannic acid aqueous solution until the solid tannic acid is obtained. Based on the technical idea of the invention, the preparation requirements of the crystal water tannic acid with different percentages can be realized by adjusting the heating temperature, the drying time and the vacuum degree according to needs.
By adopting the method, the tannic acid with different crystal water contents of 4-10% can be prepared, and the organic solvent residue is lower than the national standard (less than 25 mg/Kg).
Detailed Description
Example 1
Dissolving 100 g of tannic acid sample in 1L water (preferably deionized water) to form tannic acid aqueous solution, heating to 80 ℃, reducing the pressure to-0.09 Mpa by using an oil pump, stirring, removing about 0.5L-0.7L of water, stopping stirring until the tannic acid aqueous solution becomes solid, continuing to dry in vacuum at 80 ℃ (vacuum degree of-0.09 Mpa) for 4 hours to obtain tannic acid solid with 6% of water content, cooling to room temperature, taking out the tannic acid solid, crushing the tannic acid solid by using a crusher, and screening by using sieves with different meshes to obtain tannic acid with different meshes.
Example 2
Dissolving 100 g of tannic acid in 0.5L water to form tannic acid water solution, heating to 40 ℃, reducing the pressure to-0.09 Mpa to-0.095 Mpa by using an oil pump, removing about 0.4L of water, stopping stirring until the tannic acid water solution becomes solid, raising the vacuum temperature to 80 ℃, drying in vacuum (-0.09 Mpa vacuum degree) for 4 hours, raising the vacuum temperature to 110 ℃, keeping the temperature for 2 hours to obtain tannic acid solid with the water content of 5%, cooling to room temperature, taking out the solid, crushing the solid tannic acid by using a crusher, and screening by using sieves with different meshes to obtain tannic acid with different meshes.
Example 3
Dissolving 100 g of tannic acid in 0.3L water to form a tannic acid aqueous solution, heating to 60-65 ℃, reducing the pressure to-0.08 Mpa to-0.095 Mpa by using an oil pump, stirring until the tannic acid aqueous solution becomes solid, raising the vacuum temperature to 80 ℃, drying in vacuum (-0.095 Mpa vacuum degree) for 4 hours, raising the vacuum temperature to 110 ℃, preserving the heat for 2 hours to obtain tannic acid solid with the water content of 5%, cooling to room temperature, taking out the solid, crushing the solid tannic acid by using a crusher, and screening by using sieves with different meshes to obtain the tannic acid with different meshes.
Example 4
Dissolving 100 g of tannic acid in 0.3L water to form a tannic acid aqueous solution, heating to 60-65 ℃, reducing the pressure to-0.08 Mpa to-0.095 Mpa by using an oil pump, stirring until the tannic acid aqueous solution becomes solid, drying for 4 hours in vacuum (-0.09 Mpa vacuum degree) to obtain a tannic acid solid with the water content of 9%, cooling to room temperature, taking out the solid, crushing the solid tannic acid by using a crusher, and screening by using sieves with different meshes to obtain the tannic acid with different meshes.
Example 5
Dissolving 100 g of tannic acid in 0.3L water to form a tannic acid aqueous solution, heating to 60-65 ℃ (adopting a gradient heating mode of heating to 10 ℃ per hour), reducing the pressure to-0.08 MPa-0.095 MPa by using an oil pump, stirring the tannic acid aqueous solution for 0.5 hour, cooling to freeze the tannic acid aqueous solution into a solid, transferring the solid to a freeze dryer for freeze drying at-80 ℃ and-0.092 MPa until the water is completely drained, taking out the solid to obtain a tannic acid solid with the water content of 9%, crushing the solid tannic acid by using a crusher, and screening by using sieves with different meshes to obtain tannic acids with different meshes.
Example 6
Dissolving 100 g of tannic acid in 0.3L water to form a tannic acid aqueous solution, heating to 60-65 ℃, reducing the pressure to-0.08 MPa to-0.095 MPa by using an oil pump, stirring the tannic acid aqueous solution for 0.5 hour, cooling to freeze the tannic acid aqueous solution into a solid block, transferring the solid block to a freeze dryer for freeze drying at-80 ℃ and-0.092 MPa until the water is completely pumped, taking out the solid block to obtain a tannic acid solid with the water content of 9%, putting the solid block into a vacuum drying oven, keeping the vacuum degree to-0.085 MPa to-0.095 MPa, heating to 110 ℃, keeping the vacuum drying for 4 hours, taking out the solid block to obtain the tannic acid solid with the water content of 6%, crushing the solid tannic acid by using a crusher, and screening by using sieves with different meshes to obtain the tannic acid with different meshes.
Example 7
Dissolving 100 g of tannic acid in 0.3L water to form a tannic acid aqueous solution, heating to 60-65 ℃, stirring the tannic acid aqueous solution for 0.1 hour, cooling to freeze the tannic acid aqueous solution into blocks, transferring the tannic acid aqueous solution to a freeze dryer for freeze drying at-80 ℃ and a vacuum degree of-0.092 Mpa until water is completely drained, taking out solids to obtain tannic acid solids with the water content of 9%, putting the tannic acid solids into a vacuum drying oven, keeping the vacuum degree between-0.085 Mpa and-0.095 Mpa, heating to 110 ℃, keeping for 4 hours, taking out the solids to obtain tannic acid solids with the water content of 6%, and crushing the solid tannic acid by using a crusher, wherein the ethyl acetate residue is 1000mg/Kg and is far greater than the national standard.
Example 8
The method takes the residue determination of ethyl acetate as an example to verify the purity of the tannic acid prepared by the method. The standard solutions used were ethyl acetate standard solution # (1 #), and n-butanol standard solution # (2 #).
The chromatographic data for the standard solution are as follows.
Calibration factorf i Calculating according to the formula:
in the formula:
A s -peak area value of n-butanol (internal standard) in standard solution chromatogram;
c s -the concentration of n-butanol (internal standard) in the standard solution in milligrams per milliliter (mg/m L);
A r -peak area value of ethyl acetate standard in standard solution chromatogram;
c r concentration of ethyl acetate standards in milligrams per milliliter (mg/m L) in the standard solution.
The sample amount of the n-butanol standard sample was 0.1014 g, the sample amount of the ethyl acetate standard sample was 0.1033 g, and the sample amount of the tannic acid sample prepared by the method described in example 1 was 1.0024 g; a sample of tannic acid was prepared by the conventional method (example 7, 3 #) and the amount of the sample was 1.0015 g.
N-butanol concentration 0.1014/100 5/100 1000=0.0507 mg/m L,
the ethyl acetate concentration was 0.1033/100 x 0.1/25 x 1000=0.004132 mg/m L,
calibration factorf i =（112.36454/0.0507）/（66.46095/0.004132）=0.1378。
The chromatographic data of the sample solution is as follows.
Residual solvent (ethyl acetate) content of tannic acid sample prepared as described in example 1w 3 Units are milligrams per kilogram (mg/kg), calculated as follows:
in the formula:
Apeak area value of ethyl acetate in a chromatogram of the sample solution;
m i -mass of n-butanol (internal standard) in milligrams (mg) in the sample solution;
f i -a calibration factor;
A i -peak area value of n-butanol (internal standard) in chromatogram of sample solution;
mthe mass of the sample in grams (g).
Calculating the content of ethyl acetate:w 3 and (3) =23.35189 (5) 0.0507) 0.1378/(79.96697) 1.0024) =10.1765 mg/kg ≦ 25 mg/kg. As can be seen, the residue of ethyl acetate in the tannic acid sample prepared by the method described in example 1 is 10.1765 mg/kg, which is lower than the national standard of 25 mg/kg. From the peak area ratios in the above table (example 7), it can be seen that the method without reduced pressure, the residual amount of ethyl acetate in tannic acid was 100 times that under reduced pressure, which is far beyond the national standard.
Claims (5)
1. A method for preparing tannic acid with different crystal water in high purity is characterized by comprising the following steps,
dissolving a tannic acid sample by using water as a solvent to form a tannic acid aqueous solution, wherein the amount of the water is 0.5-10 times of that of the tannic acid sample by mass;
drying to obtain the tannic acid solid with the crystal water content of 4-9%, wherein the drying temperature is set to-20-200 ℃, and the vacuum degree is set to-0.05-0.1 Mpa.
2. The method of preparing tannic acid of different crystal waters in high purity according to claim 1, wherein the drying time is 15 to 20 hours, and the drying temperature is-20 to 60 ℃ under agitation, the degree of vacuum is-0.08 to 0.095Mpa, and the mass of the dried aqueous tannic acid solution is 100 g or less.
3. The method of preparing tannic acid of different crystal waters of high purity according to claim 1, wherein the drying temperature is set to 100 to 200 ℃ and the degree of vacuum is set to-0.05 to-0.1 Mpa after water in the aqueous solution of tannic acid is removed and tannic acid is in a solid form.
4. The method of claim 1, wherein the aqueous solution of tannic acid is dried by gradient heating at 10 ℃ per hour to obtain tannic acid solids of different crystal forms and tannic acid solids of different crystal water contents.
5. The method of preparing tannic acid of different crystal waters of high purity as claimed in claim 1, wherein the drying temperature is set to 65 ℃ and stirring is carried out for 1 hour while controlling the degree of vacuum to-0.05 to-0.1 Mpa; cooling to solidify the tannic acid aqueous solution; freeze drying in a freeze drier with freezing parameter set at-40-80 deg.c and vacuum degree not higher than-0.09 MPa; after freeze drying, putting the mixture into a vacuum drying oven, setting the vacuum degree to be-0.085 to-0.1 Mpa and the temperature to be 70 to 200 ℃, and obtaining the tannic acid solid containing 4 to 9 percent of crystal water.
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| CN102250159A (en) * | 2011-04-28 | 2011-11-23 | 贵阳单宁科技有限公司 | Method for extracting and preparing high-purity tannic acid from plant raw material containing tannin |
| CN103122011A (en) * | 2013-03-20 | 2013-05-29 | 广西壮族自治区林业科学研究院 | Method for preparing high-purity tannic acid by utilizing tara |
| CN105622679A (en) * | 2014-10-31 | 2016-06-01 | 陕西启源科技发展有限责任公司 | Preparation method of edible tannic acid |
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- 2020-05-25 CN CN202010450075.5A patent/CN111454307A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1810820A (en) * | 2006-03-01 | 2006-08-02 | 贵阳吉隆单宁化工有限公司 | Production process of tannic acid for beer |
| CN102127125A (en) * | 2011-01-05 | 2011-07-20 | 中国林业科学研究院林产化学工业研究所 | Multielement combined purification preparation process of refined tannic acid serie and combined preparation of products |
| CN102250159A (en) * | 2011-04-28 | 2011-11-23 | 贵阳单宁科技有限公司 | Method for extracting and preparing high-purity tannic acid from plant raw material containing tannin |
| CN103122011A (en) * | 2013-03-20 | 2013-05-29 | 广西壮族自治区林业科学研究院 | Method for preparing high-purity tannic acid by utilizing tara |
| CN105622679A (en) * | 2014-10-31 | 2016-06-01 | 陕西启源科技发展有限责任公司 | Preparation method of edible tannic acid |
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Application publication date: 20200728 |