CN106336446B - A kind of preparation method of potassium glycyrrhizana - Google Patents
A kind of preparation method of potassium glycyrrhizana Download PDFInfo
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- CN106336446B CN106336446B CN201610715716.9A CN201610715716A CN106336446B CN 106336446 B CN106336446 B CN 106336446B CN 201610715716 A CN201610715716 A CN 201610715716A CN 106336446 B CN106336446 B CN 106336446B
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Abstract
The invention discloses a kind of preparation methods of potassium glycyrrhizana, according to the special physico-chemical property of glycyrrhizic acid, using glycyrrhizic acid coarse powder as raw material, by extracting, decolourizing and ammonification, using specific resin converting apparatus, with the principle of ion exchange, produce that color is good, content is high and meets the potassium glycyrrhizana of professional standard, compared with prior art with following obvious advantage：A) new technology, easy to operate, energy conservation and environmental protection, highly practical；B) mode of the direct stir process of resin container is employed, directly operate at normal temperatures, it will be after product be directly contacted with resin among undissolvable solid in high concentration alcoholic solution, it is made gradually to be transformed into the soluble glycyrrhizic acid of alcohol by the conversion effet of resin, this method not only increases inventory, and the flow first dissolved after resin column is avoided, the operation cycle is greatly saved, it is good to improve efficiency character：C) advantage of ion-exchange resin technique is fully applied, equipment and the cost of material is low, treating capacity is big, and product coloration is good, yield and content are high, is suitable for industrialized production, and product color is excellent, crystal is uniform, high-quality.
Description
Technical field
Preparation field more particularly to a kind of preparation method of potassium glycyrrhizana the present invention relates to compound.
Background technology
Potassium glycyrrhizana is all widely used in industries such as medicine, food, cosmetics, and market demand is larger, at present
The preparation method of the potassium glycyrrhizana of document and patent report is few, integrates mainly through potassium solution and ammonium glycyrrhizinate
Made from reactant salt, such as application No. is 00119121.7 it is entitled《The production technology and purposes of tripotassium glycyrrhetate》Patent
In, the production technology of disclosed GLYCYRRHIZIC ACID POTASSIUM is：Thick glycyrrhizic acid is placed in reaction kettle and adds in ethyl alcohol in 1: 3 ratio,
At a temperature of 50 DEG C~60 DEG C, heating reaction 6~8 hours cools down, and vacuum filtration washs filter cake with ethyl alcohol, drains, discards filter
In neutralizing in kettle, it is 7~8 that filtrate is neutralized to PH with ethanolic potassium hydroxide liquid, generates yellow Radix Glycyrrhizae for slag, merging filtrate and cleaning solution
Sour tripotassium precipitation, then be stirred continuously, it is heated 1~2 hour in 50~60 DEG C, cooled and filtered is washed with ethyl alcohol, is drying to obtain into
Product.The method step is more, cumbersome；Production cost is high.Application No. is the entitled of 201010264190.X《A kind of glycyrrhizic acid
The preparation method of sylvite》Patent in, disclosed dipotassium glycyrrhizinate salt production process is：Extracting liquorice acid ammonium salt adds suitable quantity of water one
Determine to dissolve at temperature, obtain ammonium glycyrrhetate salting liquid；The resin column of certain model is crossed, after water is added fully to elute the other impurity of removal,
It uses the solution elution of the potassium ion containing a certain concentration instead, collects eluent, be concentrated under reduced pressure into certain volume, obtain potassium glycyrrhizana concentration
Liquid.Concentrate is taken, adds in appropriate organic solvent, stirs, stands still for crystals, is filtered, it is dry to get potassium glycyrrhizana.Though the method
Resin has so been used to convert new technology, has needed to dissolve mono-ammonium raw material, but in process of production with higher temperature before treatment
Can occur hair often and congeal knot phenomenon, and temperature is excessively high that certain destruction can be caused to resin；In addition, resin column processing and its
The regenerated period is long, leads to the increase of cost indirectly.And application No. is 201510005226.5 it is entitled《A kind of glycyrrhizic acid list
The preparation method of sylvite or di-potassium》Patent in, disclose it is a kind of using produce mono-ammonium glycyrrhizinate generation mother liquor as raw material
The method for preparing potassium glycyrrhizana, although and being converted by resin, glycyrrhizic acid reality in the mother liquor involved by this method
Content is very low, and impurity is more, although the product finally obtained content in ultraviolet detection does not see difference, through HPLC
Detection finds that its glycyrrhizic acid content is relatively low, is far insufficient for the requirement of most clients in the market；In addition, the patent of invention
In used mechanical strength of resin it is relatively low, it is difficult to tolerance stirring operation, and resin column processing and its regenerated week repeatedly for a long time
Phase is long, also results in the increase of cost indirectly.
To sum up, dipotassium glycyrrhizinate salt production process disclosed at present is mostly prepared with direct chemical reaction method, and will to raw material
Ask higher, often using mono-ammonium as starting material, cost is higher, and cannot fully meet industrialization production requirements.
Invention content
Goal of the invention：In order to overcome defect in the prior art, the present invention proposes a kind of simple for process, easy behaviour
Make, suitable for industrialized production, product colour shapeliness, high, the energy-saving and environment-friendly potassium glycyrrhizana of purity preparation method.
Technical solution：In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is：
A kind of preparation method of potassium glycyrrhizana, it is characterised in that include the following steps：
(1) preparation of Radix Glycyrrhizae acid solution：Activated carbon is added in glycyrrhizic acid coarse powder, is 60%-100% with mass concentration
Ethanol solution refluxing extraction, filter up to Radix Glycyrrhizae acid solution；
(2) ammonification and reflux：It is 4.0- that the Radix Glycyrrhizae acid solution that temperature is obtained to step (1) is maintained, which to add in weak aqua ammonia to adjust pH,
6.0, solid is precipitated in stirring；The 95% alcohol reflux extraction of 1-10 times of solid wet product weight is added in into obtained solid, while hot mistake
Filter is to get product among ammonium glycyrrhizunate；
(3) conversion of Radix Glycyrrhizae acid solution：Product among above-mentioned ammonium glycyrrhizunate are put into processed good resin container, are added
Enter enough ethanol solution stirrings until solution is clarified, extraction solution is to get Radix Glycyrrhizae acid solution；
(4) preparation of sylvite：Above-mentioned Radix Glycyrrhizae acid solution is calculated into its glycyrrhizic acid content after testing, in being concentrated in retort
To dilute alcohol, add in the potassium ion solution of the corresponding amount prepared, in potassium ion solution contained potassium ion amount in Radix Glycyrrhizae acid solution
The molar ratio of glycyrrhizic acid amount is 1:1-3:1, after reacting a period of time, no alcohol taste is concentrated into, is spray-dried to get dipotassium glycyrrhizinate
Salt.
More preferably, 1%-10% of the addition of activated carbon for glycyrrhizic acid coarse powder weight in the step (1).
Further, 5%-8% of the addition of activated carbon for glycyrrhizic acid coarse powder weight in the step (1).
More preferably, the mass concentration of ethyl alcohol is 80%-95% in the step (1).
More preferably, weak aqua ammonia adjusts pH to 4.5-5.0 in the step (2).
More preferably, the usage type of resin is cation exchange resin in the step (3).
Further, resin is one or both of 732, D001, LX-5, LS1-010 mixed in the step (3)
It closes.
Further, resin is LX-5 in the step (3).
More preferably, potassium ion solution is potassium hydroxide solution, potassium bicarbonate solution, potassium carbonate in the step (4)
One kind in solution.
Further, potassium ion solution is solution of potassium carbonate in the step (4).
Advantageous effect：The preparation method of a kind of potassium glycyrrhizana provided by the invention, according to the special physico-chemical of glycyrrhizic acid
Matter using glycyrrhizic acid coarse powder as raw material, by extracting, decolourizing and ammonification, using specific resin converting apparatus, is put with ion
The principle changed, produces that color is good, content is high and meets the potassium glycyrrhizana of professional standard, has compared with prior art as follows
Obvious advantage：A) new technology, easy to operate, energy conservation and environmental protection, highly practical；B) side of the direct stir process of resin container is employed
Formula directly operates at normal temperatures, will be after product are directly contacted with resin among undissolvable solid in high concentration alcoholic solution, warp
Crossing the conversion effet of resin makes it gradually be transformed into the soluble glycyrrhizic acid of alcohol, and this method not only increases inventory, and avoids
The flow after resin column is first dissolved, the operation cycle is greatly saved, it is good to improve efficiency character：C) fully apply from
The advantage of sub-exchange resin technology, equipment and the cost of material is low, treating capacity is big, and product coloration is good, yield and content are high, is suitable for
Industrialized production, and product color is excellent, crystal is uniform, it is high-quality.
Specific embodiment
With reference to embodiment, the present invention is described in further detail：
Embodiment 1：
A kind of preparation method of potassium glycyrrhizana, it is characterised in that include the following steps：
(1) preparation of Radix Glycyrrhizae acid solution：1kg activated carbons are added in 100kg glycyrrhizic acid coarse powder, with the quality of 6 times of amounts
A concentration of 60% ethanol solution refluxing extraction 2h at 70 DEG C is filtered up to Radix Glycyrrhizae acid solution；
(2) ammonification and reflux：It is 4.5 that the Radix Glycyrrhizae acid solution that temperature is obtained to step (1) is maintained, which to add in weak aqua ammonia to adjust pH,
Solid is precipitated in stirring；The 95% alcohol reflux 30min extractions of 3 times of solid wet product weight are added in into obtained solid, are filtered while hot,
Up to product among ammonium glycyrrhizunate；
(3) conversion of Radix Glycyrrhizae acid solution：Product among above-mentioned ammonium glycyrrhizunate are put into the D001 cations equipped with 200kg
In the resin container of exchanger resin, enough ethanol solution stirrings are added in until solution is clarified, extraction solution is molten to get glycyrrhizic acid
Liquid；
(4) preparation of sylvite：Above-mentioned Radix Glycyrrhizae acid solution is calculated into its glycyrrhizic acid content after testing, in being concentrated in retort
To dilute alcohol, add in the potassium ion solution of the corresponding amount prepared, in potassium ion solution contained potassium ion amount in Radix Glycyrrhizae acid solution
The molar ratio of glycyrrhizic acid amount is 1:After reacting 1h at 1,80 DEG C, no alcohol taste is concentrated into, is spray-dried to get one sylvite of glycyrrhizic acid
22.5kg。
Embodiment 2：
A kind of preparation method of potassium glycyrrhizana, it is characterised in that include the following steps：
(1) preparation of Radix Glycyrrhizae acid solution：5kg activated carbons are added in 100kg glycyrrhizic acid coarse powder, with the quality of 6 times of amounts
A concentration of 85% ethanol solution refluxing extraction 2h at 70 DEG C is filtered up to Radix Glycyrrhizae acid solution；
(2) ammonification and reflux：It is 4.5 that the Radix Glycyrrhizae acid solution that temperature is obtained to step (1) is maintained, which to add in weak aqua ammonia to adjust pH,
Solid is precipitated in stirring；The 5 times of 95% alcohol reflux 30min extraction of solid wet product weight is added in into obtained solid, while hot mistake
Filter is to get product among ammonium glycyrrhizunate；
(3) conversion of Radix Glycyrrhizae acid solution：Product among above-mentioned ammonium glycyrrhizunate are put into the LX-5 cations equipped with 200kg
In the resin container of exchanger resin, enough ethanol solution stirrings are added in until solution is clarified, extraction solution is molten to get glycyrrhizic acid
Liquid；
(4) preparation of sylvite：Above-mentioned Radix Glycyrrhizae acid solution is calculated into its glycyrrhizic acid content after testing, in being concentrated in retort
To dilute alcohol, add in the potassium ion solution of the corresponding amount prepared, in potassium ion solution contained potassium ion amount in Radix Glycyrrhizae acid solution
The molar ratio of glycyrrhizic acid amount is 2:After reacting 1h at 1,80 DEG C, no alcohol taste is concentrated into, is spray-dried to get dipotassium glycyrrhizinate salt
24.5kg。
Embodiment 3：
A kind of preparation method of potassium glycyrrhizana, it is characterised in that include the following steps：
(1) preparation of Radix Glycyrrhizae acid solution：10kg activated carbons are added in 100kg glycyrrhizic acid coarse powder, with the quality of 6 times of amounts
A concentration of 95% ethanol solution refluxing extraction 2h at 70 DEG C is filtered up to Radix Glycyrrhizae acid solution；
(2) ammonification and reflux：It is 5.5 that the Radix Glycyrrhizae acid solution that temperature is obtained to step (1) is maintained, which to add in weak aqua ammonia to adjust pH,
Solid is precipitated in stirring；The 95% alcohol reflux 30min extractions of 8 times of solid wet product weight are added in into obtained solid, are filtered while hot,
Up to product among ammonium glycyrrhizunate；
(3) conversion of Radix Glycyrrhizae acid solution：Product among above-mentioned ammonium glycyrrhizunate are put into the LS1-010 sun equipped with 200kg
In the resin container of ion exchange resin, enough ethanol solution stirrings are added in until solution is clarified, extraction solution is to get glycyrrhizic acid
Solution；
(4) preparation of sylvite：Above-mentioned Radix Glycyrrhizae acid solution is calculated into its glycyrrhizic acid content after testing, in being concentrated in retort
To dilute alcohol, add in the potassium ion solution of the corresponding amount prepared, in potassium ion solution contained potassium ion amount in Radix Glycyrrhizae acid solution
The molar ratio of glycyrrhizic acid amount is 2:After reacting 1h at 1,80 DEG C, no alcohol taste is concentrated into, is spray-dried to get dipotassium glycyrrhizinate salt
25.0kg。
After testing, quality report is as shown in table 1 for the potassium glycyrrhizana that embodiment 1-3 is prepared：
Table 1：Embodiment 1-3 potassium glycyrrhizana examining reports
To sum up, as can be seen from Table 1, a kind of preparation method of potassium glycyrrhizana of the present invention, the potassium glycyrrhizana of preparation accord with
Test stone is closed, there is following obvious advantage compared with traditional method：A) new technology, easy to operate, energy conservation and environmental protection, practicality
Property is strong；B) mode of the direct stir process of resin container is employed, is directly operated at normal temperatures, it will cannot in high concentration alcoholic solution
After product are directly contacted with resin among the solid of dissolving, it is made gradually to be transformed into the soluble Radix Glycyrrhizae of alcohol by the conversion effet of resin
Acid, this method not only increase inventory, and avoid the flow first dissolved after resin column, and operation week is greatly saved
Phase, it is good to improve efficiency character：C) advantage of ion-exchange resin technique is fully applied, equipment and the cost of material is low, place
Reason amount is big, and product coloration is good, yield and content are high, is suitable for industrialized production, and product color is excellent, crystal is uniform, matter
It measures.
It should be pointed out that more than specific embodiment is only illustrative of the invention and is not intended to limit the scope of the invention,
After having read the present invention, those skilled in the art fall within the modification of the various equivalent forms of the present invention power appended by the application
Profit requires limited range.
Claims (8)
1. a kind of preparation method of potassium glycyrrhizana, it is characterised in that include the following steps：
（1）The preparation of Radix Glycyrrhizae acid solution：Activated carbon is added in glycyrrhizic acid coarse powder, the ethyl alcohol for being 60%-100% with mass concentration
Solution refluxing extraction is filtered up to Radix Glycyrrhizae acid solution；
（2）Ammonification and reflux：Temperature is maintained to step（1）It is 4.0-6.0 that obtained Radix Glycyrrhizae acid solution, which adds in weak aqua ammonia and adjusts pH,
Solid is precipitated in stirring；The 95% alcohol reflux extraction of 1-10 times of solid wet product weight is added in into obtained solid, is filtered while hot, i.e.,
Obtain product among ammonium glycyrrhizunate；
（3）The conversion of Radix Glycyrrhizae acid solution：Product among above-mentioned ammonium glycyrrhizunate are put into processed good resin container, add in foot
The ethanol solution stirring of amount is until solution is clarified, and extraction solution is to get Radix Glycyrrhizae acid solution；The resin is D001, LX-5, LS1-
One kind in 010；
（4）The preparation of sylvite：Above-mentioned Radix Glycyrrhizae acid solution is calculated into its glycyrrhizic acid content after testing, it is dilute in being concentrated into retort
After alcohol, the potassium ion solution of the corresponding amount prepared is added in, contained potassium ion amount and Radix Glycyrrhizae in Radix Glycyrrhizae acid solution in potassium ion solution
The molar ratio of acid amount is 1:1-3:1, after reacting a period of time, no alcohol taste is concentrated into, is spray-dried to get potassium glycyrrhizana.
2. the preparation method of potassium glycyrrhizana according to claim 1, it is characterised in that：The step（1）Middle activated carbon
Addition be glycyrrhizic acid coarse powder weight 1%-10%.
3. the preparation method of potassium glycyrrhizana according to claim 2, it is characterised in that：The step（1）Middle activated carbon
Addition be glycyrrhizic acid coarse powder weight 5%-8%.
4. the preparation method of potassium glycyrrhizana according to claim 1, it is characterised in that：The step（1）Middle ethyl alcohol
Mass concentration is 80%-95%.
5. the preparation method of potassium glycyrrhizana according to claim 1, it is characterised in that：The step（2）Middle weak aqua ammonia
Adjust pH to 4.5-5.0.
6. the preparation method of potassium glycyrrhizana according to claim 1, it is characterised in that：The step（3）Middle resin is
LX-5。
7. the preparation method of potassium glycyrrhizana according to claim 1, it is characterised in that：The step（4）Middle potassium ion
Solution is potassium hydroxide solution, one kind in potassium bicarbonate solution, solution of potassium carbonate.
8. the preparation method of potassium glycyrrhizana according to claim 7, it is characterised in that：The step（4）Middle potassium ion
Solution is solution of potassium carbonate.
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| CN107118252B (en) * | 2017-06-16 | 2020-09-15 | 江苏天晟药业股份有限公司 | Preparation method of glycyrrhizic acid |
| CN108997456A (en) * | 2018-08-23 | 2018-12-14 | 江苏天晟药业股份有限公司 | A kind of preparation method of disodium glycyrrhizinate |
| CN112047992A (en) * | 2020-03-31 | 2020-12-08 | 张家港保税区麦福生物制品有限公司 | Preparation method of glycyrrhizic acid |
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