CN102964342A - Method for quickly precipitating and solidifying washing silymarin in process of removing solvent residue - Google Patents
Method for quickly precipitating and solidifying washing silymarin in process of removing solvent residue Download PDFInfo
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- CN102964342A CN102964342A CN2012105515749A CN201210551574A CN102964342A CN 102964342 A CN102964342 A CN 102964342A CN 2012105515749 A CN2012105515749 A CN 2012105515749A CN 201210551574 A CN201210551574 A CN 201210551574A CN 102964342 A CN102964342 A CN 102964342A
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Abstract
The invention provides a method for quickly precipitating and solidifying washing silymarin in a process of removing a solvent residue, relates to a method for solidifying silymarin, and solves the problems that the production efficiency is low, the time of removing the solvent residue is prolonged, and the silymarin suspends in water when the silymarin is superfinely crushed and mixed with water, and precipitates slowly. The method comprises the steps of: I, stirring water and the silymarin, heating a stirring tank interlayer, stopping stirring when the water temperature in a tank reaches 53-57 DEG C, naturally precipitating, and pumping out solvent residue water separated from the stirring tank after 28-32 min; II, placing silymarin slurry, in which the solvent residue is removed, into a charging basket, adding purified water at the temperature of 70-80 DEG C into the basket, and solidifying the silymarin after 18-22min; and III, splitting the solidified silymarin into blocks, and placing into a dryer for drying. The method has the advantages that the silymarin precipitates and solidifies quickly by regulating water temperature, the time for removing the solvent residue is shortened, and the production efficiency is improved.
Description
Technical field
The present invention relates to silymarin and remove the method for molten residual curing.Be specifically related to a kind of silymarin of washing and remove the method that rapid precipitation is solidified in the molten residual process.
Background technology
At present, existing silymarin is in order to improve quality, the dissolvent residual (acetone) that also contains in the silymarin after micronizing is removed, adopt the washing silymarin, because silymarin is through micronizing, suspend in water when stirring with water, the washing postprecipitation causes the low problem of production efficiency for up to more than 24 hours.
Summary of the invention
The present invention removes molten residual in order to solve existing silymarin, adopt the washing silymarin, because silymarin suspends in water when stirring with water through micronizing, precipitation is slow, so just prolonged and removed the molten residual time, quality is low, and the problem that the production efficiency of silymarin is low provides a kind of silymarin of washing to remove the method that rapid precipitation is solidified in the molten residual process.
The concrete technical scheme that addresses this problem is as follows:
A kind of silymarin of washing of the present invention is removed the method that rapid precipitation is solidified in the molten residual process.The step of this curing is as follows:
Step 1, by weight will be in the silymarin 100kg of micronizing drops into stirred pot, then in stirred pot, add water 220kg, opening stirred pot stirs the silymarin in the tank and water, stir after 25～30 minutes, in the stirred pot interlayer, input steam, when water temperature in the tank reaches 53～57 ℃, stop to stir natural sedimentation, the molten residual water that to separate out after 28～32 minutes is extracted out, and said process repeats 3 times;
Step 2, put into bucket with removing molten silymarin slurry after residual in the step 1, then add temperature in the bucket and be pure water 45～55kg of 70～80 ℃, the limit adds the waterside stirs with agitator, adds complete the stopping of water and stirs, and silymarin curing is finished after 18～22 minutes;
Step 3, the silymarin that solidifies in the step 2 is divided into piece, puts into dryer and dry and get final product.
A kind of silymarin of washing of the present invention is removed the method that rapid precipitation is solidified in the molten residual process, to adopt the conciliation water temperature to make silymarin rapid precipitation, (each wash-out is than originally saving more than 20 hours), fast setting, for going molten residual process to save the time, the quality of silymarin and the advantage of production efficiency have been improved.
Description of drawings
Fig. 1 is the structural representation of stirred pot.
Embodiment
Embodiment one: the step of the curing of present embodiment washing silymarin is as follows:
Step 1, to drop into through the silymarin 100kg of micronizing in the stirred pot by weight, then in stirred pot, add water 220kg, opening stirred pot stirs the silymarin in the tank and water, stir after 25～30 minutes, in the stirred pot interlayer, input steam, when reaching 53～57 ℃, water temperature in the tank stops to stir, natural sedimentation, the molten residual water that to separate out after 28～32 minutes is extracted out, said process repeats 3 times, more desolventizings of number of times residual effect fruit better (acetone is water-soluble, and desolventizing is residual, will remain in exactly the acetone discharge soluble in water in the silymarin);
Step 2, put into bucket with removing molten silymarin slurry after residual in the step 1, then add temperature in the bucket and be pure water 45～55kg of 70～80 ℃, the limit adds the waterside and stirs with agitator that (stirring is to allow in the bucket silymarin temperature is consistent up and down, make the even of its curing), silymarin curing is finished after 18～22 minutes;
Step 3, the silymarin that solidifies in the step 2 is divided into piece, puts into dryer and dry and get final product.
Embodiment two: not being both in the stirred pot interlayer after water and silymarin stir in the step 1 of present embodiment and embodiment one heated, when reaching 55 ℃, water temperature in the tank stops to stir, natural sedimentation after 30 minutes is extracted the molten residual water of separating out in the stirred pot out; Remove molten silymarin slurry after residual in the step 2 and put into bucket, then add temperature in the bucket and be 75 ℃ pure water, silymarin solidifies and finishes after 20 minutes.Present embodiment is preferred forms.
Claims (2)
1. wash the method that silymarin is removed rapid precipitation curing in the molten residual process for one kind, it is characterized in that the step of the method is as follows:
Step 1, by weight will be in the silymarin 100kg of micronizing drops into stirred pot, then in stirred pot, add water 220kg, opening stirred pot stirs the silymarin in the tank and water, stir after 25～30 minutes, in the stirred pot interlayer, input steam, when water temperature in the tank reaches 53～57 ℃, stop to stir natural sedimentation, the molten residual water that to separate out after 28～32 minutes is extracted out, and said process repeats 3 times;
Step 2, put into bucket with removing molten silymarin slurry after residual in the step 1, then add temperature in the bucket and be pure water 45～55kg of 70～80 ℃, the limit adds the waterside stirs with agitator, adds complete the stopping of water and stirs, and silymarin curing is finished after 18～22 minutes;
Step 3, the silymarin that solidifies in the step 2 is divided into piece, puts into and get final product after dryer is dried.
2. a kind of silymarin of washing according to claim 1 is removed the method that rapid precipitation is solidified in the molten residual process, it is characterized in that heating in the stirred pot interlayer after water and silymarin stir in the step 1, when reaching 55 ℃, water temperature stops to stir, natural sedimentation after 30 minutes is extracted the molten residual water of separating out in the stirred pot out; Remove molten silymarin slurry after residual in the step 2 and put into bucket, then add temperature in the bucket and be 75 ℃ pure water, silymarin solidifies and finishes after 20 minutes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210551574.9A CN102964342B (en) | 2012-12-18 | 2012-12-18 | Method for quickly precipitating and solidifying washing silymarin in process of removing solvent residue |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201210551574.9A CN102964342B (en) | 2012-12-18 | 2012-12-18 | Method for quickly precipitating and solidifying washing silymarin in process of removing solvent residue |
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| Publication Number | Publication Date |
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| CN102964342A true CN102964342A (en) | 2013-03-13 |
| CN102964342B CN102964342B (en) | 2015-05-13 |
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| CN201210551574.9A Expired - Fee Related CN102964342B (en) | 2012-12-18 | 2012-12-18 | Method for quickly precipitating and solidifying washing silymarin in process of removing solvent residue |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110878093A (en) * | 2019-12-18 | 2020-03-13 | 湖南千金协力药业有限公司 | Preparation method of high-purity silybin |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5764688A (en) * | 1980-10-08 | 1982-04-19 | Madaus & Co Dr | Method of obtaining silymarin from plant |
| CN1463970A (en) * | 2002-06-12 | 2003-12-31 | 中国科学院山西煤炭化学研究所 | Process for preparing silymarin |
| CN1560046A (en) * | 2004-03-03 | 2005-01-05 | 西安理工大学 | Process for extracting water grind thisvine using alcohole as single organic dissolvent |
| CN101260105A (en) * | 2007-03-06 | 2008-09-10 | 江苏天士力帝益药业有限公司 | Method for extracting silibinin |
| CN102558162A (en) * | 2010-12-20 | 2012-07-11 | 佳木斯三江水飞蓟素制品有限公司 | Processing and extraction method for silybin with low soluble residues and high content |
-
2012
- 2012-12-18 CN CN201210551574.9A patent/CN102964342B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5764688A (en) * | 1980-10-08 | 1982-04-19 | Madaus & Co Dr | Method of obtaining silymarin from plant |
| CN1463970A (en) * | 2002-06-12 | 2003-12-31 | 中国科学院山西煤炭化学研究所 | Process for preparing silymarin |
| CN1560046A (en) * | 2004-03-03 | 2005-01-05 | 西安理工大学 | Process for extracting water grind thisvine using alcohole as single organic dissolvent |
| CN101260105A (en) * | 2007-03-06 | 2008-09-10 | 江苏天士力帝益药业有限公司 | Method for extracting silibinin |
| CN102558162A (en) * | 2010-12-20 | 2012-07-11 | 佳木斯三江水飞蓟素制品有限公司 | Processing and extraction method for silybin with low soluble residues and high content |
Non-Patent Citations (1)
| Title |
|---|
| 段更利: "《药物分析基础》", 31 May 2001, article "（六）沉淀条件的选择", pages: 80 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110878093A (en) * | 2019-12-18 | 2020-03-13 | 湖南千金协力药业有限公司 | Preparation method of high-purity silybin |
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