CN106279345B - A kind of industrialized preparing process of thick glycyrrhizic acid - Google Patents

A kind of industrialized preparing process of thick glycyrrhizic acid Download PDF

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Publication number
CN106279345B
CN106279345B CN201610666967.2A CN201610666967A CN106279345B CN 106279345 B CN106279345 B CN 106279345B CN 201610666967 A CN201610666967 A CN 201610666967A CN 106279345 B CN106279345 B CN 106279345B
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acid
feed liquid
extraction
thick
glycyrrhizic acid
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CN106279345A (en
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张志明
杨香瑜
额尔敦巴雅尔
安晓东
连运河
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Chenguang Biotech Group Co Ltd
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Chenguang Biotech Group Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07JSTEROIDS
    • C07J63/00Steroids in which the cyclopenta(a)hydrophenanthrene skeleton has been modified by expansion of only one ring by one or two atoms
    • C07J63/008Expansion of ring D by one atom, e.g. D homo steroids
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07HSUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
    • C07H1/00Processes for the preparation of sugar derivatives
    • C07H1/06Separation; Purification
    • C07H1/08Separation; Purification from natural products
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07HSUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
    • C07H15/00Compounds containing hydrocarbon or substituted hydrocarbon radicals directly attached to hetero atoms of saccharide radicals
    • C07H15/20Carbocyclic rings
    • C07H15/24Condensed ring systems having three or more rings
    • C07H15/256Polyterpene radicals

Abstract

The invention discloses a kind of industrialized preparing process of thick glycyrrhizic acid, comprise the following steps:Radix glycyrrhizae is pulled into by wire drawing machine Filamentous or powdered, is extracted by the use of hot water as Extraction solvent, obtain extracting solution, the feed liquid of extraction is cooled down, after cooling centrifugation obtain clarification feed liquid;Feed liquid after centrifugation is carried out to heavy 2 5h of standing acid after adjusting acid, tune sour in sour tank, after the feed liquid after sour sink is filtered, the solid filtered out washes to obtain wet product, and wet product is dried to obtain thick radix glycyrrhizae acid product.The present invention is extracted using hot water circulated in countercurrent, and combines cooling impurity removal process, is saved water source, is ensured the recovery rate of product, later-period purification technique is simple to operation, and obtained thick glycyrrhizic acid unit of the product content >=45%, easily realizes industrialized production.

Description

A kind of industrialized preparing process of thick glycyrrhizic acid
Technical field
The invention belongs to natural extract technical field, more particularly to a kind of industrialized preparing process of thick glycyrrhizic acid.
Background technology
Glycyrrhizic acid is the main compound in radix glycyrrhizae, and glycyrrhizic acid is mainly applied in fields such as food, medicine, daily use chemicals at present, With good physiological function.
The extracting mode of glycyrrhizic acid is many at present, and main Extraction solvent has dilute alcohol solution, weak aqua ammonia and ammonia ethanol solution, Substantial amounts of impurity component can be caused to be suggested using these solvent extractions, the purifying to later product causes to bear.It is such as public The number of opening is in CN102304165A patents, and using dilute alcohol as solvent extraction, the later stage also needs to hand over using ion for glycyrrhizic acid extraction Change resin to be purified, not only lose time but also the also danger of dissolvent residual.Publication No. CN1031300863A patents In, using ammonia ethanol as solvent extraction glycyrrhizic acid, obtained glycyrrhizic acid purity is extremely low, and content is only capable of reaching 9% or so, and Have the danger of dissolvent residual.Obtained in Publication No. CN103588831A patents using ammonia ethanol as Extraction solvent Extracting solution is after peracid sinks, it is also necessary to by preparing liquid phase purified glycyrrhizic acid, although obtained product purity is higher, and technique It is too cumbersome, it is impossible to meet industrialized production.
Industrial glycyrrhizic acid extracting mode is mainly extracted using cold water diacolation mode, which takes longer, and recovery rate is low, And the later stage can produce substantial amounts of waste water.Wastewater treatment considerably increases industry cost.Such as Publication No. In CN200910232810 patents, extraction puies forward mode using water and carries out, extraction need to spend 48 it is small when as long as, and can produce at least The waste water of 10 times of volumes, and recovery rate is relatively low.Therefore on the premise of recovery rate is ensured, a kind of relatively low water of water consumption is developed Technique is put forward, problem of environmental pollution can not only be solved, and the present situation of purifying products complex process can be solved, is more advantageous to reality Existing industrialized production.
The content of the invention
Alcohol extracting and buck extraction impurity are more in order to solve in existing glycyrrhizic acid production method, and cold water extraction rate is low, time-consuming The problem of, the present invention provides a kind of industrialized preparing process of thick glycyrrhizic acid, and this method is consolidated circulated in countercurrent using hot water liquid and extracted, Both water consumption is reduced, improves glycyrrhizic acid recovery rate, while is avoided in excessive impurity incorporation product, simplifies purifying process road Line.
In order to solve the above technical problems, the present invention adopts the following technical scheme that:A kind of industrialized production side of thick glycyrrhizic acid Method, comprises the following steps:
(1)Pretreatment of raw material:Radix glycyrrhizae is pulled into by wire drawing machine Filamentous or powdered;
(2)Extraction:Extracted by the use of hot water as Extraction solvent, obtain extracting solution;
(3)Cooling removal of impurities:The feed liquid of extraction is cooled down, is centrifuged after cooling and obtains clarification feed liquid;
(4)Adjust acid:Feed liquid after centrifugation is carried out adjusting acid in the heavy tank of acid, the heavy 2-5h of acid is stood after adjusting acid;
(5)Filter and wash:After feed liquid filtering of the acid after heavy, the solid content filtered out washes to obtain wet product;
(6)Dry finished product:Wet product is dried to obtain thick radix glycyrrhizae acid product.
Step of the present invention(5)Middle filtering is filtered using two passes, when feed temperature≤50 DEG C, is directly filtered.
Step of the present invention(5)Middle filtering is filtered using two passes, as 50 DEG C of feed temperature >, first passes through cooling Tower reduces feed temperature to less than 25 DEG C, then is filtered.
" method that liquid consolidates circulated in countercurrent extraction " concrete operation method of the present invention is as follows:Extractor and pressure series connection of pumps For a working cell, there may be n identical working cells in a set of extraction system(n≥2), radix glycyrrhizae is from first job Unit enters, and extracts 1-2h after being mixed in extractor with water, enters second working cell from radix glycyrrhizae through vibrosieve;And water Enter from n-th working cell, mixed in extractor with radix glycyrrhizae, through vibrosieve from, water enters (n-1)th working cell, Carry out as stated above successively.What the new water of extracting method guarantee contacted forever is all the radix glycyrrhizae that will extract end, is extracted Water in journey can recycled for multiple times, greatly improve extraction efficiency.
Step of the present invention(2)The temperature of middle hot water is 40-80 DEG C, extraction time 5-7 times, feed liquid mass ratio 1:5-7, Each extraction time is 1-1.5h.
Step of the present invention(3)Middle cooling is that feed liquid is cooled to 5-20 DEG C, precipitation is separated out completely.
Step of the present invention(4)The middle acid solution adjusted used in acid is sulfuric acid or hydrochloric acid, concentration 10-30%;Feed liquid is adjusted It is 1.3-1.7 to pH.
Step of the present invention(4)The middle acid adjusted used in acid sinks tank needs with stirring and nozzle;During the tune acid Speed of agitator turns/min for 50-200;The step(5)In be washed to wet product pH value 3-3.5.
Step of the present invention(5)Middle filtering uses plate and frame filter.
Step of the present invention(6)In drying condition be 40-70 DEG C of drying of vacuum, drying time 10-12h.
Recovery rate computational methods of the present invention are:Recovery rate=(Every pot of 1 feed liquid quality * feed liquid units glycyrrhizic acid content+last One pot of last feed liquid quality * feed liquid unit glycyrrhizic acid content)/ total amount of feeding * feed material glycyrrhizic acid contents * 100%
Thick glycyrrhizic acid product inspection method reference in the present invention:2015 editions Chinese Pharmacopoeia detection methods.
Had the beneficial effect that using caused by above-mentioned technical proposal:1st, extraction is extracted using hot water circulated in countercurrent, and is tied Cooling impurity removal process is closed, water source can be saved, ensures the recovery rate of product, and impurity significantly reduces in feed liquid after removal of impurities, Later-period purification technique is simple to operation, obtained thick glycyrrhizic acid unit of the product content >=45%;Save purification step.2nd, product Filtered during filtering using two passes, avoid the fever of filter process middle pump body or feed temperature is too high, cause part glycyrrhizic acid Product is dissolved in supernatant, so as to cause the relatively low phenomenon of product yield.3rd, this method technique is simple to operation, and what is obtained is thick The unit content of product is higher, saves later stage cumbersome purification step, is easier to realize industrial operation.
Embodiment
The present invention is described in further details below in conjunction with embodiment.
Embodiment 1
The licorice raw material 350kg after wire drawing is taken, raw material glycyrrhizic acid content is 3.5%, 45 DEG C of Extracting temperature, extraction unit number 5 It is a, feed liquid mass ratio 1:6, it is every all over extraction 1.5h, feed intake altogether 7 pots, glycyrrhizic acid extracts yield 98.6%;Extracting solution is cooled down immediately To 20 DEG C, impurity is centrifuged off after 30min, then feed liquid is transferred in the heavy tank of acid and carries out adjusting acid, adjusts the stirring during acid Rotating speed is 50 turns/min, and the heavy 2h of acid after feed liquid tune acid to pH1.3, will be stood with 10% sulfuric acid.
By feed liquid plate-frame filtering of the acid after heavy, feed liquid inceptive filtering temperature is at 25 DEG C, after 20nin is filtered, since pump is sent out Heat, causes feed temperature to reach 55 DEG C, then switches to cooling duct, after cooling tower circulation temperature lowering 20min, measures feed liquid Temperature reaches 20 DEG C, is then switched to filtration channel again.
After filtering, 3 washings stop cleaning when solid content pH is washed till 3, and wet 65 DEG C of vacuum drying of product obtain The thick radix glycyrrhizae acid products of 25.35kg, thick glycyrrhizic acid unit of the product content are 46.21%, and total content yield is 95.63%.
Embodiment 2
The powdered licorice raw material 400kg after wire drawing is taken, raw material glycyrrhizic acid content is 2.80%, 65 DEG C of Extracting temperature, extraction Unit number 5, feed liquid mass ratio 1:5, it is every all over extraction 1.2h, feed intake altogether 8 pots, glycyrrhizic acid extracts yield 97.9%;By feed liquid immediately 15 DEG C are cooled to, impurity is centrifuged off after 60min, then feed liquid is transferred in the heavy tank of acid and carries out tune acid, during tune acid Speed of agitator is 200 turns/min, and the heavy 3h of acid after feed liquid tune acid to pH1.5, will be stood with 15% hydrochloric acid.
By feed liquid plate-frame filtering of the acid after heavy, feed liquid inceptive filtering temperature is at 20 DEG C, after 40nin is filtered, since pump is sent out Heat, causes feed temperature to reach 51 DEG C, then switches to cooling duct, after cooling tower circulation temperature lowering 15min, measures feed liquid Temperature reaches 23 DEG C, is then switched to filtration channel again.
After filtering, 4 washings stop cleaning when solid content pH is washed till 3.5, and wet 65 DEG C of vacuum drying of product obtain To the thick radix glycyrrhizae acid products of 23.87kg, thick glycyrrhizic acid unit of the product content is 45.11%, and total content yield is 96.14%.
Embodiment 3
The licorice raw material 700kg after wire drawing is taken, raw material glycyrrhizic acid content is 3.81%, 80 DEG C of Extracting temperature, extraction unit number For 6, feed liquid mass ratio 1:7, it is every all over extraction 1h, feed intake altogether 7 pots, glycyrrhizic acid extracts yield 97.0%;Feed liquid is cooled to immediately 20 DEG C, impurity is centrifuged off after 1.5h, then feed liquid is transferred in the heavy tank of acid and carries out adjusting acid, adjusts the speed of agitator during acid For 100 turns/min, the heavy 2.5h of acid after feed liquid tune acid to pH1.7, will be stood with 30% sulfuric acid.
By feed liquid plate-frame filtering of the acid after heavy, feed liquid inceptive filtering temperature is at 25 DEG C, after 30nin is filtered, since pump is sent out Heat, causes feed temperature to reach 58 DEG C, then switches to cooling duct, after cooling tower circulation temperature lowering 30min, measures feed liquid Temperature reaches 21 DEG C, is then switched to filtration channel again.
After filtering, 3 washings stop cleaning when solid content pH is washed till 3, and wet 65 DEG C of vacuum drying of product obtain The thick radix glycyrrhizae acid products of 53.31kg, thick glycyrrhizic acid unit of the product content are 47.31%, and total content yield is 94.57%.
Above example is only to illustrative and not limiting technical scheme, although with reference to above-described embodiment to this hair It is bright to be described in detail, it will be understood by those of ordinary skill in the art that:Still the present invention can be modified or be waited With replacing, any modification or partial replacement without departing from the spirit and scope of the present invention, it should all cover the power in the present invention Among sharp claimed range.

Claims (7)

1. a kind of industrialized preparing process of thick glycyrrhizic acid, it is characterised in that comprise the following steps:
(1)Pretreatment of raw material:Radix glycyrrhizae is pulled into by wire drawing machine Filamentous or powdered;
(2)Extraction:Extracted by the use of hot water as Extraction solvent, obtain extracting solution;
(3)Cooling removal of impurities:The feed liquid of extraction is cooled down, is centrifuged after cooling and obtains clarification feed liquid;
(4)Adjust acid:Feed liquid after centrifugation is carried out adjusting acid in the heavy tank of acid, the heavy 2-5h of acid is stood after adjusting acid;
(5)Filter and wash:After feed liquid filtering of the acid after heavy, the solid content filtered out washes to obtain wet product;
(6)Dry finished product:Wet product is dried to obtain thick radix glycyrrhizae acid product;
The step(5)Middle filtering is filtered using two passes, and as 50 DEG C of feed temperature >, first passing through cooling tower reduces feed liquid Temperature is to less than 25 DEG C, then is filtered;
The step(2)Middle extracting method is " method that liquid consolidates circulated in countercurrent extraction ", and concrete operation method is as follows:Extractor with Pressure series connection of pumps is a working cell, and there are n identical working cells in a set of extraction system, n >=2, radix glycyrrhizae is from first A working cell enters, and extracts 1-2h after being mixed in extractor with water, enters second job note from radix glycyrrhizae through vibrosieve Member;And water enters from n-th of working cell, mixed in extractor with radix glycyrrhizae, through vibrosieve from water enters (n-1)th work Make unit, carry out as stated above successively;
The step(3)Middle cooling is that feed liquid is cooled to 5-20 DEG C, precipitation is separated out completely;
The step(4)The middle acid adjusted used in acid sinks tank needs with stirring and nozzle;It is described adjust acid during speed of agitator be 50-200 turns/min.
A kind of 2. industrialized preparing process of thick glycyrrhizic acid according to claim 1, it is characterised in that the step(5) Middle filtering is filtered using two passes, when feed temperature≤50 DEG C, is directly filtered.
A kind of 3. industrialized preparing process of thick glycyrrhizic acid according to claim 1, it is characterised in that the step(2) The temperature of middle hot water is 40-80 DEG C, extraction time 5-7 times, feed liquid mass ratio 1:5-7, each extraction time are 1-1.5h.
A kind of 4. industrialized preparing process of thick glycyrrhizic acid according to claim 1, it is characterised in that:The step(4) The middle acid solution adjusted used in acid is sulfuric acid or hydrochloric acid, concentration 10-30%;It is 1.3-1.7 that feed liquid, which is adjusted to pH,.
A kind of 5. industrialized preparing process of thick glycyrrhizic acid according to claim 1-4 any one, it is characterised in that:Institute State step(5)In be washed to wet product pH value 3-3.5.
A kind of 6. industrialized preparing process of thick glycyrrhizic acid according to claim 1-4 any one, it is characterised in that institute State step(5)Middle filtering uses plate and frame filter.
A kind of 7. industrialized preparing process of thick glycyrrhizic acid according to claim 1-4 any one, it is characterised in that:Institute State step(6)In drying condition be 40-70 DEG C of drying of vacuum, drying time 10-12h.
CN201610666967.2A 2016-08-15 2016-08-15 A kind of industrialized preparing process of thick glycyrrhizic acid Active CN106279345B (en)

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CN108997470A (en) * 2018-08-31 2018-12-14 杨雯君 A method of extracting glycyrrhizic acid
CN111100181A (en) * 2019-12-31 2020-05-05 中国医药健康产业股份有限公司 Method for extracting glycyrrhizic acid crude product from liquorice

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JPS6219436B2 (en) * 1979-12-15 1987-04-28 Maruzen Kasei Co Ltd
KR20010068749A (en) * 2000-01-08 2001-07-23 김경재 A manufacturing method of licorice extract suitable to production of soy sauce
CN103467559A (en) * 2013-09-17 2013-12-25 南京通泽农业科技有限公司 New method for extracting glycyrrhizic acid from liquorice
CN103860631A (en) * 2014-03-04 2014-06-18 内蒙古普凡生生物科技有限公司 Method for preparing liquorice active substances
CN104262448B (en) * 2014-09-07 2017-02-08 四川宝鼎香中药科技开发有限公司 Method for extracting glycyrrhizic acid for licorice
CN204265665U (en) * 2014-11-07 2015-04-15 新疆昌吉康隆生物科技有限公司 One is provided with the heavy tank Potenlini preparation facilities of acid
CN105541957A (en) * 2016-03-04 2016-05-04 脱德明 Extraction method for increasing content of glycyrrhizic acid in leftover materials of liquorice

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