CN103127741A - Method for enhancing natural product solvent extraction through membrane separation process - Google Patents
Method for enhancing natural product solvent extraction through membrane separation process Download PDFInfo
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Abstract
The invention provides a method for enhancing natural product solvent extraction through a membrane separation process. The method is based on a basic principle that: during a natural product solvent extraction process, after extraction process is started for a period of time or when active component in an extraction liquid reaches a certain concentration, the extraction liquid is continuously delivered into a membrane separation device through an extraction device. During the membrane separation process, a separation membrane with a retention performance upon active component is selected; under the effect of pressure, the solvent penetrates the separation membrane, and the active component is retained and thus concentrated. The concentrated active component solution is outputted as a product or is delivered into subsequent sections; and the permeated liquid with the active component being removed is returned back to the extraction device. According to the method, through the membrane separation process, active component dissolved in the extraction process is removed from the extraction device, and concentration is realized at the same time, such that efficiency and active component recovery rate of the extraction process are improved, solvent dose is reduced, and concentration and desolvation costs are reduced.
Description
Technical field
The present invention relates to utilize the film separation process to strengthen the method for solvent extraction natural products, particularly by membrane separation concentrated compression process, the active component in the solvent extraction process is in time shifted out, obtain simultaneously the method for concentrated product.The invention belongs to the natural prodcuts active component and extract separation field.
Background technology
Solvent extraction method is the method for active component of extracting the solid natural products such as the most frequently used natural plants from Chinese herb, non-Chinese medicine, non-Chinese medicine natural animal, natural minerals, edible fungus.Solvent extraction method is the difference according to the active component in natural products, selects the solvent that active component is had the selective dissolution ability, under different conditions, and the method that active ingredient is dissolved out from the solid natural products.When solvent is added in appropriate fragmentation or pretreated solid natural products raw material, solvent enters in the cell of solid-phase or natural products by diffusion, osmosis, the dissolving solable matter, cause solid-phase and liquid concentration difference mutually, and then the intracellular active component that makes solid-phase or natural products is constantly to external diffusion, during solvent constantly enters again in solid-phase or cell, so repeatedly come and go, until two phase liquid concentration is when reaching dynamic equilibrium, leach solution, continue to add novel solvent, just can be the progressively stripping of needed composition.According to the difference of active material, can select different solvents, solvent can be divided into water and sour water or buck, hydrophilic organic solvent, lipophilicity organic solvent.Solvent extraction method is different with technique according to actual conditions, can be divided into infusion process, percolation, decocting method, reflux extraction, continuous extraction etc.
In various solvent extraction processes, along with the carrying out of leaching process, the content of the active component in solution all can improve gradually, between the solid-liquid two-phase or the inside and outside concentration difference of cell reduce, the solvent extraction effect descends, and improves extraction rate as need, just need to change solvent, to guarantee concentration difference.Common solvent extraction process needs to change solvent 2-3 time, and solvent load is generally about 8-12 times of amount of solid.It is long that this mode exists extraction time, and the solvent use amount is large, and the active component extraction efficiency is low, and active component reclaims the problems such as incomplete.At present, proposed a lot of methods, comprised that hot reflux low temperature extracts, supercritical extract, ultrasonic wave extracts, microwave abstracting, the improved extracting methods such as counter current chromatography extraction have all obtained certain effect.But, remain the extracting method of main flow as the solvent extraction method of representative take infusion process, percolation, decocting method, above-mentioned improving one's methods all needs new equipment is significantly changed or set up to original solvent extraction equipment, and concentrating of extract still needs to adopt mode of heating, in concentration process, solvent still exists phase transformation and condensation process, needs energy consumption large, and has the volatilization loss of solvent.
Membrane separation technique is due to its technique green non-pollution, and energy consumption is low, and separative efficiency is high, has in recent years obtained paying close attention to widely.Carry out in the concentrated process of natural product extraction liquid at using membrane separating technology, processed solution is under the promotion of pressure differential, and solvent sees through fenestra and flows out, suspended particulates, colloid molecule and the large molecule of solute etc. are trapped within main body solution, thereby the realize target material is concentrated.Due in the membrane technology concentration process, solvent does not undergo phase transition, and does not need the heat of transformation, so running cost even compare with energy-conservation Multi-effect Evaporation Processes, also has the advantage on energy consumption well below the needed energy consumption of heating evaporation operation.On the other hand, owing to there is no phase transition process, and membrane process is closed-loop operation, and the solvent evaporates amount is little, to the nonaqueous solvents leaching process, can reduce significantly solvent loss.
Advantage based on the film separation process, the present invention proposes a kind of method that the solvent extraction natural products is strengthened in film separation process, the method in time shifts out the active component of dissolving in the solvent extraction process by the film separation process and realizes simultaneously concentrated from extraction equipment, reduced the concentration of the active component in the extraction equipment, the efficient of leaching process and the rate of recovery of active component have been improved, consumption and the loss amount of solvent have been reduced, operating cost due to the film separation process will lower than evaporation operation, can also reduce the cost of concentrated desolventizing process greatly simultaneously.
Summary of the invention
The object of the present invention is to provide a kind of film separation process to strengthen the method for solvent extraction natural products, this method is with respect to the solvent extraction process of routine, can decrease extraction time, improve the rate of recovery of extraction efficiency and active component, reduce consumption and the loss amount of solvent, can also greatly reduce the concentrated running cost of extract simultaneously.
the present invention is directed to the problem that exists in the conventional solvent extraction process of natural products, film separation process and leaching process are combined, in the solvent extraction process, when leaching process begins after in certain hour or extract, active component reaches finite concentration, continuously extract is transported in film device by extraction equipment, the diffusion barrier that active component is had cutoff performance is selected in the film separation process, under pressure, solvent sees through diffusion barrier, active component is trapped and is concentrated, active component solution after concentrated is as output of products or enter follow-up workshop section, the liquid that sees through that has removed active component turns back in extraction equipment.
Described leaching process is dipping process, diacolation process, decoction process, refluxing extraction process or continuous leaching process, and leaching process is heating leaching process or normal temperature leaching process.
Described diffusion barrier is selected milipore filter, NF membrane or the reverse osmosis membrane of cellulose, cellulose acetate, SPSF, polyamide, polyimides, polyether sulfone, sulfonated polyether sulfone, poly-piperazine or polyvinyl alcohol material, and the diffusion barrier of selection has cutoff performance to active component to be extracted.
The mode of operation of described film separation process is cross-flow filtration mode, end-filtration mode or draws filter type.
Described film separation process is by filtration, and heat exchange is cooling, boosts, and extract enters membrane module, and concentrate output sees through the liquid heat exchange, sees through liquid and returns to the extraction equipment step and consist of.To the normal temperature leaching process, extract is pressed and delivered in membrane module by feed pump after directly removing by filter suspended particulate.To the heating leaching process, need to be after filtration system, enter membrane module after the temperature that the cooling heat exchange can be born to membrane module.
Described membrane module is rolling, doughnut formula, tubular type or flat.
Described heat exchange step is for the heating leaching process, mode of operation is that the extract that comes from extractor is as thermal source, membrane process see through liquid as low-temperature receiver, carry out heat exchange, the liquid that sees through after heating turns back to extraction equipment, and cooled extract directly enters film device or further enters film device after cooling with cooling water.
Pressure limit in described film separation process is 0.5MPa～6.0MPa, and temperature is 15-70 ℃.
The solvent extraction process that film separation process provided by the invention is strengthened is compared with conventional solvent extraction process, has following outstanding characteristics and advantages:
1. the method in time shifts out the active component in leaching process by the film separation process from extraction equipment, thereby reduces the concentration of active component in extract, improves the rate of recovery of extraction efficiency and active component, reduces the addition of solvent.
2. the film separation process adopts the infiltration of pressure-driven solvent by diffusion barrier, there is no phase transition process, and therefore concentrated cost is significantly less than the heating concentration process.
3. the film separation process closed-loop operation that adopts of the method and there is no phase transition process, the solvent evaporates amount is little, to the nonaqueous solvents leaching process, can significantly reduce solvent loss.
Description of drawings
Fig. 1. the method schematic diagram of solvent extraction natural products is strengthened in the film separation process.
The specific embodiment
The present invention will be further described below in conjunction with embodiment.Theme protection domain involved in the present invention is not limited only to these embodiment.
Embodiment 1:
The volume of extraction equipment is 3L, add 2L water, 200g rabdosia lophanthide raw material, after heating 30 minutes under 100 ℃, bottom extraction equipment, extract is taken out, remove after filtration suspended particulate, enter heat transmission equipment, by the film separation process see through liquid and the cooling water heat exchange cools to 40 ℃, be pressurized to 3.0MPa and enter membrane module.Select the reverse osmosis membrane that the rabdosia lophanthide active component is had high cutoff performance in membrane module, under pressure-driven, moisture sees through diffusion barrier, and the active ingredient in extract is all held back fully, sees through fluid solid content lower than 0.001%.Adjust the operating parameter of film separation process, make the concentration of concentrate reach 10 times of charging extract concentration, in extract, 90% moisture is removed, and concentrate is as output of products or enter follow-up workshop section.See through liquid and enter heat exchanger, extract is lowered the temperature, the temperature that sees through simultaneously liquid is brought up to approximately 70 ℃, turns back to extractor.After the film separation process was carried out 1 hour, stopped heating extracted and the film lock out operation.Obtain approximately 150mL of concentrate this moment, remains approximately 1.85L in extraction equipment, and in concentrate, solid content is 12%, and the solid content in the residue extract is 0.6%, and total solid yield (ratio of soluble solids thing total amount and material quantity) is about 14.6%.Under same rabdosia lophanthide material quantity and amount of solvent condition, directly heating was extracted after 2 hours, and the solid yield of the extract that obtains is about 12% left and right.The embodiment result shows, the extracting method that membrane process is strengthened can improve the yield of active component, and can significantly reduce extraction time.
Embodiment 2:
The volume of extraction equipment is 3L, add 2L water, 200g rabdosia lophanthide raw material, 100 ℃ of heating are after 30 minutes, bottom extraction equipment, extract is taken out, remove after filtration suspended particulate, enter heat transmission equipment, by the film separation process see through liquid and the cooling water heat exchange cools to 40 ℃, be pressurized to 1.0MPa and enter membrane module.Select molecular cut off to be about the NF membrane of 500Da in membrane module, under pressure-driven, moisture sees through diffusion barrier, and the most active ingredients in extract are held back, the little molecule infiltrations such as part active component and inorganic salts are crossed film, see through fluid solid content and are about 0.01%.Adjust the operating parameter of film separation process, make the concentration of concentrate reach 10 times of extract, in extract, 90% moisture is removed, and concentrate is as output of products or enter follow-up workshop section.See through liquid and enter heat exchanger, extract is lowered the temperature, the temperature that sees through simultaneously liquid is brought up to approximately 70 ℃, turns back to extractor.After the film separation process was carried out 1 hour, stopped heating extracted and the film lock out operation.Obtain approximately 200mL of concentrate this moment, the about 1.8L of residue in extraction equipment, and in concentrate, solid content is 10.5%, and the solid content in extract is 0.6%, and total solid yield is approximately 15%.Under same rabdosia lophanthide material quantity and amount of solvent condition, simple heating was extracted after 2 hours, and the total solid yield of the extract that obtains is about 12% left and right.The embodiment result shows, the extracting method that membrane process is strengthened can improve the yield of active component, reduces extraction time.
Embodiment 3:
The volume of extraction equipment is 3L, add 1.2L water, 200g rabdosia lophanthide raw material, 100 ℃ of heating are after 30 minutes, bottom extraction equipment, extract is taken out, remove after filtration suspended particulate, enter heat transmission equipment, by the film separation process see through liquid and the cooling water heat exchange cools to 40 ℃, be pressurized to 3.0MPa and enter membrane module.Select the reverse osmosis membrane that the rabdosia lophanthide active component is had high cutoff performance in membrane module, under pressure-driven, moisture sees through diffusion barrier, and the active ingredient in extract is all held back fully, sees through fluid solid content and is about 0.001%.Adjust the operating parameter of film separation process, make the concentration of concentrate reach 6 times of extract, in extract, 83% moisture is removed, and concentrate is as output of products or enter follow-up workshop section.See through liquid and enter heat exchanger, extract is lowered the temperature, the temperature that sees through simultaneously liquid is brought up to approximately 70 ℃, turns back to extractor.After the film separation process was carried out 1 hour, stopped heating extracted and the film lock out operation.After the film separation process was carried out 1.5 hours, stopped heating extracted and the film lock out operation.Obtain approximately 125mL of concentrate this moment, the about 1075mL of residue in extraction equipment, and in concentrate, solid content is 12%, and the solid content in extract is 1.3%, and total solid yield is approximately 14.4%.The embodiment result shows, the extracting method that membrane process is strengthened can reduce the use amount of solvent in the situation that substantially keep identical solid yield.
Embodiment 4:
The volume of extraction equipment is 3L, add 2L water, 200kg rainbow conk raw material, 100 ℃ of heating are after 30 minutes, bottom extraction equipment, extract is taken out, remove after filtration suspended particulate, enter heat transmission equipment, by the film separation process see through liquid and cooling water heat exchange to 40 ℃, be pressurized to 1.5MPa and enter the film concentrator.Select the NF membrane that the rainbow conk active component is had high cutoff performance in membrane module, under pressure-driven, moisture sees through diffusion barrier, and the most active ingredients in extract are held back, the little molecule infiltrations such as part active component and inorganic salts are crossed film, see through fluid solid content lower than 0.005%.Adjust the operating parameter of film separation process, make the concentration of concentrate reach 10 times of extract, in extract, 90% moisture is removed, and concentrate is as output of products or enter follow-up workshop section.See through liquid and enter heat exchanger, extract is lowered the temperature, the temperature that sees through simultaneously liquid is brought up to approximately 70 ℃, turns back to extractor.After the film separation process was carried out 1.5 hours, stopped heating extracted and the film lock out operation.Obtain approximately 100mL of concentrate this moment, the about 1.9L of residue in extraction equipment, and in concentrate, solid content is 15%, and the solid content in extract is 0.48%, and total solid yield is approximately 12%.Under same rainbow conk material quantity and amount of solvent condition, simple heating was extracted after 2 hours, and the solid yield of the extract that obtains is about 10% left and right.The embodiment result shows, the extracting method that membrane process is strengthened can improve the yield of rainbow conk active component.
Embodiment 5:
The volume of extraction equipment is 3m
3, add 2m
3Water, 200kg rabdosia lophanthide raw material, 100 ℃ of heating were taken out extract in extraction equipment bottom after 30 minutes, removed after filtration suspended particulate, entered heat transmission equipment, by the film separation process see through liquid and cooling water heat exchange to 40 ℃, be pressurized to 3.0MPa and enter membrane module.Select the reverse osmosis membrane that the rabdosia lophanthide active component is had high cutoff performance in membrane module, under pressure-driven, moisture sees through diffusion barrier, and the active ingredient in extract is all held back fully, sees through fluid solid content lower than 0.001%.Adjust the operating parameter of film separation process, make the concentration of concentrate reach 10 times of extract, in extract, 90% moisture is removed, and concentrate is as output of products or enter follow-up workshop section.See through liquid and enter heat exchanger, extract is lowered the temperature, the temperature that sees through simultaneously liquid is brought up to approximately 70 ℃, turns back to extractor.After the film separation process was carried out 1 hour, stopped heating extracted and the film lock out operation.Obtain approximately 150L of concentrate this moment, remains approximately 1.85m in extraction equipment
3, in concentrate, solid content is 12%, and the solid content of residue in extract is 0.6%, and total solid yield is approximately 14.6%.Under same rabdosia lophanthide material quantity and amount of solvent condition, simple heating was extracted after 2 hours, and the total solid yield of the extract that obtains is about 12% left and right.The embodiment result shows, the extracting method that membrane process is strengthened can improve the yield of active component, and can significantly reduce extraction time.
Embodiment 6:
The volume of extraction equipment is 3L, add 2L ethanol (concentration 95%), 200g ginkgo leaf raw material, 80 ℃ of heating are after 30 minutes, bottom extraction equipment, extract is taken out, remove after filtration suspended particulate, enter heat transmission equipment, by the film separation process see through liquid and cooling water heat exchange to 40 ℃, be pressurized to 4.0MPa and enter membrane module.Select the reverse osmosis membrane that Active Components of Ginkgo Leaves is had high cutoff performance in membrane module, under pressure-driven, solvent sees through diffusion barrier, and the active ingredient in extract is all held back fully, sees through fluid solid content lower than 0.001%.Adjust the parameter of film separation process, make the concentration of concentrate reach 4 times of extract, in extract, 75% solvent is removed, and concentrate is as output of products or enter follow-up workshop section.See through liquid and enter heat exchanger, extract is lowered the temperature, the temperature that sees through simultaneously liquid is brought up to approximately 70 ℃, turns back to extractor.After the film separation process was carried out 2 hours, stopped heating extracted and the film lock out operation.Obtain approximately 100mL of concentrate this moment, the about 1.9L of residue in extraction equipment, and in concentrate, solid content is 20%, and the solid content in the residue extract is 1%, and total solid yield is approximately 19.5%.Under same ginkgo leaf material quantity and amount of solvent condition, simple heating was extracted after 3 hours, and the total solid yield of the extract that obtains is about 16.6% left and right.The embodiment result shows, the extracting method that membrane process is strengthened can improve the yield of ginkgo leaf active component, and the time that can significantly reduce leaching process.
Claims (8)
1. the method for solvent extraction natural products is strengthened in a film separation process, it is characterized in that beginning after in certain hour or extract, active component reaches finite concentration when leaching process, continuously extract is transported in membrane separation plant by extraction equipment, the diffusion barrier that active component is had cutoff performance is selected in the film separation process, under pressure, solvent sees through diffusion barrier, active component is trapped and is concentrated, active component solution after concentrated is as output of products or enter follow-up workshop section, and the liquid that sees through that has removed active component turns back in extraction equipment.
2. method according to claim 1 is characterized in that: described leaching process is dipping process, diacolation process, decoction process, refluxing extraction process or leaching process continuously.
3. method according to claim 1, it is characterized in that: described diffusion barrier is selected milipore filter, NF membrane or the reverse osmosis membrane of cellulose, cellulose acetate, SPSF, polyamide, polyimides, polyether sulfone, sulfonated polyether sulfone, poly-piperazine or polyvinyl alcohol material, and the diffusion barrier of selection has cutoff performance to the active component of extracting.
4. method according to claim 1, it is characterized in that: the mode of operation of described film separation process is cross-flow filtration mode, end-filtration mode or draws filter type.
5. method according to claim 1 is characterized in that: described film separation process is by filtration, and heat exchange is cooling, boosts, and extract enters membrane module, and concentrate output sees through the liquid heat exchange, sees through liquid and returns to the extraction equipment step and consist of.
6. method according to claim 5, it is characterized in that: described membrane module is rolling, doughnut formula, tubular type or flat.
7. method according to claim 5, it is characterized in that: described heat exchange step is for the heating leaching process, mode of operation is that the extract that comes from extractor is as thermal source, membrane process see through liquid as low-temperature receiver, carry out heat exchange, the liquid that sees through after heating turns back to extraction equipment, and cooled extract directly enters film device or further enters film device after cooling with cooling water.
8. method according to claim 1, it is characterized in that: the pressure limit in described film separation process is 0.5MPa～6.0MPa, temperature is 15-70 ℃.
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| CN103356801A (en) * | 2013-07-23 | 2013-10-23 | 宁波立华制药有限公司 | Method for preparing bazhen granule by low-temperature continuous extraction combined with membrane separation technology |
| CN103861317A (en) * | 2014-02-25 | 2014-06-18 | 厦门世达膜科技有限公司 | Soxhlet extraction device based on membrane technology |
| CN104162289A (en) * | 2014-08-10 | 2014-11-26 | 胡刘满 | Equipment for rapidly extracting total flavones of rhododendra |
| CN104174183A (en) * | 2014-08-10 | 2014-12-03 | 胡刘满 | System for extracting flavone in stems and leaves of plants |
| CN104759110A (en) * | 2015-03-12 | 2015-07-08 | 浙江天草生物科技股份有限公司 | Plant continuous extraction system |
| CN105061379A (en) * | 2014-08-10 | 2015-11-18 | 胡刘满 | Equipment for rapidly extracting flavone from plants |
| CN105153736A (en) * | 2014-08-10 | 2015-12-16 | 王选明 | Energy-efficient equipment for extracting plant pigments |
| CN107446707A (en) * | 2017-09-22 | 2017-12-08 | 山东理工大学 | UF membrane strengthens lard ordinary-pressure hydrolysis reaction and prepares fatty acid process |
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| CN103356801A (en) * | 2013-07-23 | 2013-10-23 | 宁波立华制药有限公司 | Method for preparing bazhen granule by low-temperature continuous extraction combined with membrane separation technology |
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| CN105153736B (en) * | 2014-08-10 | 2019-04-12 | 河北瑞龙生物科技有限公司 | Extract the energy-saving equipment of phytochrome |
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| CN107446707A (en) * | 2017-09-22 | 2017-12-08 | 山东理工大学 | UF membrane strengthens lard ordinary-pressure hydrolysis reaction and prepares fatty acid process |
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Application publication date: 20130605 |