CN2887403Y - Device for separating surface active substance from aqueous extraction of traditional Chinese medicine - Google Patents

Abstract

The utility model discloses a device for separating surface active substance from aqueous extraction of the traditional Chinese medicine which automatically separates and collects the surface active substance from aqueous extraction of the traditional Chinese medicine such as saponin by making use of the principle of foam separation, and comprises a single stage foam separation tower, a multiple stage foam separation device and a foam breaking device; wherein the single stage foam separation tower comprises a gas distributor, a bubbling section, a bubble dilating section and a foam delivery pipe which are all connected with normal grinding joints, the first stage foam separation tower of the multiple stage foam separation device is connected with the raw material pool by a general feed pipe, the last stage foam separation tower is communicated with the raw material pool by a residual liquid duct, and the aqueous extraction could be recycled. The utility model is simple in structure, easy to install and operate, low in production cost, small in volume, and has a small floor area, is made of transparent material which allows naked-eye observing the condition of the foam and foam operation in the tower, has a high separation efficiency, makes the purity of the product obviously increased in comparison with the raw material liquid, and completely realizes the mechanization and automation of the art of separation of aqueous extraction. The device can effectively separate and collect the liquorice saponin in the aqueous extraction of liquorice.

Description

The device of surface reactive material in a kind of separating traditional Chinese medicine water extract

Technical field:

The utility model relates to the device of active material in a kind of separation, the enrichment Chinese traditional medicine water extract, particularly a kind of device that utilizes surface reactive materials such as the separation of foam separation principle, enrichment glycyrrhizin.

Background technology:

Foamet be rose in 20th century, with bubble as concentrate a kind of new separation technology of surface reactive material of separating medium.Over nearly 30 years, this The Application of Technology field is constantly enlarged, and especially the foam adsorbing separation to materials such as metal ion, protein, enzyme and Chinese herb soap glycosides enjoys people to pay close attention to.So-called foam separating technology is meant and a kind ofly provides gas-liquid interface based on surface-active difference between solute with form of foam, separates the separation method that concentrates the surface-active solute.Characteristics such as this technology has that equipment is simple, easy operating, cost are low, good separating effect are used widely in fields such as ore dressing, sewage disposal, Biochemical Engineering.

Active material in the Chinese traditional medicine water extract as saponin(e, has the capillary characteristic of the aqueous solution of reduction, has surface-active.Saponin(e is a class can produce a large amount of lasting foams through jolting in the aqueous solution a complicated molecule, and being linked to each other by carbon bond with triterpenes, steroidal or steroid alkaloid by sugar chain forms.They extensively are present in stem, leaf and the root of plant, as genseng, pseudo-ginseng, gynostemma pentaphylla, radix bupleuri, the root of bidentate achyranthes, balloonflower root, the Radix Astragali, Radix Glycyrrhizae, ilex pubescens, polygala root, soapberry etc., and have physiologically active.Show through The experimental results; these saponin(es have pharmacological action widely and biologically active such as immunization, antitumor, antimycotic, the spiral shell that goes out, killing blood fluke, prevent and treat angiocardiopathy etc., but also can be used as natural food sweetener, protective agent, blowing agent, flavoring agent, antioxidant etc.Because saponins compound polarity is big, water-soluble strong, separation, refining acquiring a certain degree of difficulty.The separation of saponin(e, process for purification adopt the heavy method of acid, alcohol deposition method, macroporous absorbent resin method etc. more.Shortcomings such as these methods all must be special with a large amount of organic chemical reagents or needs, not only increased cost, and brought pollution to a certain extent, in addition, also exists mechanization degree low, and the technology reappearance is relatively poor.

In recent years, marked improvement along with separation means, both at home and abroad except that using classical saponin(e separation method, some have been developed again to the effectively new isolation technics of saponin(e, as separation, process for purification such as extractive technique such as supercritical liquid extraction technique, semi-bionic extraction, ultrasonic extraction, macroporous absorbent resin technology and high performance liquid chromatography (HPLC), droplet countercurrent chromatographies.The one-time investment of supercritical liquid extraction technique equipment is too big, has improved cost; Ultrasound assisted extraction technique still is confined in quality analysis of traditional Chinese medicine and a small amount of the extraction at present, is still waiting further its equipment etc. is groped but be used for large-scale production; Semi-bionic extraction will obtain to stablize feasible technology in the middle of using, and realizes that suitability for industrialized production still need do lot of experiments, at present this technology industrial applications that still is unrealized.There are shortcomings such as adsorptive selectivity is poor, technical difficulty is big, resin regeneration difficulty in the macroporous absorbent resin technology.But, process stabilizing, feasible, economy, good separating effect, simple equipments, cheap and easy to get, can realize that the process equipment that engineering is amplified does not also have.

Utilize the successful experience of foam separating technology in other sector application, and make full use of the natural surface-active effect of Chinese medicine saponin(e, with the bubble is separating medium, saponins and the surface-active macromolecular compound of other tool in separation, the enrichment Chinese medicine extract, be the modern study of foam separating technology, but open research report, the patent of this aspect are not seen as yet so far.

Summary of the invention:

The purpose of the present utility model is intended to overcome the defective of above-mentioned technology, a kind of separation, enrichment saponin component foam separator are provided, this device can be realized automation, the serialization production of saponins surface reactive material, improves the quality of product, reduces production costs.The technical solution of the utility model is as follows:

The utility model comprises multistage foam separator and broken bulb apparatus, and multistage foam separator is for multistage polyphone foam lock out operation.Multistage foam separator described in the utility model be by two-stage and more than, as three grades, level Four, Pyatyi, six grades, seven grades compositions, each grade foam separating tower connects with connecting duct.Every grade of foam separating tower is made up of gas distributor, bubbling segment, foam amplification section, foam delivery line, and the gas distributor below is connected to air inlet, is used to be input into compressed air, and the charging aperture position difference of foam separating towers at different levels reduces step by step, and its structure is seen Fig. 1.

Device of the present invention, constitute by multistage foam separator and broken foamite system, described multistage foam separator is formed by connecting with conduit respectively by two above foam separating towers, foam separating tower is by gas access (8), gas distributor (9), bubbling area (10), foam amplification region (11), charging aperture (12), foam delivery line (13) is formed, wherein gas access (8) are positioned at below of foam separating tower, gas distributor (9) is positioned at the top, gas access, bubbling area (10) is positioned at the gas distributor top, foam amplification region (11) is positioned at the bubbling area top, charging aperture (12) is between bubbling area and foam amplification region, the top is foam delivery line (13), the charging aperture position difference of foam separating towers at different levels, knockout tower (1) charging aperture position is the highest, reduce step by step, described broken foamite system is by foam inlet, the foam solution outlet, air outlet slit and an internal fan are formed, and described foam inlet extend into brokenly foamite system inside from the middle part, and the foam solution outlet is positioned at brokenly the foamite system bottom, air outlet slit is positioned at brokenly foamite system top, and the internal fan air port is between foam inlet and air outlet slit.

Wherein gas distributor is a glass sand plate, be by with separate post jamb coefficient of expansion machine with glass pulverize, the sand powder sintering between No. two sieves and No. three sieves forms.

Broken bulb apparatus described in the utility model is made up of foam inlet, foam solution outlet, air outlet slit and an internal fan.The inlet of bulb apparatus is collected and sent constantly into brokenly to foam endlessly, is broken into liquid under the continuous cold blowing of blower fan is moving, discharged by the foam solution outlet again, obtains product.

The utility model is simple in structure, is easy to install and operation, and with low cost, volume is little, and floor space is little, and the mechanization degree height can be realized automation, the product purity height, and quality is good; Can in separate, enrichment have surface-active material, as saponin(e, specifically has surface-active material as glycyrrhizin and as contained saponin(es such as genseng, pseudo-ginseng, gynostemma pentaphylla, radix bupleuri, the root of bidentate achyranthes, balloonflower root, the Radix Astragali, ilex pubescens, polygala root, soapberry etc.

Principle of the present utility model is to utilize the gas distributor with very tiny aperture that gas dispersion is become micro-bubble, gas, water are fully mixed, because the effect of bubble surface tension force, make glycyrrhizin, protein, fiber and mucus etc. in the water have surface-active organic substance and be adsorbed in bubble surface, foam separator utilizes the poor of gas, water proportion again, have surface active ingredient and can with the bubble of the material of surface active ingredient complexing under buoyancy, rise to liquid level, form foam.Purify the liquid phase main body thereby reach, concentrate, the purpose of release surface active component.Foam separator is the organic particle in the separation solution, saponin(e, protein, metal ion etc. effectively.The gained foam is more stable, can adopt brokenly bulb apparatus to carry out froth breaking, obtains the foam solution product.

The course of work of multistage foam separator described in the utility model and principle (Fig. 1): material liquid injects in the first order foam separating tower from feed reservoir with water pump, compressed air blasts in the tower from knockout towers at different levels lower end, foam is discharged from the foam delivery line, raffinate after at different levels handling flows into the next stage foam separating tower from residual liquid outlet, continuing foam separates, the residual liquid that the residual liquid outlet of afterbody is discharged is back to feed reservoir once more, circular treatment can't be accumulated to outlet until foam.

The course of work of broken bulb apparatus described in the utility model and principle (Fig. 2): stable foam is disposed to brokenly the foam inlet of bulb apparatus from the afterbody foam delivery line of multistage foam separator, under the blowing of the continuous cold air of internal fan, lather collapse becomes liquid, and discharge from the outlet of the foam solution of bottom, the circulating air that is produced is discharged by the air outlet slit at top.

Description of drawings:

Fig. 1 is a multistage foam separator of the present utility model;

Wherein 1～7 be respectively one to seven grade of foam separating tower 8, gas access 9, gas distributor 10, bubbling area 11, foam amplification region 12, charging aperture 13, foam delivery line 14, connecting duct

Fig. 2 is a broken bulb apparatus of the present utility model;

Wherein 1, foam inlet 2, foam solution outlet 3, air outlet slit 4, internal fan

Wherein, the foam of multistage foam separator afterbody foam delivery line and broken bulb apparatus inlet links to each other with pipeline.

The specific embodiment:

Further specify below in conjunction with specific embodiment.

Embodiment 1 is as accompanying drawing 1, and multistage foam separator described in the utility model can be to be formed by connecting with emulsion tube respectively by seven grades of foam separating towers.Foam separating towers at different levels are made up of gas access, gas distributor, bubbling segment, foam amplification section, foam delivery line, on the bubbling segment shell of foam separating towers at different levels a charging aperture are arranged, and every grade charging aperture position difference reduces step by step.The collected foam of foam delivery line that merges foam separating towers at different levels top, and bubble is broken in its unification handle.The raffinate of discharging from residual liquid outlet follows back feed reservoir again, and recycling can't be accumulated to outlet, shut-down operation until foam.

Embodiment 2 is as accompanying drawing 2, and broken bulb apparatus described in the utility model is made up of foam inlet, foam solution outlet, air outlet slit and an internal fan.The foam of collected foam being sent constantly into brokenly bulb apparatus enters the mouth, and is broken into liquid under the continuous cold blowing of blower fan is moving, is discharged by the foam solution outlet again, obtains product, and the gas of generation is discharged by air outlet slit.

Embodiment 3 utilizes the explanation of the beneficial effect of the utility model generation.

Take by weighing Radix Glycyrrhizae meal 100g, add 15 times of water gagings and decoct 3 times, each 2 hours, collecting decoction.High speed centrifugation, 4000r/min30 minute, get supernatant, 4 times of dilute with waters add the foam separator, carry out foam and separate under the best intermittent operation technological parameter condition that obtains through The effects.Collect foam, froth breaking, foam solution, are pulverized to constant weight in 70 ℃ of constant temperature vacuum drying, get the glycyrrhizic acid inclusion compound powder.

Simultaneously, adopt following contrast method to prepare glycyrrhizic acid inclusion compound:

(1) extracting liquorice meal 100g adds 15 times of water gagings and decocts 3 times, and each 2 hours, collecting decoction.Decompression concentrates.Concentrate adds 3.5mol/L sulfuric acid after being cooled to room temperature, and adjust pH is 2, leaves standstill 12 hours, and the glycyrrhizic acid precipitation is separated out.Filter, precipitation is washed 3 times with distilled water, and water is drained, and, pulverizes to constant weight in 70 ℃ of constant temperature vacuum drying, gets the glycyrrhizic acid inclusion compound powder.

(2) extracting liquorice meal 100g adds 15 times of water gagings and decocts 3 times, and each 2 hours, collecting decoction.Be evaporated to 1/6 of original volume, slowly add 85% ethanol, the limit edged stirs, in solution, contain amount of alcohol and reach about 65%, standing over night, it is standby to get supernatant, precipitation adds 65% ethanol with the supernatant equal volume again, fully stirs standing over night, the taking-up supernatant is standby, and precipitation is used 65% alcohol extract once again, merges No. three extracts [3], filter, reclaim ethanol, in 70 ℃ of constant temperature vacuum drying to constant weight, pulverize, get the glycyrrhizic acid inclusion compound powder.

(3) extracting liquorice meal 100g adds 12 times of amount 0.5% ammoniacal liquor diacolations, floods half an hour before the diacolation, and the diacolation flow velocity is 5ml/min/kg, collects percolate.Get percolate decompression and concentrate, it is 2 that the concentrated sulfuric acid that adds 3.5mol/L in concentrate transfers to pH value, leaves standstill, and separates out precipitation and filters, and distillation water washing and precipitating 3 times, is pulverized to constant weight in 70 ℃ of constant temperature vacuum drying, gets the glycyrrhizic acid inclusion compound powder.

(4) take by weighing Radix Glycyrrhizae meal 100g, carry out refluxing extraction as solvent with 60% ethanolic solution that contains ammonia 0.3%.Adding for the first time the solvent amount is 5 times that Radix Glycyrrhizae is measured, and second and third time respectively is 4 times of amounts; 2h refluxes for the first time, second and third time respectively is 1.5h, merges extract, filters, filtrate decompression concentrates, it is 2 that the concentrated sulfuric acid that adds 3.5mol/L in concentrate transfers to the pH value, leaves standstill, and separates out precipitation and filters, distillation water washing and precipitating 3 times,, pulverize to constant weight in 70 ℃ of constant temperature vacuum drying, get the glycyrrhizic acid inclusion compound powder.

Above method gained glycyrrhizic acid adopts high performance liquid chromatography to carry out assay, and condition determination is as follows:

Chromatographic column: Diamonsil C18 (250mm * 4.6mm, 5 μ m); Detect wavelength: 250nm; Column temperature: 40 ℃; Phase flows: methyl alcohol-0.2mol/L ammonium acetate solution-glacial acetic acid (67: 33: 1).

Sample preparation methods is decided to be: the about 0.2g of extracting liquorice acid crude, accurate claim surely, and put in the tool plug conical flask, the accurate respectively acetone 35ml that adds, close plug claims to decide weight, and ultrasonic processing 30min is put coldly, and close plug claims to decide weight again, supplies the weight that subtracts mistake with acetone, shakes up.Filter, get subsequent filtrate promptly.

The computing formula of evaluation index:

Glycyrrhizic acid inclusion compound purity=glycyrrhizic acid weight (g)/glycyrrhizic acid inclusion compound weight (g) * 100%

Glycyrrhizic acid total amount (g) * 100% in glycyrrhizic acid total amount (g)/medicinal material in the glycyrrhizic acid extraction rate of transform=extract

Glycyrrhizic acid total amount (g) * 100% in glycyrrhizic acid total amount (g)/extract in the glycyrrhizic acid purifying rate of transform=crude product

Glycyrrhizic acid purity in glycyrrhizic acid purity/extract solid content in the purity raising ratio=crude product

Result of the test such as following table:

Method	Water is proposed acid heavy (1)	Water extract-alcohol precipitation (2)	Weak aqua ammonia diacolation acid heavy (3)	Ammonia ethanol is proposed acid heavy (4)	Water is carried foam and is separated
						Medicinal material treating capacity (g) is extracted glycyrrhizic acid purity (%) glycyrrhizic acid inclusion compound purity (%) the purity raising ratio use solvent production cycle (day) in the rate of transform (%) the purifying rate of transform (%) the extract solid content	100 71.94 75.65 21.66 44.71 2.06 water, sulfuric acid (transferring pH) 2	100 71.01 97.52 16.69 27.65 1.66 water, ethanol 4	100 78.89 71.98 23.54 56.78 2.41 ammoniacal liquor, sulfuric acid (transferring pH) 4	100 86.35 69.47 23.12 23.79 1.03 ammoniacal liquor, ethanol, sulfuric acid (transferring pH) 2	100 71.16 91.86 16.05 33.65 2.10 water, hydrochloric acid (transferring pH) 2

Claims (1)

1, the device of surface reactive material in a kind of separating traditional Chinese medicine water extract, it is characterized in that, constitute by multistage foam separator and broken foamite system, described multistage foam separator is formed by connecting with conduit respectively by two above foam separating towers, foam separating tower is by gas access (8), gas distributor (9), bubbling area (10), foam amplification region (11), charging aperture (12), foam delivery line (13) is formed, wherein gas access (8) are positioned at below of foam separating tower, gas distributor (9) is positioned at the top, gas access, bubbling area (10) is positioned at the gas distributor top, foam amplification region (11) is positioned at the bubbling area top, charging aperture (12) is between bubbling area and foam amplification region, the top is foam delivery line (13), the charging aperture position difference of foam separating towers at different levels, knockout tower (1) charging aperture position is the highest, reduce step by step, described broken foamite system is by foam inlet, the foam solution outlet, air outlet slit and an internal fan are formed, described foam inlet extend into brokenly foamite system inside from the middle part, the foam solution outlet is positioned at brokenly the foamite system bottom, air outlet slit is positioned at brokenly foamite system top, and the internal fan air port is between foam inlet and air outlet slit.

Images