CN103071390B - System and method for purifying several natural substances through ultrafiltration and membrane extraction coupled technique - Google Patents
System and method for purifying several natural substances through ultrafiltration and membrane extraction coupled technique Download PDFInfo
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- CN103071390B CN103071390B CN201310047146.7A CN201310047146A CN103071390B CN 103071390 B CN103071390 B CN 103071390B CN 201310047146 A CN201310047146 A CN 201310047146A CN 103071390 B CN103071390 B CN 103071390B
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Abstract
The invention relates to a system and a method for purifying several natural substances through an ultrafiltration and membrane extraction coupled technique. The system comprises an ultrafiltration membrane assembly and a same-level extraction and back-extraction membrane assembly which is connected with a back-extraction agent storage tank, an extraction agent storage tank, a back-extraction solution storage tank and a buffer tank. An ultrafiltrate and raffinate storage tank is respectively connected with the buffer tank and the ultrafiltration membrane assembly. Extraction membranes and back-extraction membranes are arranged in the same-level extraction and back-extraction membrane assembly. After plants are extracted by adopting a conventional method, an extraction solution is ultrafiltrated, a trapped solution is collected or is reconcentrated, the pH (potential of hydrogen) value of the trapped solution is regulated, then the trapped solution is fed into the same-level extraction and back-extraction membrane assembly, target substances in the trapped solution are separated through extraction and back-extraction or extraction only, and a back-extraction solution or an extraction solution is treated by adopting a conventional method to obtain the target substances. Two techniques, i.e. ultrafiltration and membrane extraction are coupled in use, the pollution of the extraction membranes can be remarkably reduced, the advantages of high efficiency, high accuracy, small pollution and low cost of membrane extraction for substance separation are fully exploited, and the membrane extraction technique can be used in the field of natural substance separation.
Description
Technical field
The invention belongs to natural materials separation technology field, relate to a kind of separation and purification system for middle polarity natural materials such as Alkaloids in Plants, flavones, anthraquinone, saponin(es, be specifically related to the system of a kind of coupling ultrafiltration technology and a few class natural materials of membrane extraction technology separation and purification; The invention still further relates to a kind of method of utilizing the above a few class natural materials of this system separation and purification.
Background technology
In plant, there is the multiple natural materials with value, as alkaloid, flavones, saponin(e, anthraquinone etc., in plant, extract these materials, need further separation and purification to improve purity, the methods such as industrial main employing liquid-liquid extraction method, chromatography, the precipitation method, film separation are at present carried out separation and purification.
Liquid-liquid extraction method utilizes separated each material (solute) different from the distribution coefficient between extraction phase at water, by two alternate repeated dispensing separate substances, applies more extensive.Main single-stage or the multistage dynamic countercurrent abstraction technique of adopting at present.But this technology solvent selection scope in the time of concrete application is little, two-phase has axial mixing in extraction process, and solvent entrainment loss phenomenon is serious, and in product, organic solvent is easily residual, and production cost is also higher.
Chromatography is divided into adsorption chromatography, partition chromatography, ion-exchange chromatography, gel chromatography etc. according to principle difference.Adsorption chromatography is sorbent used silica gel, activated alumina, macroreticular resin etc.Each separated material can vary in size to realize by the absorption affinity producing with adsorbent and separate; Partition chromatography is mainly by the hydrophobic grouping that the is bonded to silicon particle surface phase that fixes, and each separated material is because of different separation of distribution coefficient between mobile phase and fixing phase (hydrophobic grouping layer); Ion-exchange chromatography utilizes anion and cation exchange resin, and the principle of inhaling mutually by the charges of different polarity can be by the material with positive and negative different electric charges separately; Gel chromatography adopts organic or inorganic gel, utilizes the resistance difference of separated material in gel to reach separation object.The effect of chromatographic technique separation and purification natural materials is better, and gained material purity is higher.But adsorption chromatography, partition chromatography technical point use a large amount of organic solvents from purifying natural material demand, not only need to reclaim organic solvent, and easy residual organic solvent in product.Ion-exchange chromatography needs regenerating resin, technological process more complicated, and the preparation amount of gel chromatography is less, produces cost higher, and separating effect is not as good as absorption and partition chromatography.
The precipitating reagent that the precipitation method are different according to the chemical property different choice of separated material, but the purity of products obtained therefrom is all lower, and also precipitating reagent easily enters the product after separation.
Ultrafiltration and membrane extraction all belong to membrane separation technique.Ultrafiltration is to filter the vary in size technology of material of mode isolated molecule amount, for purifying Chinese medicine extract have that precision is high, the feature such as good impurity removing effect, cost are low, environmental protection.But due to the extract complicated component of plant, the pollution problem of film makes the application of this technology once limited, and along with the development of masking technique, membrane pollution problem is resolved gradually in recent years, and ultrafiltration is progressively promoted in the application in this field.
Membrane extraction technology claims again fixing membrane interface abstraction technique.With solid film bond breaker liquid phase and solvent phase, carry out mass transfer by the micropore on film, be full of micropore with the liquid of the better phase of film wetability and arrive the opposite side of film, two-phase liquid is at film Surface Contact generation mass transfer.As new isolation technics, membrane extraction has following advantage: 1) dispersion and the agglomeration process of phase when thering is no traditional liquid-liquid extraction, can avoid extractant with droplet form carrying secretly in feed liquid, reduce extractant loss.2) feed liquid phase and each comfortable film two side flow of solvent phase when membrane extraction, form direct liquid-liquid diphase unlike traditional counter-current extraction and flow, and therefore in the time of slective extraction agent, require wider to physical property such as density, viscosity, interfacial tensions.3) in Membrane Extraction, two-phase is done respectively single-phase flowing in film both sides, makes process avoid " back-mixing " impact and " liquid flooding " condition restriction, can significantly improve extraction efficiency.4) can realize extraction back extraction process at the same level, improve the mass-transfer efficiency of process, simplify the operation.5) feed liquid phase and solvent phase exist in film both sides simultaneously, can avoid the loss of film internal solvent in membrane micropore.This technology is mainly used in Industrial Wastewater Treatment at present, reclaims the metal such as the organic compound such as phenols, phenyl amines and Cd, Zn in waste water.
The independent use of above-mentioned these methods all cannot realize high efficiency, the low-cost separation purifying of natural materials.
Summary of the invention
The object of this invention is to provide a kind of coupling ultrafiltration and the membrane extraction technical point system from purifying natural material, natural materials that can efficiently accurately separation and purification is extracted from plant.
Another object of the present invention is to provide a kind of method of utilizing said system separation and purification natural materials.
For achieving the above object, the technical solution adopted in the present invention is: the system of a kind of ultrafiltration and a few class natural materials of membrane extraction coupling technique purifying, comprise hyperfiltration membrane assembly and extraction reextraction membrane module at the same level,
Extraction reextraction membrane module at the same level comprises peer's extraction reextraction membrane module shell of vertical setting, and the upper and lower of extraction reextraction membrane module side wall of outer shell at the same level is respectively equipped with extractant loop exit and extractant loop head; In extraction reextraction membrane module shell at the same level, be connected with successively the first pressure stability plate, the first division board, first fluid distribution plate, the second division board, the 3rd division board, the second pressure stability plate, the 4th division board and second fluid distribution plate from top to bottom; In extraction reextraction membrane module shell at the same level, be vertically provided with multiple reextraction films and multiple spe membrane, reextraction film upper end is between the first pressure stability plate and the first division board, and reextraction film lower end is between the 4th division board and second fluid distribution plate; Spe membrane upper end is between the second division board and first fluid distribution plate, and spe membrane lower end is between the 3rd division board and the second pressure stability plate; Extraction reextraction membrane module cover top portion at the same level is provided with the charging aperture that the space between the first division board and first fluid distribution plate communicates and the anti-stripping agent outlet communicating with the space between the first pressure stability plate and extraction reextraction membrane module sheath top plate at the same level; Extraction reextraction membrane module shell bottom plate at the same level is provided with the raffinate outlet that the space between the second pressure stability plate and the 4th division board communicates and the reextraction colvent inlet communicating with the space between second fluid distribution plate and extraction reextraction membrane module shell bottom plate at the same level;
Charging aperture is connected with ultrafiltrate and raffinate storage tank by the second compression pump, and ultrafiltrate and raffinate storage tank are connected with surge tank with pipeline after the film of hyperfiltration membrane assembly respectively, and surge tank is also connected with raffinate outlet; Anti-stripping agent outlet is connected with anti-stripping agent storage tank, and extractant loop exit is connected with extractant storage tank, and extractant storage tank is connected with extractant loop head by the 4th compression pump; Reextraction colvent inlet is connected with strippant storage tank by the 3rd compression pump.
Another technical scheme of the present invention is: a kind of method of utilizing a few class natural materials of said system purifying, specifically carry out according to the following steps:
Step 1: extract vegetable drug by conventional method, obtain aqueous extract;
Step 2: by aqueous extract ultrafiltration in hyperfiltration membrane assembly, ultrafiltration sees through liquid and sends into ultrafiltrate and raffinate storage tank;
Or by aqueous extract ultrafiltration in hyperfiltration membrane assembly, it is D1.1～1.25 that ultrafiltration is concentrated into relative density through liquid, sends into ultrafiltrate and raffinate storage tank;
Step 3: if there is the different target substance of multiple Acidity of Aikalinity to need separating and extracting in aqueous extract, send into the liquid of ultrafiltrate and raffinate storage tank by following two kinds of mode processing:
First kind of way: according to the suitable pH value of target substance of extracting, regulate the pH value of ultrafiltrate and raffinate storage pot liquid, then send into the space between the first division board and first fluid distribution plate through charging aperture, and enter equably the space between first fluid distribution plate and the second division board by the micropore in first fluid distribution plate, then flow into spe membrane, regulate the liquid after pH value in conveying ultrafiltrate and raffinate storage tank in, extractant in extractant storage tank is sent into extraction reextraction membrane module at the same level through extractant loop head, at extractant from lower to upper in flow process, enter in the liquid after the adjusting pH value of spe membrane and need the target substance separating to enter extractant by spe membrane mass transfer, in liquid after feed adjustment pH value, also the strippant in strippant storage tank is sent into extraction reextraction membrane module at the same level through reextraction colvent inlet, strippant enters the space between second fluid distribution plate and the 4th division board by the micropore in second fluid distribution plate, and enter reextraction film from lower end, strippant flows from the bottom up in reextraction film, the isolation of target substances that needs entering in extractant enters strippant by reextraction membrane mass transfer, the strippant of the full film journey of flowing through flows out into the space between the first pressure stability plate and the first division board from reextraction film upper end, enter the space between the first pressure stability plate and extraction reextraction membrane module sheath top plate at the same level by the micropore in the first pressure stability plate again, then export and flow into anti-stripping agent storage tank by anti-stripping agent,
Regulate the raffinate that the liquid after pH value is flowed through after full film journey in spe membrane to flow into the space between the 3rd division board and the second pressure stability plate from spe membrane lower end, and enter the space between the second pressure stability plate and the 4th division board by the micropore in the second pressure stability plate, flow into surge tank through raffinate outlet; The extractant of full shell side of flowing through flows into extractant storage tank through extractant loop exit;
After the liquid in ultrafiltrate and raffinate storage tank is used up, then the raffinate in surge tank is sent into ultrafiltrate and raffinate storage tank, then this raffinate is carried out to separating and extracting for the second time, repeat extraction reextraction until target substance extraction is complete;
Raffinate after front a kind of target substance extraction is completely sent into ultrafiltrate and raffinate storage tank, regulate the pH value of this raffinate mutually suitable with the pH value of the second target material that needs to separate, then repeat to extract reextraction separation process, extraction needs the target substance separating, until this target substance extraction completely; Repeat this measure, by the materials different multiple acidity in extract extract and separate respectively;
After each target substance extraction completely, all adopt existing method to reclaim the strippant in the anti-stripping agent in anti-stripping agent storage tank, obtain the target natural materials of this extract and separate;
The second way: according to the suitable pH value of target substance of extracting, regulate the pH value of ultrafiltrate and raffinate storage pot liquid; Then send into the space between the first division board and first fluid distribution plate through charging aperture, enter equably the space between first fluid distribution plate and the second division board by first fluid distribution plate, and enter spe membrane; Regulate the liquid after pH value in conveying ultrafiltrate and raffinate storage tank in, extractant in extractant storage tank is sent into extraction reextraction membrane module at the same level through extractant loop head, when extractant is flowed through the full shell side of reextraction membrane module from lower to upper, enter and in the liquid after the adjusting pH value of spe membrane, need the target substance separating to enter extractant by spe membrane mass transfer, the extractant that comprises target substance flows into extractant storage tank through extractant loop exit; Continue the liquid that regulates pH value in ultrafiltrate and raffinate storage tank to send into extraction reextraction membrane module at the same level, after the liquid in ultrafiltrate and raffinate storage tank is used up, again the raffinate in surge tank is sent into ultrafiltrate and raffinate storage tank, again this raffinate is carried out to separating and extracting for the second time, repeat extraction and strip until regulate the target substance extraction in the liquid after pH value complete; Raffinate after front a kind of target substance extraction is completely sent into ultrafiltrate and raffinate storage tank, regulate the pH value of this raffinate mutually suitable with the pH value of the second target substance that needs to separate, then repeat extraction separation process, extraction needs the target substance separating, until this second target substance extraction completely; Repeat this measure, by the materials different multiple Acidity of Aikalinity in aqueous extract extract and separate respectively;
After each target substance extraction completely, all adopt the solvent of extract in existing method recovery extractant storage tank, can obtain the target natural materials of this extract and separate.
If the Acidity of Aikalinity indifference of target substance in aqueous extract, the liquid after ultrafiltration is sent in ultrafiltrate and raffinate storage tank (3) after by described first kind of way or described second way extract and separate, just in the time processing this liquid without the pH value that regulates this liquid, after extract and separate is complete, obtain water extraction and get the mixture of certain the class target substance comprising in ultrafiltration.
Isolation and purification method tool of the present invention has the following advantages:
1) the preliminary processes coupling of isolation and purification method of the present invention using ultrafiltration as membrane extraction used, and makes membrane extraction become possibility for the separation and purification of natural materials.By the plant extraction liquid that needs membrane extraction in advance ultrafiltration can effectively remove and stop up the suspension of spe membrane micropore and by the soluble large molecule material (amylose, small molecular protein, pectin, polysaccharide etc.) of adsorption fouling spe membrane.Remove macromolecular substances and can make the reduced viscosity of feed liquid, the resistance to mass tranfer while being conducive to reduce membrane extraction, also can obtain the feed liquid that target component concentration is higher by concentrated its appropriateness when as enough low in ultrafiltrate viscosity, to improve mass transfer rate.Two kinds of technology couplings of ultrafiltration and membrane extraction are used, can bring into play the advantage of membrane extraction separation and purification material, can alleviate again spe membrane and pollute, improve membrane extraction efficiency, extend film cleaning frequency and life-span, make membrane extraction technology produce practical value at natural materials separation field.
2) in the time containing surface reactive material (as saponin(e, phospholipid etc.) in plant extraction liquid, traditional liquid-liquid extraction technology can decline because emulsion causes a large amount of extractant entrainment loss and separating effect, when emulsion is serious, due to layering difficulty, can make this technology lose use value.Isolation and purification method of the present invention is owing in use there is no dispersion and the agglomeration process of phase, therefore can separate smoothly containing the target substance in the extract of surface reactive material, can be used for the separation and purification of the extract containing surfactant that liquid-liquid extraction technology cannot be suitable for.
3) because membrane extraction technology requires wider to the physical property of extractant, make isolation and purification method of the present invention have more extractant available than liquid-liquid extraction technology, extractant circulates at shell side in addition, it is convenient to change, and therefore can be realized accurately and being separated by replacing extractant according to the dissolubility of separated material is different; In addition to thering is the material of Acidity of Aikalinity, as alkaloid, flavones etc., also can change by gradient the pH value of ultrafiltrate, anti-stripping agent, the material with Acidity of Aikalinity is accurately separated according to the strong and weak difference of Acidity of Aikalinity.
4) in the time adopting single stage membrane extraction scheme, extraction process is not subject to " back-mixing " impact and " liquid flooding " condition restriction, and extraction efficiency is high, and in reclaiming extract, organic extraction solvent can obtain target substance.
5) in the time adopting extraction reextraction scheme at the same level, because the separated material that enters extractant through extraction has entered anti-stripping agent by reextraction simultaneously, therefore separated material can not reach capacity in extractant, in addition extractant between the shell side of membrane module and receiver in sealing recurrent state, loss amount is few, can effectively reduce Solvent quantity.In separation and purification process, if water is as strippant, finally can obtain product by reclaiming aqueous solution of back extraction, extract obtained middle organic solvent-free is residual.
6), in the time adopting extraction reextraction scheme at the same level of the present invention, when organic extractant uses, in sealing state, not only consumption is few but also carry secretly few.Whole process is not substantially to environmental emission organic solvent gas, and production security is high, environmentally safe.
7) separation and purification system of the present invention adopts hollow fiber film assembly to carry out membrane extraction, the mass transfer area of unit volume is large, adopted extraction reextraction technology at the same level simultaneously, membrane extraction efficiency is high, the space that therefore whole system take up space takies much smaller than liquid liquid counter-current extraction, column chromatography extraction column used and chromatographic column; And can obtain separated material from extracting ultrafiltrate one step, and the technique of adsorbing-washing chromatographic column-eluant, eluent wash-out-processing chromatographic column than the upper prop of chromatographic technique is simple, and process cycle is short, and cost is far below common process.
Brief description of the drawings
Fig. 1 is the structural representation of separation and purification system of the present invention.
Fig. 2 is the structural representation of membrane module of stripping in separation and purification system of the present invention.
In figure: 1. the first compression pump, 2. hyperfiltration membrane assembly, 3. ultrafiltrate and raffinate storage tank, 4. the second compression pump, 5. extraction reextraction membrane module at the same level, 6. the 3rd compression pump, 7. strippant storage tank, 8. extractant storage tank, 9. the 4th compression pump, 10. anti-stripping agent storage tank, 11. surge tanks, 12. extraction reextraction membrane module shells at the same level, 13. first pressure stability plates, 14. first division boards, 15. first fluid distribution plates, 16. second division boards, 17. extractant loop exits, 18. reextraction films, 19. spe membranes, 20. the 3rd division boards, 21. second pressure stability plates, 22. the 4th division boards, 23. second fluid distribution plates, 24. reextraction colvent inlets, 25. raffinate outlets, 26. extractant loop heads, 27. anti-stripping agent outlets, 28. charging apertures.
Detailed description of the invention
Below in conjunction with the drawings and specific embodiments, the present invention is described in detail.
As shown in Figure 1, separation and purification system of the present invention comprises ultrafiltration part and membrane extraction part, and ultrafiltration part comprises the first compression pump 1, hyperfiltration membrane assembly 2, ultrafiltrate and raffinate storage tank 3 and surge tank 11; Membrane extraction part comprises the second compression pump 4, extraction reextraction membrane module 5 at the same level, the 3rd compression pump 6, strippant storage tank 7, extractant storage tank 8, the 4th compression pump 9 and anti-stripping agent storage tank 10.
Wherein the structure of extraction reextraction membrane module 5 at the same level as shown in Figure 2, comprise peer's extraction reextraction membrane module shell 12 of the hollow of vertical setting, the side wall upper part of extraction reextraction membrane module shell 12 at the same level is provided with extractant loop exit 17, and extraction reextraction membrane module shell at the same level 12 lower sidewall are provided with extractant loop head 26; Extraction reextraction membrane module shell 12 at the same level is interior, the axis direction of edge extraction at the same level reextraction membrane module shell 12 is connected with the first pressure stability plate 13, the first division board 14, first fluid distribution plate 15, the second division board 16, the 3rd division board 20, the second pressure stability plate 21, the 4th division board 22 and second fluid distribution plate 23 from top to bottom successively; The position of the second division board 16 is higher than the position of extractant loop exit 17, and the position of the 3rd division board 20 is lower than the position of extractant loop head 26; In extraction reextraction membrane module shell 12 at the same level, be provided with the reextraction film 18 of hollow fiber that extraction reextraction membrane module shell multiple and at the same level 12 axis parallel or tubulose and multiple and peer and extract hollow fiber that reextraction membrane module shell 12 axis parallel or the spe membrane 19 of tubulose, the length of reextraction film 18 is greater than the length of spe membrane 19; The upper end of reextraction film 18 is between the first pressure stability plate 13 and the first division board 14, and the lower end of reextraction film 18 is between the 4th division board 22 and second fluid distribution plate 23; The upper end of spe membrane 19 is between the second division board 16 and first fluid distribution plate 15, and the lower end of spe membrane 19 is between the 3rd division board 20 and the second pressure stability plate 21; Extraction at the same level reextraction membrane module shell 12 tops are provided with charging aperture 28 and anti-stripping agent outlet 27, and charging aperture 28 communicates with the space between the first division board 14 and first fluid distribution plate 15; Anti-stripping agent outlet 27 communicates with the space between the first pressure stability plate 13 and extraction reextraction membrane module shell at the same level 12 top boards; Extraction reextraction membrane module shell at the same level 12 base plates are provided with raffinate outlet 25 and reextraction colvent inlet 24, and raffinate outlet 25 communicates with the space between the second pressure stability plate 21 and the 4th division board 22; Reextraction colvent inlet 24 communicates with the space between second fluid distribution plate 23 and extraction reextraction membrane module shell at the same level 12 base plates.
Formed for ultrafiltration feed liquid or the mobile feed liquid space of raffinate by charging aperture 28, the first division board 14, the second division board 16, spe membrane 19, the 3rd division board 20, the 4th division board 22 and raffinate outlet 25, the first fluid distribution plate 15 that is positioned at this feed liquid space is made up of the flaky material with micropore, by making ultrafiltrate or raffinate flow velocity, pressure everywhere after distribution plate consistent to the ultrafiltration feed liquid of being carried by pump or the certain resistance of raffinate, prevent that channeling from occurring; The second pressure stability plate 21 is also made up of porous media, by extracting the stable of part microporous barrier pipe (silk) internal pressure to maintain to the certain resistance of raffinate that the microporous barrier pipe (silk) of flowing through has extracted.
The top board of reextraction colvent inlet 24, the 4th division board 22, reextraction film 18, the first division board 13, extraction reextraction membrane module shell 12 at the same level, base plate and the anti-stripping agent outlet 27 of extraction reextraction membrane module shell 12 at the same level form for the mobile separate space of anti-stripping agent, identical with in feed liquid space of material, structure and the effect of the fluid distributing board in this separate space and pressure stability plate.
Form by extractant loop head 26, extraction reextraction membrane module shell 12 at the same level, extractant loop exit 17 space circulating for extractant.
Mass exchange (mass transfer) between each space can only be undertaken by the micropore on spe membrane, reextraction film.
Charging aperture 28 is also connected with the second compression pump 4, the second compression pump 4 is connected with ultrafiltrate and raffinate storage tank 3, ultrafiltrate and raffinate storage tank 3 are connected with surge tank 11 with pipeline after the film of hyperfiltration membrane assembly 2 respectively, the film preceding pipeline of hyperfiltration membrane assembly 2 is connected with the first compression pump 1, and surge tank 11 is also connected with raffinate outlet 25; Anti-stripping agent outlet 27 is connected with anti-stripping agent storage tank 10, and extractant loop exit 17 is connected with extractant storage tank 8, and extractant storage tank 8 is connected with extractant loop head 26 by the 4th compression pump 9; Reextraction colvent inlet 24 is connected with strippant storage tank 7 by the 3rd compression pump 6.
The first pressure stability plate 13 and the second pressure stability plate 21 are made up of the flaky material with micropore, and increasing film tube fluid resistance by appropriateness, to maintain film overpressure stable.
First fluid distribution plate 15 and second fluid distribution plate 23 are made up of the flaky material with micropore, make liquid that the second compression pump 4 and the 3rd compression pump 6 the carry corresponding space internal pressure distributing equilibrium at membrane module by increasing fluid resistance, prevent that difference from appearring in different film liquid in pipe flow velocitys.
The spe membrane of hollow fiber type and reextraction film are microporous barrier, and material can be organic substance, can be also inorganic matters, pore diameter range 0.05～10 μ m.
Hyperfiltration membrane assembly 2 is doughnut formula, volume membrane type or tubular type, and the material of milipore filter can be organic film, can be also inoranic membrane.
The present invention also provides a kind of method of utilizing above-mentioned separation and purification system separation and purification natural materials, specifically carries out according to the following steps:
Step 1: adopt conventional method to extract vegetable drug, obtain the aqueous extract containing multiple natural materials;
Step 2: the aqueous extract in step 1 is sent into hyperfiltration membrane assembly 2 by the first compression pump 1 and carry out ultrafiltration, using molecular cut off in ultra-filtration process is the Inorganic Ultrafiltration Membrane of 2000～500000 daltonian organic milipore filters or aperture 2～200nm; Ultrafiltration sees through liquid and sends in ultrafiltrate and raffinate storage tank 3, for subsequent use;
Or, the aqueous extract in step 1 to be sent into hyperfiltration membrane assembly 2 by the first compression pump 1 and carry out ultrafiltration, in ultra-filtration process, using molecular cut off is 2000～500000 daltonian organic milipore filters, or the Inorganic Ultrafiltration Membrane of aperture 2～200nm; After ultrafiltration sees through liquid and is concentrated into relative density and is D1.1～1.25, then send in ultrafiltrate and raffinate storage tank 3, for subsequent use;
Extractant is sent in extractant storage tank 8;
Strippant is sent in strippant storage tank 7;
Step 3: if while having the different target substance of multiple Acidity of Aikalinity to need separating and extracting in aqueous extract, process the liquid in ultrafiltrate and raffinate storage tank 3 by following two kinds of modes:
First kind of way: the suitable pH value of a kind of target substance of extracting as required, the pH value of adjusting ultrafiltrate and raffinate storage tank 3 interior liquid, by the second compression pump 4, the liquid after ultrafiltrate and the interior adjusting of raffinate storage tank 3 pH value is sent into charging aperture 28, enter in extraction reextraction membrane module 5 at the same level in space between the first division board 14 and first fluid distribution plate 15 through charging aperture 28, and enter equably in the space between first fluid distribution plate 15 and the second division board 16 by the micropore in first fluid distribution plate 15, and be gathered on the second division board 16, in the time of the end face of liquid level one end between first fluid distribution plate 15 and the second division board 16 higher than spe membrane 19 of the liquid of assembling on the second division board 16, liquid enters spe membrane 19, in liquid after feed adjustment pH value, by the 4th compression pump 9, the extractant in extractant storage tank 8 is sent into extraction reextraction membrane module 5 at the same level through extractant loop head 26, extractant is flowed through from lower to upper after peer extracts reextraction membrane module 5 full shell sides and is flowed out through the extractant loop exit 17 of peer's extraction reextraction membrane module 5, and flow back to extractant storage tank 8, form circulating of extractant, circulating in process of extractant, enter and in the liquid after the adjusting pH value of spe membrane 19, need the target substance extracting to enter extractant by the fenestra mass transfer on spe membrane 19, in liquid after feed adjustment pH value, with the 3rd compression pump 6, the strippant in strippant storage tank 7 is sent into extraction reextraction membrane module 5 at the same level through reextraction colvent inlet 24, strippant enters in the space between second fluid distribution plate 23 and the 4th division board 22 by the micropore in second fluid distribution plate 23, and enter reextraction film 18 from reextraction film 18 lower ends, strippant flows from the bottom up in reextraction film 18, in flow process, the target substance that need to extract entering in extractant enters strippant by the micropore mass transfer of reextraction film 18, strippant is flowed through and is formed the anti-stripping agent that includes target substance after full film journey, this anti-stripping agent flows out in the space between the first pressure stability plate 13 and the first division board 14 from reextraction film 18 upper ends, enter in the space between the first pressure stability plate 13 and extraction reextraction membrane module shell at the same level 12 top boards by the micropore in the first pressure stability plate 13 again, then exporting 27 by anti-stripping agent flows in anti-stripping agent storage tank 10,
Regulate the liquid after pH value in spe membrane 19, to flow through after full film journey, become raffinate, this raffinate flows out from spe membrane 19 lower ends, enter in the space between the 3rd division board 20 and the second pressure stability plate 21, and enter in the space between the second pressure stability plate 21 and the 4th division board 22 by the micropore in the second pressure stability plate 21, send into surge tank 11 through raffinate outlet 25;
After the liquid in ultrafiltrate and raffinate storage tank 3 is used up, again the raffinate in surge tank 11 is sent into ultrafiltrate and raffinate storage tank 3, by the second compression pump 4, the raffinate in ultrafiltrate and raffinate storage tank 3 is sent into extraction reextraction membrane module 5 at the same level and carry out separating and extracting for the second time, repeat extraction reextraction until target substance extracts completely; Then adopt existing method to reclaim the strippant in the anti-stripping agent in anti-stripping agent storage tank 10, obtain the target substance of this extract and separate;
Raffinate after front a kind of target substance extraction is completely sent in ultrafiltrate and raffinate storage tank 3, regulate the pH value of this raffinate mutually suitable with the pH value of the second target material that need to extract, then repeat to extract reextraction separation process, extraction needs the target substance separating, until this target substance extraction completely; Repeat this measure, by the materials different multiple acidity in extract extract and separate respectively; After each target substance extraction completely, all adopt existing method to reclaim the strippant in the anti-stripping agent in anti-stripping agent storage tank 10, obtain the target natural materials of this extract and separate;
First kind of way is membrane extraction reextraction process at the same level.
The second way: the pH value suitable according to a kind of target substance that will extract, the pH value of adjusting ultrafiltrate and raffinate storage tank 3 interior liquid, then by the second compression pump 4, the liquid after ultrafiltrate and the interior adjusting of raffinate storage tank 3 pH value is sent into charging aperture 28, enter in extraction reextraction membrane module 5 at the same level in space between the first division board 14 and first fluid distribution plate 15 through charging aperture 28, and enter equably in the space between first fluid distribution plate 15 and the second division board 16 by the micropore in first fluid distribution plate 15, and be gathered on the second division board 16, in the time of the end face of liquid level one end between first fluid distribution plate 15 and the second division board 16 higher than spe membrane 19 of the liquid of assembling on the second division board 16, liquid enters spe membrane 19, in liquid after feed adjustment pH value, by the 4th compression pump 9, the extractant in extractant storage tank 8 is sent into extraction reextraction membrane module 5 at the same level through extractant loop head 26, extractant is flowed through from lower to upper and is flowed out through the extractant loop exit 17 of peer's extraction reextraction membrane module 5 after the full shell side of reextraction membrane module 5, and flow back to extractant storage tank 8, form circulating of extractant, circulating in process of extractant, enter and in the liquid after the adjusting pH value of spe membrane 19, need the target substance extracting to enter extractant by the fenestra mass transfer on spe membrane 19, carry the extractant of target substance and flow through from the bottom up after full film journey, flow out from extractant loop exit 17, and flow back to extractant storage tank 8, continue the liquid of ultrafiltrate and the interior adjusting of raffinate storage tank 3 pH value to send into extraction reextraction membrane module 5 at the same level, until flowing through extraction reextraction membrane module 5 at the same level completely, this liquid enters surge tank 11, raffinate is sent in ultrafiltrate and raffinate storage tank 3 and extracted for the second time again, repeat this process until regulate the target substance extraction in the liquid after pH value complete, raffinate after front a kind of target substance extraction is completely sent in ultrafiltrate and raffinate storage tank 3, regulate the pH value of this raffinate mutually suitable with the pH value of the second target substance that need to extract, then repeat extraction separation process, extraction needs the target substance separating, until this target substance extraction completely, repeat this measure, by the materials different multiple Acidity of Aikalinity in ultrafiltrate extract and separate respectively, after each target substance extraction completely, all adopt the solvent of extract in existing method recovery extractant storage tank 8, can obtain the target natural materials of this extract and separate.
The second way is Membrane Extraction.
If the Acidity of Aikalinity indifference of target substance in aqueous extract, can process the liquid in ultrafiltrate and raffinate storage tank 3 by above-mentioned first kind of way or the second way respectively, be the pH value without this liquid of adjusting in the time of the liquid of processing in ultrafiltrate and raffinate storage tank 3, the mixture of certain class target substance that can obtain comprising in water extraction ultrafiltrate after extract and separate is complete.
Extractant is a kind of organic solvent of not mixing mutually with water or the mixture of several organic solvents.In extraction separation process, the linear rate of flow of several liquid ratio is: ultrafiltration sees through liquid or Cui Yu Ye ︰ Cui Qu Ji ︰ strippant=1 ︰ 0.2～6 ︰ 0.2～1.
embodiment 1
Get root of kudzu vine 50kg, add water 12 times and measure refluxing extraction, extract 1.5 hours at every turn, extract 2 times, merge to obtain extract 1100kg; Extract is filtered with the daltonian external compression type hollow fiber ultrafiltration membrane of molecule interception 500000, collect ultrafiltration and see through the about 1000kg of liquid; With ethyl acetate be extractant, weak aqua ammonia is anti-stripping agent, ultrafiltration is seen through to liquid and complete extraction reextraction process at the same level, 25 DEG C of membrane extraction temperature by the step 3 in the inventive method.The flowing velocity that ultrafiltration sees through liquid, extractant, strippant is respectively 0.1m/s, 0.3 m/s, 0.06m/s, and ultrafiltration sees through liquid through 4 membrane extractions.Collect anti-stripping agent, volume is that ultrafiltration sees through 2 times of liquid, about 2000kg; Anti-stripping agent is concentrated into 600kg with the daltonian NF membrane nanofiltration of molecule interception 150, discards through liquid, trapped fluid is evaporated to after relative density 1.30, vacuum drying, obtains Pueraria Flavonid, content 88.2%.
embodiment 2
Extracting liquorice 50kg, adds 12 times of amount refluxing extraction of the 0.2% NaOH aqueous solution, extracts 2 hours at every turn, extracts 2 times, merges to obtain extract 1100kg; Ceramic membrane ultrafitration by extract with aperture 10nm, collects ultrafiltration and sees through the about 1000kg of liquid; Ultrafiltration is seen through to liquid watery hydrochloric acid adjust pH to 4, with ethyl acetate be extractant, weak aqua ammonia is strippant, ultrafiltration is seen through to liquid and carry out peer by the step 3 in the inventive method and extract reextraction process, 25 DEG C of membrane extraction temperature; The flowing velocity that ultrafiltration sees through liquid, extractant, anti-stripping agent is respectively 0.1m/s, 0.3m/s, 0.1m/s, and ultrafiltration sees through liquid through 4 membrane extractions; Collect anti-stripping agent, volume is that ultrafiltration sees through 4 times of liquid, about 4000kg; Anti-stripping agent is concentrated into 500kg with the daltonian NF membrane nanofiltration of molecule interception 200, discards through liquid, by trapped fluid adjust pH to 3.5, be evaporated to after relative density 1.30, vacuum drying, obtains glycyrrhiza total flavonoid, content 88.2%; Watery hydrochloric acid for raffinate is adjusted to pH to 2.5, with ethyl acetate be extractant, weak aqua ammonia is anti-stripping agent, carries out peer extract reextraction, 30 DEG C of membrane extraction temperature by the step 3 in the inventive method.The flowing velocity of raffinate, extractant, strippant is respectively 0.1m/s, 0.3m/s, 0.06m/s, obtains the about 2400kg of anti-stripping agent through 4 membrane extractions; Anti-stripping agent is concentrated into 500kg with the daltonian NF membrane nanofiltration of molecule interception 200, discards through liquid.Trapped fluid is reduced to after relative density 1.30, and vacuum drying, obtains ammonium glycyrrhizunate, content 98%.
embodiment 3
Get kuh-seng 50kg, add 12 times of amount refluxing extraction of 0.2% aqueous hydrochloric acid solution, extract 2 times, each 1 hour, merge to obtain extract 1100kg; Ceramic membrane ultrafitration by aqueous extract with aperture 100nm, collects ultrafiltration and sees through the about 1100kg of liquid; Ultrafiltration is seen through to liquid NaOH solution and adjust pH to 8.0, the mixed liquor (volume ratio 1:1) of ethyl acetate and ether is extractant, 1% hydrochloric acid is strippant, ultrafiltration is seen through to liquid and complete extraction reextraction process at the same level, 25 DEG C of membrane extraction temperature by the step 3 in the inventive method.The flowing velocity that ultrafiltration sees through liquid, extractant, strippant is respectively 0.1m/s, 0.6m/s, 0.1m/s, and ultrafiltration sees through liquid through 4 membrane extractions; Collect anti-stripping agent, volume is that ultrafiltration sees through 4 times of liquid, about 4000kg; Anti-stripping agent is concentrated into 600kg with the daltonian NF membrane nanofiltration of molecule interception 200, discards through liquid, trapped fluid is evaporated to after relative density 1.30, vacuum drying, obtains Banlangen, content 83.2%.
embodiment 4
Get giant knotweed 50kg, add 14 times of amount 2%NaOH aqueous solution refluxing extraction, extract 1 hour at every turn, extract 2 times, merge to obtain extract 1300kg; Ceramic composite membrane ultrafiltration by aqueous extract with aperture 20nm, collects ultrafiltration and sees through the about 1200kg of liquid; Ultrafiltration is seen through to liquid 20% hydrochloric acid solution and adjust pH to 2.0, using the mixed liquor (2:1) of ethyl acetate and ether is extractant, uses 5%NaHCO
3for anti-stripping agent, ultrafiltration is seen through to liquid and complete extraction reextraction process at the same level by the step 3 in the inventive method, collect NaHCO
3the aqueous solution is anti-stripping agent.Again with 5%Na
2cO
3the aqueous solution is anti-stripping agent, and raffinate is carried out to peer's extraction reextraction process again by step 3 of the present invention, collects Na
2cO
3anti-stripping agent.Again taking the 2%NaOH aqueous solution as anti-stripping agent, by Na
2cO
3raffinate carries out peer's extraction reextraction process again by step 3 of the present invention, collects NaOH anti-stripping agent.Membrane extraction temperature is always 25 DEG C, and the flowing velocity that ultrafiltration sees through liquid (raffinate), extractant, anti-stripping agent is respectively 0.1,0.6,0.02m/s, and ultrafiltration sees through liquid through 4 membrane extractions.Each anti-stripping agent volume be ultrafiltration see through liquid (raffinate) 1/4, about 250kg.Each anti-stripping agent is evaporated to 50kg.Again by 5%NaHCO
3anti-stripping agent regulates PH to 2.0 with hydrochloric acid, and filtration is precipitated, and precipitation is washed with water to neutrality, dry, obtains Rhein, purity 87%.By 5%Na
2cO
3anti-stripping agent regulates PH to 2.0 with hydrochloric acid, and filtration is precipitated, and precipitation is washed with water to neutrality, dry, obtains archen, purity 75%.2%NaOH anti-stripping agent is regulated to PH to 2.0 with hydrochloric acid, and filtration is precipitated, and precipitation is washed with water to neutrality, dry, obtains Chrysophanol and Physcion mixture.
embodiment 5
Get radix bupleuri 50kg, add 10 times of water gaging refluxing extraction, extract 1 hour at every turn, extract 2 times, merge to obtain aqueous extract 900kg.Ceramic composite membrane ultrafiltration by aqueous extract with aperture 200nm, collects ultrafiltration and sees through the about 850kg of liquid.With n-butanol be extractant, water is anti-stripping agent, ultrafiltration is seen through to liquid and complete extraction reextraction process at the same level by step 3 of the present invention, collects anti-stripping agent.Membrane extraction temperature is 60 DEG C, and the flowing velocity that ultrafiltration sees through liquid, extractant, anti-stripping agent is respectively 0.1,0.6,0.06m/s, and ultrafiltration sees through liquid through 4 membrane extractions.Obtain the about 2050kg of anti-stripping agent.Each anti-stripping agent is concentrated into 400kg with the daltonian NF membrane nanofiltration of molecule interception 1050, discards through liquid, trapped fluid is evaporated to after relative density 1.30, vacuum drying, obtains thick bupleurum total saponin, content 78.4%.By thick bupleurum total saponin ether cold soaking, obtain bupleurum total saponin (ether insoluble matter), content 82.7%.
embodiment 6
Get pseudo-ginseng 20kg, pulverizing is 20 order particles, by 4 times of water gagings, pectase 3g, cellulase 5g, mixes, and is heated to 50 DEG C, enzymolysis 2 hours, then add 6 times of water gagings, refluxing extraction, extracts 1.5 hours, collects extract.The dregs of a decoction add 10 times of water gagings again, and refluxing extraction is extracted 1.5 hours, merges to obtain aqueous extract 360kg.With this aqueous extract of ceramic composite membrane ultrafiltration of aperture 2nm, collect ultrafiltration and see through the about 320kg of liquid.With n-butanol be extractant, water is anti-stripping agent, ultrafiltration is seen through to liquid and complete extraction reextraction process at the same level by step 3 of the present invention, collects anti-stripping agent.Membrane extraction temperature is 55 DEG C, and the flowing velocity that ultrafiltration sees through liquid, extractant, anti-stripping agent is respectively 0.1,0.02,0.06m/s, and ultrafiltration sees through liquid through 4 membrane extractions.Obtain the about 1280kg of anti-stripping agent.Each anti-stripping agent is concentrated into 400kg with the daltonian NF membrane nanofiltration of molecule interception 100, discards through liquid, trapped fluid is evaporated to after relative density 1.1, spraying is dry, obtains arasaponin, content 76%.
embodiment 7
Get tea dust 20kg (40 order), add 10 times of water gagings and extract, extract 0.5 hour at every turn, extract 3 times, control and extract temperature 70 C-80 DEG C, merge to obtain aqueous extract 550kg.With the ceramic composite membrane ultrafiltration aqueous extract of aperture 10nm, collect ultrafiltration and see through the about 500kg of liquid.With ethyl acetate be extractant, water is anti-stripping agent, ultrafiltration is seen through to liquid and complete extraction reextraction process at the same level by the step 3 in the inventive method, collects anti-stripping agent.Membrane extraction temperature is 35 DEG C, and the flowing velocity that ultrafiltration sees through liquid, extractant, anti-stripping agent is respectively 0.1,0.02,0.1m/s, and ultrafiltration sees through liquid through 4 membrane extractions, obtains the about 2000kg of anti-stripping agent; Each anti-stripping agent is concentrated into 300kg with the daltonian NF membrane nanofiltration of molecule interception 150, discards through liquid, be evaporated to D=1.10(25 DEG C), spraying is dry, obtains Tea Polyphenols, with colorimetric method for determining, content 82.4%.
embodiment 8
Get motherwort meal 50kg, add 10 times of amount refluxing extraction of 0.05% aqueous hydrochloric acid solution, extract 1 hour at every turn, extract 3 times, merge to obtain extract 1400kg.Ceramic composite membrane ultrafiltration by aqueous extract with aperture 5nm, collects ultrafiltration and sees through the about 1450kg of liquid.With chloroform be extractant, 0.1% aqueous hydrochloric acid solution water is anti-stripping agent, ultrafiltration is seen through to liquid and complete extraction reextraction process at the same level by step 3 of the present invention, collects anti-stripping agent.Membrane extraction temperature is 30 DEG C, and the flowing velocity that ultrafiltration sees through liquid, extractant, anti-stripping agent is respectively 0.1,0.3,0.02m/s, and ultrafiltration sees through liquid through 4 membrane extractions.Obtain the about 860kg of anti-stripping agent.Each anti-stripping agent is concentrated into 350kg with the daltonian NF membrane nanofiltration of molecule interception 150, discards through liquid, be evaporated to D=1.10(25 DEG C), spraying is dry, obtains motherwort total alkaloid, with colorimetric method for determining, content 62.4%.
embodiment 9
Get epimedium herb 20kg, add 30 times of water gagings, soak 1.5 hours, refluxing extraction is extracted 2 hours at every turn, extracts 2 times, merges to obtain extract 1150kg.By molecule interception 2000 daltonian spiral wound membrane filtrations for aqueous extract, collect ultrafiltration and see through the about 1100kg of liquid.With ethyl acetate be extractant, by ultrafiltration see through liquid complete Membrane Extraction by the step 3 in the inventive method, collect extract.Membrane extraction temperature is 30 DEG C, and the flowing velocity that ultrafiltration sees through liquid, extractant is respectively 0.1,0.02,0.02m/s, and ultrafiltration sees through liquid through 4 membrane extractions.Obtain the about 300kg of extract; Ethyl acetate membrane extraction liquid is reclaimed to solvent, and vacuum drying obtains barren wort total chromocor, with colorimetric method for determining, and content 68.4%.
Claims (7)
1. a system for ultrafiltration and a few class natural materials of membrane extraction coupling technique purifying, is characterized in that, comprises hyperfiltration membrane assembly (2) and extraction reextraction membrane module at the same level (5),
Extraction reextraction membrane module at the same level (5) comprises peer's extraction reextraction membrane module shell (12) of the hollow of vertical setting, and the upper and lower of extraction reextraction membrane module shell (12) sidewall at the same level is respectively equipped with extractant loop exit (17) and extractant loop head (26); In extraction reextraction membrane module shell at the same level (12), be connected with successively the first pressure stability plate (13), the first division board (14), first fluid distribution plate (15), the second division board (16), the 3rd division board (20), the second pressure stability plate (21), the 4th division board (22) and second fluid distribution plate (23) from top to bottom; In extraction reextraction membrane module shell at the same level (12), be vertically provided with multiple reextraction films (18) and multiple spe membrane (19), reextraction film (18) upper end is positioned between the first pressure stability plate (13) and the first division board (14), and reextraction film (18) lower end is positioned between the 4th division board (22) and second fluid distribution plate (23); Spe membrane (19) upper end is positioned between the second division board (16) and first fluid distribution plate (15), and spe membrane (19) lower end is positioned between the 3rd division board (20) and the second pressure stability plate (21); Extraction at the same level reextraction membrane module shell (12) top is provided with the charging aperture (28) that the space between the first division board (14) and first fluid distribution plate (15) communicates and the anti-stripping agent communicating with the first pressure stability plate (13) and the space extracting between reextraction membrane module shell (12) top board at the same level exports (27); Extraction reextraction membrane module shell (12) base plate at the same level is provided with the raffinate outlet (25) that the space between the second pressure stability plate (21) and the 4th division board (22) communicates and extracts with second fluid distribution plate (23) and peer the reextraction colvent inlet (24) that the space between reextraction membrane module shell (12) base plate communicates;
Charging aperture (28) is connected with ultrafiltrate and raffinate storage tank (3) by the second compression pump (4), ultrafiltrate and raffinate storage tank (3) are connected with surge tank (11) with pipeline after the film of hyperfiltration membrane assembly (2) respectively, and surge tank (11) is also connected with raffinate outlet (25); Anti-stripping agent outlet (27) is connected with anti-stripping agent storage tank (10), and extractant loop exit (17) is connected with extractant storage tank (8), and extractant storage tank (8) is connected with extractant loop head (26) by the 4th compression pump (9); Reextraction colvent inlet (24) is connected with strippant storage tank (7) by the 3rd compression pump (6).
2. the system of ultrafiltration according to claim 1 and a few class natural materials of membrane extraction coupling technique purifying, is characterized in that, described reextraction film (18) is hollow fiber or tubulose.
3. the system of ultrafiltration according to claim 1 and a few class natural materials of membrane extraction coupling technique purifying, is characterized in that, described spe membrane (19) is hollow fiber or tubulose.
4. the system of ultrafiltration according to claim 1 and a few class natural materials of membrane extraction coupling technique purifying, it is characterized in that, described the first pressure stability plate (13), first fluid distribution plate (15), the second pressure stability plate (21) and second fluid distribution plate (23) all adopt by the flaky material with micropore to be made.
5. a method of utilizing a few class natural materials of system purifying described in claim 1, is characterized in that, the method is specifically carried out according to the following steps:
Step 1: extract vegetable drug by conventional method, obtain aqueous extract;
Step 2: adopt the system of a few class natural materials of purifying, this system comprises hyperfiltration membrane assembly (2) and extraction reextraction membrane module at the same level (5),
Extraction reextraction membrane module at the same level (5) comprises peer's extraction reextraction membrane module shell (12) of the hollow of vertical setting, and the upper and lower of extraction reextraction membrane module shell (12) sidewall at the same level is respectively equipped with extractant loop exit (17) and extractant loop head (26); In extraction reextraction membrane module shell at the same level (12), be connected with successively the first pressure stability plate (13), the first division board (14), first fluid distribution plate (15), the second division board (16), the 3rd division board (20), the second pressure stability plate (21), the 4th division board (22) and second fluid distribution plate (23) from top to bottom; In extraction reextraction membrane module shell at the same level (12), be vertically provided with multiple reextraction films (18) and multiple spe membrane (19), reextraction film (18) upper end is positioned between the first pressure stability plate (13) and the first division board (14), and reextraction film (18) lower end is positioned between the 4th division board (22) and second fluid distribution plate (23); Spe membrane (19) upper end is positioned between the second division board (16) and first fluid distribution plate (15), and spe membrane (19) lower end is positioned between the 3rd division board (20) and the second pressure stability plate (21); Extraction at the same level reextraction membrane module shell (12) top is provided with the charging aperture (28) that the space between the first division board (14) and first fluid distribution plate (15) communicates and the anti-stripping agent communicating with the first pressure stability plate (13) and the space extracting between reextraction membrane module shell (12) top board at the same level exports (27); Extraction reextraction membrane module shell (12) base plate at the same level is provided with the raffinate outlet (25) that the space between the second pressure stability plate (21) and the 4th division board (22) communicates and extracts with second fluid distribution plate (23) and peer the reextraction colvent inlet (24) that the space between reextraction membrane module shell (12) base plate communicates;
Charging aperture (28) is connected with ultrafiltrate and raffinate storage tank (3) by the second compression pump (4), ultrafiltrate and raffinate storage tank (3) are connected with surge tank (11) with pipeline after the film of hyperfiltration membrane assembly (2) respectively, and surge tank (11) is also connected with raffinate outlet (25); Anti-stripping agent outlet (27) is connected with anti-stripping agent storage tank (10), and extractant loop exit (17) is connected with extractant storage tank (8), and extractant storage tank (8) is connected with extractant loop head (26) by the 4th compression pump (9); Reextraction colvent inlet (24) is connected with strippant storage tank (7) by the 3rd compression pump (6);
By aqueous extract ultrafiltration in hyperfiltration membrane assembly (2), ultrafiltration sees through liquid and sends into ultrafiltrate and raffinate storage tank (3);
Or by aqueous extract ultrafiltration in hyperfiltration membrane assembly (2), it is D1.1～1.25 that ultrafiltration is concentrated into relative density through liquid, sends into ultrafiltrate and raffinate storage tank (3);
Step 3: if there is the different target substance of multiple Acidity of Aikalinity to need separating and extracting in aqueous extract, send into the liquid of ultrafiltrate and raffinate storage tank (3) by following two kinds of mode processing:
First kind of way: according to the suitable pH value of target substance of extracting, regulate the pH value of ultrafiltrate and the interior liquid of raffinate storage tank (3), then send into the space between the first division board (14) and first fluid distribution plate (15) through charging aperture (28), and enter equably the space between first fluid distribution plate (15) and the second division board (16) by the micropore in first fluid distribution plate (15), then flow into spe membrane (19); Regulate the liquid after pH value in conveying ultrafiltrate and raffinate storage tank (3) in, extractant in extractant storage tank (8) is sent into extraction reextraction membrane module at the same level (5) through extractant loop head (26), at extractant from lower to upper in flow process, enter in the liquid after the adjusting pH value of spe membrane (19) and need the target substance separating to enter extractant by spe membrane (19) mass transfer; in liquid after feed adjustment pH value, also the strippant in strippant storage tank (7) is sent into extraction reextraction membrane module at the same level (5) through reextraction colvent inlet (24), strippant enters the space between second fluid distribution plate (23) and the 4th division board (22) by the micropore in second fluid distribution plate (23), and enter reextraction film (18) from lower end, strippant flows from the bottom up in reextraction film (18), the isolation of target substances that needs entering in extractant enters strippant by the film of stripping (18) mass transfer, the strippant of the full film journey of flowing through flows out into the space between the first pressure stability plate (13) and the first division board (14) from reextraction film (18) upper end, enter the space between the first pressure stability plate (13) and extraction reextraction membrane module shell (12) top board at the same level by the micropore in the first pressure stability plate (13) again, then export (27) by anti-stripping agent and flow into anti-stripping agent storage tank (10),
Regulate the raffinate that the liquid after pH value is flowed through after full film journey in spe membrane (19) to flow into the space between the 3rd division board (20) and the second pressure stability plate (21) from spe membrane (19) lower end, and enter the space between the second pressure stability plate (21) and the 4th division board (22) by the micropore in the second pressure stability plate (21), flow into surge tank (11) through raffinate outlet (25); Flow through full shell side extractant through extractant loop exit (17) flow into extractant storage tank (8);
After the liquid in ultrafiltrate and raffinate storage tank (3) is used up, again the raffinate in surge tank (11) is sent into ultrafiltrate and raffinate storage tank (3), again this raffinate is carried out to separating and extracting for the second time, repeat extraction reextraction until target substance extraction is complete;
Raffinate after front a kind of target substance extraction is completely sent into ultrafiltrate and raffinate storage tank (3), regulate the pH value of this raffinate mutually suitable with the pH value of the second target material that needs to separate, then repeat to extract reextraction separation process, extraction needs the target substance separating, until this target substance extraction completely; Repeat this measure, by the materials different multiple acidity in extract extract and separate respectively;
After each target substance extraction completely, all adopt existing method to reclaim the strippant in the anti-stripping agent in anti-stripping agent storage tank (10), obtain the target natural materials of this extract and separate;
The second way: according to the suitable pH value of target substance of extracting, regulate the pH value of ultrafiltrate and the interior liquid of raffinate storage tank (3); Then send into the space between the first division board (14) and first fluid distribution plate (15) through charging aperture (28), enter equably the space between first fluid distribution plate (15) and the second division board (16) by first fluid distribution plate (15), and enter spe membrane (19); Regulate the liquid after pH value in conveying ultrafiltrate and raffinate storage tank (3) in, extractant in extractant storage tank (8) is sent into extraction reextraction membrane module at the same level (5) through extractant loop head (26), when extractant is flowed through the full shell side of reextraction membrane module (5) from lower to upper, enter and in the liquid after the adjusting pH value of spe membrane (19), need the target substance separating to enter extractant by spe membrane (19) mass transfer, the extractant that comprises target substance is through extractant loop exit (17) inflow extractant storage tank (8); Continue the liquid that regulates pH value in ultrafiltrate and raffinate storage tank (3) to send into extraction reextraction membrane module at the same level (5), after the liquid in ultrafiltrate and raffinate storage tank (3) is used up, again the raffinate in surge tank (11) is sent into ultrafiltrate and raffinate storage tank (3), again this raffinate is carried out to separating and extracting for the second time, repeat extraction and strip until regulate the target substance extraction in the liquid after pH value complete; Raffinate after front a kind of target substance extraction is completely sent into ultrafiltrate and raffinate storage tank (3), regulate the pH value of this raffinate mutually suitable with the pH value of the second target substance that needs to separate, then repeat extraction separation process, extraction needs the target substance separating, until this second target substance extraction completely; Repeat this measure, by the materials different multiple Acidity of Aikalinity in aqueous extract extract and separate respectively;
After each target substance extraction completely, all adopt the solvent of extract in existing method recovery extractant storage tank (8), can obtain the target natural materials of this extract and separate;
If the Acidity of Aikalinity indifference of target substance in aqueous extract, the liquid after ultrafiltration is sent in ultrafiltrate and raffinate storage tank (3) after by described first kind of way or described second way extract and separate, just in the time processing this liquid without the pH value that regulates this liquid, after extract and separate is complete, obtain water extraction and get the mixture of certain the class target substance comprising in ultrafiltration.
6. the method for a few class natural materials of purifying according to claim 5, is characterized in that, in the ultra-filtration process of described step 2, using molecular cut off is 2000～500000 daltonian organic milipore filters, or uses the Inorganic Ultrafiltration Membrane of aperture 2～200nm.
7. the method for a few class natural materials of purifying according to claim 5, it is characterized in that, in described step 3 extraction separation process, the linear rate of flow ratio of several liquid is: ultrafiltration sees through liquid or Cui Yu Ye ︰ Cui Qu Ji ︰ strippant=1 ︰ 0.2～6 ︰ 0.2～1.
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| CN106422810A (en) * | 2016-10-17 | 2017-02-22 | 四川久润环保科技有限公司 | After-treatment device and method for preparing hollow fiber membrane through thermally induced phase separation |
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| CN109731368B (en) * | 2019-02-28 | 2021-12-17 | 甘肃中医药大学 | Method for purifying water-soluble natural organic substances by solid film chemical extraction |
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| CN1356923A (en) * | 1999-04-29 | 2002-07-03 | Dsm生物技术股份有限公司 | Method for separating organic substances from aqueous mixture |
| CN101659794A (en) * | 2009-09-27 | 2010-03-03 | 广西山云生化科技有限公司 | New process for extracting high-purity gardenia yellow pigment by membrane separation and purification technology |
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| CN1356923A (en) * | 1999-04-29 | 2002-07-03 | Dsm生物技术股份有限公司 | Method for separating organic substances from aqueous mixture |
| CN101659794A (en) * | 2009-09-27 | 2010-03-03 | 广西山云生化科技有限公司 | New process for extracting high-purity gardenia yellow pigment by membrane separation and purification technology |
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