CN101712908A - Method and device for extracting aroma component - Google Patents
Method and device for extracting aroma component Download PDFInfo
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- CN101712908A CN101712908A CN200910095060A CN200910095060A CN101712908A CN 101712908 A CN101712908 A CN 101712908A CN 200910095060 A CN200910095060 A CN 200910095060A CN 200910095060 A CN200910095060 A CN 200910095060A CN 101712908 A CN101712908 A CN 101712908A
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Abstract
The invention relates to a method and a device for extracting an aroma component. The method comprises the following steps of: (1) performing pretreatment on a material, and then performing pressure reduction treatment on the treated material in an extraction container; (2) introducing a solvent into the extraction container to mix the solvent and the material, and extracting the mixture to obtain extract liquor; (3) putting the extract liquor into a vaporization separation device to separate out a crude extract of the aroma component, and simultaneously separating the solvent, compressing and cooling the solvent, and then reclaiming the solvent for cyclic utilization; and (4) putting the crude extract of the aroma component into a refining system to perform refining treatment to prepare a refined extract. The extraction device comprises an extraction separation system, the refining system, a solvent purification system, a vacuum system and a heat exchange system. The aroma component extracted by the method and the device has no solvent residue, and the effective active components of a natural plant raw material can be maintained to the utmost extent.
Description
Technical field
The invention belongs to the fine chemical technology field, be specifically related to a kind of method and apparatus that extracts aroma component.
Background technology
At present, the method for extraction aroma component mainly contains and presses mill method, distillation method, solvent-extraction process, supercritical CO from natural phant
2Extraction, ultrasonic extraction etc.It is narrower to press mill method range of application, relatively is applicable to fresh fruit, particularly citrus, but is applied in poor effect on the dried plant material.The distillation method service temperature is higher, and the time is longer, and lower boiling and water soluble ingredient disappearance are bigger.Supercritical CO
2Extraction process only is fit to the extraction of apolar substance to equipment requirement of withstand voltage height.And ultrasonic extraction still rests on laboratory stage, uses with a certain distance from heavy industrialization to also have.
Solvent-extraction process is according to the dissolving properties of various compositions in solvent in the raw material, select for use activeconstituents solubleness big, to not needing the little solvent of stripping composition solubleness, and the method that effective constituent is dissolved out in the cell tissue.When solvent was added in the raw material, solvent had dissolved soluble substance, and has caused the concentration difference inside and outside the cell, thereby desirable ingredients has been bordering on complete stripping or most of stripping owing to diffusion, osmosis penetrate in the cell by cell walls gradually.Solvent-extraction process commonly used mainly contains pickling process, percolation, decocting method, reflux extraction and continuous extraction.Pickling process is relatively simple, but leaching yield is relatively poor, and particularly water is a solvent, and its extracting solution is easy to moldy metamorphism, must note adding suitable preservatives.The percolation leaching efficiency is higher, and leach liquor is clarification, but solvent-oil ratio is big, time-consuming length, and operation does not still want to take the trouble.Decocting method is easy, and most of composition can be proposed to some extent in the plant, but the raw material that contains volatile component and effective constituent preheating destructible should not be used this method, and to containing the raw material of polyose, after the decoction, flowing fluid ratio is than thickness, and specific filtration resistance is difficulty.Reflux extraction and continuous extraction are used propane, butane, sherwood oil etc. always and are made solvent, and this kind solvent has peculiar smell and remains in easily in the extract, influences product quality; In addition, when using these two kinds of methods, solvent is reflux in water-bath, generally will keep for some time of seething with excitement, and makes that extraction composition heated time is longer, so the labile composition of case of thermal instability is lost more.
In sum, traditional extraction aroma component method mainly has the following disadvantages: 1) extract the temperature height, middle lower boiling aroma component loss is many, and there are notable difference in the fragrance and the natural matter of goods; 2) only can single ground extraction water dissolubility or fat-soluble material, and solvent-oil ratio is big; 3) solvent remains in the extract easily, if solvent is impure then can to bring peculiar smell, influences product quality; 4) equipment requirement of withstand voltage height, investment, energy consumption is higher.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, provide a kind of extraction the aroma component no solvent residue, can keep the method for the extraction aroma component of natural plant raw material effective active composition, the present invention that the equipment that extracts aroma component also is provided to greatest extent.
The objective of the invention is to be achieved through the following technical solutions.
A kind of method of extracting aroma component may further comprise the steps:
1) material is carried out pre-treatment, in extraction container, the material after handling is carried out reduced pressure treatment then;
2) solvent being fed in the extraction container and mixing of materials, is-25 ℃～30 ℃ in temperature, extracts under the processing condition of pressure 0.1MPa～0.6MPa, obtains extraction liquid;
3) extraction liquid being sent into the vaporization tripping device, is that-25 ℃～30 ℃, pressure are to isolate the aroma component primary extract under the condition of 0.1MPa～0.2MPa in temperature, and simultaneously with separated from solvent, recycling is reclaimed in compressed, cooling back;
4) the aroma component primary extract being sent into refining system, is-10 ℃～40 ℃ in temperature, and pressure is to be lower than refinement treatment under the condition of 0.06MPa, makes extract;
The described pre-treatment of step 1) of the present invention is sieving and grading, store ageing, fragrant, dipping is given birth in fermentation, one or more the combination of treatment process in dry, in small, broken bits; When material being carried out when in small, broken bits, the raw meal particle size after then in small, broken bits is no more than 3cm; Material pressure of living in is not higher than 0.076MPa during described reduced pressure treatment.Step 2) described material and solvent be mixed into material: solvent was by weight 1: 1
～10Mix, extract 25min～8h then.Adopt forced refluence or stirring means in the extraction process.The described solvent of step 3) of the present invention is a dme, also can be the mixture into dme and water, and wherein, the shared weight percent of water is no more than 8%.Raw material of the present invention is meant spice berry, comprise the root, stem, leaf, flower of plant, really, in the seed one or more contain the position of aroma component.The described solvent recovery cycle utilization of step 3) of the present invention can recycle more than 8 times at the solvent with a kind of materials abstraction; When the solvent cycle access times are less than 6 times, solvent is carried out directly recycling after adsorption and purification is handled; After solvent cycle is used full 6 times, need solvent is carried out carrying out washing treatment earlier, carry out again recycling after adsorption and purification is handled.With material and solvent, extract and isolate the natural pigment primary extract 2～3 times through circulating after, the primary extract that obtains for 2～3 times can be carried out refinement treatment in the lump.
The present invention also provides a kind of equipment that extracts aroma component, and this equipment comprises extracting and separating system, refining system, solvent purification system, vacuum system and heat-exchange system; The extracting and separating system comprises by the extraction kettle of pipeline connection and vaporization tripping device; The solvent purification system comprises by the dme washing device of pipeline connection and dme adsorption and purification device, the dme washing device is communicated with the vaporization tripping device by pipeline, and dme adsorption and purification device is communicated with vaporization tripping device and gaseous state solvent surge tank respectively by pipeline; Refining system is communicated with vaporization tripping device and dme adsorption and purification device respectively by pipeline; Vacuum system is by pipeline and extracting and separating system, refining system, solvent purification system connectivity; Heat-exchange system comprises dme storage tank, first interchanger and second interchanger, first interchanger, one end is communicated with the dme storage tank, the other end is communicated with dme adsorption and purification device, and second interchanger, one end is communicated with extraction kettle, and the other end is communicated with the dme storage tank.
Solvent purification of the present invention system also comprises gaseous solvent surge tank and the compressor by pipeline connection, the gaseous solvent surge tank is communicated with dme adsorption and purification device, compressor is the oil free compressor that has filtering and purifying, and is communicated with first interchanger.
The invention has the beneficial effects as follows: 1. extract at low temperatures, separation, refinement treatment, guarantee the chemically reactive of extract, the fragrance of goods is near natural matter; 2. solvent extraction ability is strong, has good water-solubility and fat-soluble, can extract water-soluble and fat-soluble aroma component in the natural plant raw material simultaneously, at utmost to reduce the aroma component loss; 3. compare extract free from extraneous odour and residual with conventional solvent sherwood oil, butane, propane etc.; 4. the dme production cost is low, recyclable utilization again, and solvent loss is little, and facility investment, energy consumption reduce, and whole leaching process cost effectively reduces.
Further set forth content of the present invention below in conjunction with Figure of description.
Description of drawings
Fig. 1 is the synoptic diagram that the present invention extracts equipment.
Among the figure, 1-dme storage tank, 2-first valve, the 3-volume pump, 4-second interchanger, 5-second valve, the 6-vacuum system, 7-the 3rd valve, 8-the 4th valve, the 9-extraction kettle, 10-solvent cycle hydrocarbon pump, 11-the 5th valve, 12-the 6th valve, 13-reducing valve, 14-the 7th valve, 15-the 8th valve, the 16-tripping device of vaporizing, 17-dme washing device, 18-dme adsorption and purification device, 19-the 9th valve, 20-first interchanger, 21-compressor, 22-gaseous solvent surge tank, the 23-refining system, 24-the tenth valve.
Embodiment
As shown in the figure, extraction equipment of the present invention mainly comprises extracting and separating system, refining system 23, solvent purification system, vacuum system 6 and heat-exchange system; The extracting and separating system comprises by the extraction kettle 9 of pipeline connection and vaporization tripping device 16; The solvent purification system comprises by the dme washing device 17 of pipeline connection and dme adsorption and purification device 18, dme washing device 17 is communicated with vaporization tripping device 16 by pipeline, and dme adsorption and purification device 18 is communicated with vaporization tripping device 16 and gaseous state solvent surge tank 22 respectively by pipeline; Refining system 23 is communicated with vaporization tripping device 16 and dme adsorption and purification device 18 respectively by pipeline; Vacuum system 6 is by pipeline and extracting and separating system, refining system, solvent purification system connectivity; Heat-exchange system comprises that dme storage tank 1, first interchanger 20 and second interchanger, 4, the first interchanger, 20 1 ends are communicated with dme storage tank 1, and the other end is communicated with gaseous solvent surge tank 22 by compressor 21; Second interchanger, 4 one ends are communicated with extraction kettle 9, and the other end is communicated with dme storage tank 1 by volume pump 3.Compressor 21 should adopt oil free compressor or the compressor unit that has filtration unit.Extraction solvent used in the present invention belongs to inflammable, explosive material, can move the vacuum system that needs setting can be simultaneously vacuumizes total system or individual equipment according to equipment.
Concrete technical process is as follows:
1) will be in the raw material of pre-treatment be packed extraction kettle 9 into, close first valve 2, the 9th valve 19, starting 6 pairs of extracting and separating systems of vacuum system, refining system, solvent purification system and connecting pipeline vacuumizes, in extraction container the material after handling is carried out reduced pressure treatment then, material pressure of living in is not higher than 0.076MPa during reduced pressure treatment.
2) close the 3rd valve 7, the 6th valve 12, reducing valve 13, open first valve 2, start volume pump 3, solvent is fed extraction kettle 9 by required raw material and weight of solvent ratio, closing second valve 5, open the 4th valve 8, the 5th valve 11, solvent cycle hydrocarbon pump 10, is-25 ℃～30 ℃ in temperature, carry out extracting operation under the processing condition of pressure 0.1MPa～0.6MPa, obtain extraction liquid.
3) be extracted to required time after, open the 6th valve 12, the 9th valve 19 and reducing valve 13, extraction liquid enters into vaporization tripping device 16, close the 7th valve 14, open the 8th valve 15, adjusting the vaporization separation temperature and be-25 ℃～30 ℃, pressure is 0.1MPa～0.2MPa, and liquid is isolated the aroma component primary extract through the tripping device 16 of vaporizing.One batch raw material is repeated 2～3 extractions successively and separates, and gradation obtains the aroma component primary extract.Simultaneously, solvent gas feeds dme adsorption and purification device 18 through the 8th valve 15 and carries out purification process, gas of dimethyl ether behind the purifying enters gaseous solvent surge tank 22, compressed machine 21 compressions and first interchanger 20 are cooled to liquid dimethyl ether, liquid dimethyl ether is got back in the dme storage tank 1 and is reclaimed solvent, and recirculation is used; But after solvent cycle is used 6 times, need close the 8th valve 15, open the 7th valve 14, will feed dme washing device 17 and dme adsorption and purification device 18 washing and purifying successively through the isolating gas of dimethyl ether of vaporizing, enter gaseous solvent surge tank 22 then, finish the recovery solvent.At solvent, only need additional a small amount of fresh solvent and water promptly to can be recycled more than 8 times with a kind of materials abstraction.When the solvent cycle access times are less than 6 times, solvent is carried out directly recycling after adsorption and purification is handled; After solvent cycle is used full 6 times, need solvent is carried out carrying out washing treatment earlier, carry out again recycling after adsorption and purification is handled.
4) opening the tenth valve 24, the aroma component primary extract that is enriched in vaporization tripping device 16 is fed refining systems 23 through the tenth valve 24, is-10 ℃～40 ℃ in temperature, and pressure is to be lower than refinement treatment under the condition of 0.06MPa, makes extract.From extraction kettle 9, take out extract remainder then.
The heat transferring medium that uses in the heat-exchange system is generally 0 ℃～90 ℃ deionized waters, if extraction kettle 9 service temperatures, should dispose refrigerator and the suitable refrigeration agent of configuration less than 0 ℃, second interchanger 4 and extraction kettle 9 is forced cooling.
Separation system, refining system 23, solvent purification system, vacuum system 6 and heat-exchange system etc. are adopted in the present device stand-alone device and parts all can adopt prior art, only need these stand-alone device and parts are assembled by the present invention to get final product.
Embodiment 1:
With foreign oranges and tangerines drying, pulverize and sieving and grading, require granular size at 0.80mm～15.00mm, pack into then in the extraction kettle 9, close first valve 2, the 9th valve 19, start 6 pairs of extracting and separating systems of vacuum system, refining system, solvent purification system and connecting pipeline are evacuated to 0.076MPa, close the 3rd valve 7, the 6th valve 12, reducing valve 13, open first valve 2, start volume pump 3, solvent (wherein the accounting of water is 8%) is pressed natural plant raw material fed extraction kettle 9 than 1: 4 with weight of solvent, close second valve 5, open the 4th valve 8, the 5th valve 11, solvent cycle hydrocarbon pump 10, control pressure is 20 ℃～25 ℃ of 0.40MPa～0.50MPa and extraction temperature, forced refluence extraction 2h, open valve the 6th valve 12 and reducing valve 13, extraction liquid enters into vaporization tripping device 16, close the 7th valve 14, open the 8th valve 15, adjusting vaporization separation temperature and pressure, is 20 ℃～25 ℃ in temperature, pressure is to isolate gas of dimethyl ether and aroma component crude extract under the condition of 0.20MPa; Gas of dimethyl ether feeds dme adsorption and purification device 18 through the 8th valve 15 and carries out purification process, gas of dimethyl ether behind the purifying enters gaseous solvent surge tank 22, compressed machine 21 compressions and first interchanger 20 are cooled to liquid dimethyl ether, liquid dimethyl ether is got back to and is carried out solvent recuperation in the dme storage tank 1, and recirculation is used 3 times.After finishing above-mentioned extracting operation 2 times, will be enriched in the aroma component primary extract of vaporization tripping device 16 bottoms, and feed refining systems 23 through the tenth valve 24, be 20 ℃～25 ℃ in temperature, and pressure is the refining extract that obtains under the condition of 0.05MPa.Primary extract be raw material heavy 3%, the extract of making accounts for 95% of crude extract weight.Afterwards, from extraction kettle 9, take out extract remainder.
Embodiment 2:
With sieving and grading, ageing, fragrant iris chip drying is given birth in fermentation, ageing, be crushed to 0.30mm～0.83mm, pack into then in the extraction kettle 9, close first valve 2, the 9th valve 19, start 6 pairs of extracting and separating systems of vacuum system, refining system, solvent purification system and connecting pipeline are evacuated to 0.06MPa, close the 3rd valve 7, the 6th valve 12, reducing valve 13, open first valve 2, start volume pump 3, solvent (wherein the accounting of water is 1%) is pressed natural plant raw material fed extraction kettle 9 than 1: 10 with weight of solvent, close second valve 5, open the 4th valve 8, the 5th valve 11, solvent cycle hydrocarbon pump 10, control pressure is 25 ℃～30 ℃ of 0.50MPa～0.60MPa and extraction temperature, forced refluence extraction 30min, open valve the 6th valve 12 and reducing valve 13, extraction liquid enters into vaporization tripping device 16, close the 7th valve 14, open the 8th valve 15, adjusting vaporization separation temperature and pressure, is 25 ℃～30 ℃ in temperature, pressure is to isolate gas of dimethyl ether and aroma component crude extract under the condition of 0.20MPa; Gas of dimethyl ether feeds dme adsorption and purification device 18 through the 8th valve 15 and carries out purification process, gas of dimethyl ether behind the purifying enters gaseous solvent surge tank 22, compressed machine 21 compressions and first interchanger 20 are cooled to liquid dimethyl ether, liquid dimethyl ether is got back to and is carried out solvent recuperation in the dme storage tank 1, and recirculation is used 4 times.After finishing above-mentioned extracting operation 3 times, will be enriched in the aroma component primary extract of vaporization tripping device 16 bottoms, and feed refining systems 23 through the tenth valve 24, be 40 ℃ in temperature, and pressure is the refining extract that obtains under the condition of 0.04MPa.Primary extract be raw material heavy 13%～15%, the extract of making accounts for 97% of crude extract weight.Afterwards, from extraction kettle 9, take out extract remainder.
Embodiment 3:
Rose is in small, broken bits to 3cm, flood with clear water, remove surface-moisture, pack into then in the extraction kettle 9, close first valve 2, the 9th valve 19, start 6 pairs of extracting and separating systems of vacuum system, refining system, solvent purification system and connecting pipeline are evacuated to 0.075MPa, close the 3rd valve 7, the 6th valve 12, reducing valve 13, open first valve 2, start volume pump 3, solvent (wherein the accounting of water is 6%) is pressed natural plant raw material fed extraction kettle 9 than 1: 2 with weight of solvent, close second valve 5, open the 4th valve 8, the 5th valve 11, solvent cycle hydrocarbon pump 10, control pressure is 0.14MPa～0.15MPa and extraction temperature-10 ℃～-5 ℃, forced refluence extraction 25min, open valve the 6th valve 12 and reducing valve 13, extraction liquid enters into vaporization tripping device 16, close the 7th valve 14, open the 8th valve 15, adjusting vaporization separation temperature and pressure, is-10 ℃～-5 ℃ in temperature, pressure is to isolate gas of dimethyl ether and aroma component crude extract under the condition of 0.10MPa; Gas of dimethyl ether feeds dme adsorption and purification device 18 through the 8th valve 15 and carries out purification process, gas of dimethyl ether behind the purifying enters gaseous solvent surge tank 22, compressed machine 21 compressions and first interchanger 20 are cooled to liquid dimethyl ether, liquid dimethyl ether is got back to and is carried out solvent recuperation in the dme storage tank 1, and recirculation is used 3 times.After finishing above-mentioned extracting operation 2 times, will be enriched in the aroma component primary extract of vaporization tripping device 16 bottoms, and feed refining systems 23 through the tenth valve 24, be 0～5 ℃ in temperature, and pressure is the refining extract that obtains under the condition of 0.06MPa.Primary extract be raw material heavy 0.05%, the extract of making accounts for 90% of crude extract weight.Afterwards, from extraction kettle 9, take out extract remainder.
Embodiment 4:
With the Herba Artemisiae annuae drying and crushing to 5.00mm, pack into then in the extraction kettle 9, close first valve 2, the 9th valve 19, start 6 pairs of extracting and separating systems of vacuum system, refining system, solvent purification system and connecting pipeline are evacuated to 0.05MPa, close the 3rd valve 7, the 6th valve 12, reducing valve 13, open first valve 2, start volume pump 3, solvent (wherein the accounting of water is 4%) is pressed natural plant raw material fed extraction kettle 9 than 1: 10 with weight of solvent, close second valve 5, open the 4th valve 8, the 5th valve 11, solvent cycle hydrocarbon pump 10, control pressure is 25 ℃～30 ℃ of 0.50MPa～0.60MPa and extraction temperature, behind the forced refluence extraction 4h, open valve the 6th valve 12 and reducing valve 13, extraction liquid enters into vaporization tripping device 16, close the 7th valve 14, opening the 8th valve 15, adjust vaporization separation temperature and pressure, is 25 ℃～30 ℃ in temperature, pressure is to isolate gas of dimethyl ether and aroma component crude extract under the condition of 0.20MPa; Gas of dimethyl ether feeds dme adsorption and purification device 18 through the 8th valve 15 and carries out purification process, gas of dimethyl ether behind the purifying enters gaseous solvent surge tank 22, compressed machine 21 compressions and first interchanger 20 are cooled to liquid dimethyl ether, liquid dimethyl ether is got back to and is carried out solvent recuperation in the dme storage tank 1, and recirculation is used 8 times.Should emphasize especially after solvent cycle is used 6 times, gas of dimethyl ether is fed after dme washing device 17 washs, feed dme adsorption and purification device 18 purifying again, carry out solvent recuperation after entering gaseous solvent surge tank 22 then.After finishing above-mentioned extracting operation 3 times, will be enriched in the aroma component primary extract of vaporization tripping device 16 bottoms, and feed refining systems 23 through the tenth valve 24, be 35～40 ℃ in temperature, and pressure is the refining extract that obtains under the condition of 0.03MPa.Primary extract be raw material heavy 6%, the extract of making accounts for 95% of crude extract weight.Afterwards, from extraction kettle 9, take out extract remainder.
Embodiment 5:
The rubbing of fresh camellia and salt is mixed, and wherein to be that fresh tea is spent heavy by 10% for the consumption of salt.At room temperature stored ageing 7 days, pack into then in the extraction kettle 9, close first valve 2, the 9th valve 19, start 6 pairs of extracting and separating systems of vacuum system, refining system, solvent purification system and connecting pipeline are evacuated to 0.07MPa, close the 3rd valve 7, the 6th valve 12, reducing valve 13, open first valve 2, start volume pump 3, solvent (wherein the accounting of water is 3%) is pressed natural plant raw material fed extraction kettle 9 than 1: 1.5 with weight of solvent, close second valve 5, open the 4th valve 8, the 5th valve 11, solvent cycle hydrocarbon pump 10, control pressure is 5 ℃～10 ℃ of 0.22MPa～0.27MPa and extraction temperature, forced refluence extraction 6h opens valve the 6th valve 12 and reducing valve 13, and extraction liquid enters into vaporization tripping device 16, close the 7th valve 14, opening the 8th valve 15, adjust vaporization separation temperature and pressure, is 5 ℃～10 ℃ in temperature, pressure is to isolate gas of dimethyl ether and aroma component crude extract under the condition of 0.20MPa; Gas of dimethyl ether feeds dme adsorption and purification device 18 through the 8th valve 15 and carries out purification process, gas of dimethyl ether behind the purifying enters gaseous solvent surge tank 22, compressed machine 21 compressions and first interchanger 20 are cooled to liquid dimethyl ether, liquid dimethyl ether is got back to and is carried out solvent recuperation in the dme storage tank 1, and recirculation is used 5 times.After finishing above-mentioned extracting operation 3 times, will be enriched in the aroma component primary extract of vaporization tripping device 16 bottoms, and feed refining systems 23 through the tenth valve 24, be 5～10 ℃ in temperature, and pressure is the refining extract that obtains under the condition of 0.05MPa.Primary extract be raw material heavy 2.5%, the extract of making accounts for 95% of crude extract weight.Afterwards, from extraction kettle 9, take out extract remainder.
Embodiment 6:
Lavandula angustifolia is dry and be crushed to 0.45mm～0.83mm, pack into then in the extraction kettle 9, close first valve 2, the 9th valve 19, start 6 pairs of extracting and separating systems of vacuum system, refining system, solvent purification system and connecting pipeline are evacuated to 0.05MPa, close the 3rd valve 7, the 6th valve 12, reducing valve 13, open first valve 2, start volume pump 3, solvent (wherein the accounting of water is 5%) is pressed natural plant raw material fed extraction kettle 9 than 1: 2 with weight of solvent, close second valve 5, open the 4th valve 8, the 5th valve 11, solvent cycle hydrocarbon pump 10, control pressure is 15 ℃～20 ℃ of 0.34MPa～0.4MPa and extraction temperature, forced refluence extraction 5h opens valve the 6th valve 12 and reducing valve 13, and extraction liquid enters into vaporization tripping device 16, close the 7th valve 14, opening the 8th valve 15, adjust vaporization separation temperature and pressure, is 25 ℃～30 ℃ in temperature, pressure is to isolate gas of dimethyl ether and aroma component crude extract under the condition of 0.15MPa; Gas of dimethyl ether feeds dme adsorption and purification device 18 through the 8th valve 15 and carries out purification process, gas of dimethyl ether behind the purifying enters gaseous solvent surge tank 22, compressed machine 21 compressions and first interchanger 20 are cooled to liquid dimethyl ether, liquid dimethyl ether is got back to and is carried out solvent recuperation in the dme storage tank 1, and recirculation is used 2 times.After finishing above-mentioned extracting operation 3 times, will be enriched in the aroma component primary extract of vaporization tripping device 16 bottoms, and feed refining systems 23 through the tenth valve 24, be 25～30 ℃ in temperature, and pressure is the refining extract that obtains under the condition of 0.02MPa.Primary extract be raw material heavy 4.5%, the extract of making accounts for 93% of crude extract weight.Afterwards, from extraction kettle 9, take out extract remainder.
Embodiment 7:
With the Flower of Arabian Jasmine drying, pulverize and sieving and grading, control its size at 5.00mm～15.00mm, pack into then in the extraction kettle 9, close first valve 2, the 9th valve 19, start 6 pairs of extracting and separating systems of vacuum system, refining system, solvent purification system and connecting pipeline are evacuated to 0.07MPa, close the 3rd valve 7, the 6th valve 12, reducing valve 13, open first valve 2, start volume pump 3, solvent (all being dme) is pressed natural plant raw material fed extraction kettle 9 than 1: 1 with weight of solvent, close second valve 5, open the 4th valve 8, the 5th valve 11, solvent cycle hydrocarbon pump 10, control pressure is 0.1MPa～0.14MPa and extraction temperature-25 ℃～-10 ℃, behind the forced refluence extraction 8h, open valve the 6th valve 12 and reducing valve 13, extraction liquid enters into vaporization tripping device 16, close the 7th valve 14, open the 8th valve 15, adjusting vaporization separation temperature and pressure, is-25 ℃～-10 ℃ in temperature, pressure is to isolate gas of dimethyl ether and aroma component crude extract under the condition of 0.2MPa; Gas of dimethyl ether feeds dme adsorption and purification device 18 through the 8th valve 15 and carries out purification process, gas of dimethyl ether behind the purifying enters gaseous solvent surge tank 22, compressed machine 21 compressions and first interchanger 20 are cooled to liquid dimethyl ether, liquid dimethyl ether is got back to and is carried out solvent recuperation in the dme storage tank 1, and recirculation is used 2 times.After finishing above-mentioned extracting operation 2 times, will be enriched in the aroma component primary extract of vaporization tripping device 16 bottoms, and feed refining systems 23 through the tenth valve 24, be-10～-5 ℃ in temperature, and pressure is to make with extra care under the condition of 0.03MPa to obtain extract.Primary extract be raw material heavy 3.4%, the extract of making accounts for 85% of crude extract weight.Afterwards, from extraction kettle 9, take out extract remainder.
Embodiment 8:
Garlic is removed the peel, clean, be crushed to below the 0.83mm, pack into then in the extraction kettle 9, close first valve 2, the 9th valve 19, start 6 pairs of extracting and separating systems of vacuum system, refining system, solvent purification system and connecting pipeline are evacuated to 0.06MPa, close the 3rd valve 7, the 6th valve 12, reducing valve 13, open first valve 2, start volume pump 3, solvent (wherein the accounting of water is 7%) is pressed natural plant raw material fed extraction kettle 9 than 1: 2 with weight of solvent, close second valve 5, open the 4th valve 8, the 5th valve 11, solvent cycle hydrocarbon pump 10, control pressure are 25 ℃～30 ℃ of 0.5MPa～0.6MPa and extraction temperature, forced refluence extraction 40min, open valve the 6th valve 12 and reducing valve 13, extraction liquid enters into vaporization tripping device 16, closes the 7th valve 14, opens the 8th valve 15, adjusting vaporization separation temperature and pressure, is 30 ℃～35 ℃ in temperature, pressure is to isolate gas of dimethyl ether and aroma component crude extract under the condition of 0.1MPa; Gas of dimethyl ether feeds dme adsorption and purification device 18 through the 8th valve 15 and carries out purification process, gas of dimethyl ether behind the purifying enters gaseous solvent surge tank 22, compressed machine 21 compressions and first interchanger 20 are cooled to liquid dimethyl ether, liquid dimethyl ether is got back to and is carried out solvent recuperation in the dme storage tank 1, and recirculation is used 3 times.After finishing above-mentioned extracting operation 3 times, will be enriched in the aroma component primary extract of vaporization tripping device 16 bottoms, and feed refining systems 23 through the tenth valve 24, be 30～35 ℃ in temperature, and pressure is not more than the refining extract that obtains under the condition of 0.015MPa.Primary extract be raw material heavy 8%, the extract of making accounts for 93% of crude extract weight.Afterwards, from extraction kettle 9, take out extract remainder.
Claims (11)
1. a method of extracting aroma component is characterized in that, may further comprise the steps:
1), in extraction container, the material after handling is carried out reduced pressure treatment then with the material pre-treatment;
2) solvent being fed in the extraction container and mixing of materials, is-25 ℃～30 ℃ in temperature, extracts under the processing condition of pressure 0.1MPa～0.6MPa, obtains extraction liquid;
3) extraction liquid being sent into the vaporization tripping device, is that-25 ℃～30 ℃, pressure are to isolate the aroma component primary extract under the condition of 0.1MPa～0.2MPa in temperature, and simultaneously with separated from solvent, recycling is reclaimed in compressed, cooling back;
4) the aroma component primary extract being sent into refining system, is-10 ℃～40 ℃ in temperature, and pressure is made extract for refinement treatment under the condition that is not higher than 0.06MPa;
2. the method for extraction aroma component as claimed in claim 1 is characterized in that, the described pre-treatment of step 1) is sieving and grading, store ageing, fragrant, dipping is given birth in fermentation, one or more the combination of treatment process in dry, in small, broken bits; When material being carried out when in small, broken bits, the raw meal particle size after then in small, broken bits is no more than 3cm; Material pressure of living in is not higher than 0.076MPa during described reduced pressure treatment.
3. the method for extraction aroma component as claimed in claim 1 is characterized in that step 2) material that is mixed into of described material and solvent: solvent mixes by weight 1: 1～10, extracts 25min～8h then.
4. as the method for claim 1 or 3 described extraction aroma components, it is characterized in that, adopt forced refluence or stirring means in the extraction process.
5. the method for extraction aroma component as claimed in claim 1 is characterized in that, the described solvent of step 3) is a dme.
6. the method for extraction aroma component as claimed in claim 1 is characterized in that, the described solvent of step 3) is the mixture of dme and water, and wherein, the shared weight percent of water is no more than 8%.
7. as the method for claim 1 or 2 or 3 described extraction aroma components, it is characterized in that described raw material is meant spice berry, comprise the root, stem, leaf, flower of plant, really, in the seed one or more contain the position of aroma component.
8. the method for extraction aroma component as claimed in claim 1 is characterized in that, the described solvent recovery cycle utilization of step 3) can recycle more than 8 times at the solvent with a kind of materials abstraction; When the solvent cycle access times are less than 6 times, solvent is carried out directly recycling after adsorption and purification is handled; After solvent cycle is used full 6 times, need solvent is carried out carrying out washing treatment earlier, carry out again recycling after adsorption and purification is handled.
9. the method for extraction aroma component as claimed in claim 1 is characterized in that, with material and solvent, extract and isolate the natural pigment primary extract 2～3 times through circulating after, the primary extract that obtains for 2～3 times is carried out refinement treatment in the lump.
10. an equipment that extracts aroma component is characterized in that, this equipment comprises extracting and separating system, refining system (23), solvent purification system, vacuum system (6) and heat-exchange system; The extracting and separating system comprises extraction kettle (9) and the vaporization tripping device (16) by pipeline connection; The solvent purification system comprises by the dme washing device (17) of pipeline connection and dme adsorption and purification device (18), dme washing device (17) is communicated with vaporization tripping device (16) by pipeline, and dme adsorption and purification device (18) is communicated with vaporization tripping device (16) and gaseous state solvent surge tank (22) respectively by pipeline; Refining system (23) is communicated with vaporization tripping device (16) and dme adsorption and purification device (18) respectively by pipeline; Vacuum system (6) is by pipeline and extracting and separating system, refining system, solvent purification system connectivity; Heat-exchange system comprises dme storage tank (1), first interchanger (20) and second interchanger (4), first interchanger (20) one ends are communicated with dme storage tank (1), the other end is communicated with dme adsorption and purification device (18), second interchanger (4) one ends are communicated with extraction kettle (9), and the other end is communicated with dme storage tank (1).
11. a kind of equipment that extracts aroma component as claimed in claim 11, it is characterized in that, described solvent purification system also comprises gaseous solvent surge tank (22) and the compressor (21) by pipeline connection, gaseous solvent surge tank (22) is communicated with dme adsorption and purification device (18), compressor (21) is the oil free compressor that has filtering and purifying, and is communicated with first interchanger (20).
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| CN200910095060A CN101712908A (en) | 2009-10-15 | 2009-10-15 | Method and device for extracting aroma component |
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| CN200910095060A CN101712908A (en) | 2009-10-15 | 2009-10-15 | Method and device for extracting aroma component |
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| CN103122277A (en) * | 2013-01-23 | 2013-05-29 | 兰州大学 | Method for extracting natural flavor with dimethyl ether |
| CN103602522A (en) * | 2013-12-04 | 2014-02-26 | 中山鼎晟生物科技有限公司 | Extraction method for plant aromatic stock solution and preparation method for solidified essence from aromatic stock solution |
| CN104087424A (en) * | 2014-08-04 | 2014-10-08 | 安阳市晶华油脂工程有限公司 | Method for one-step extraction and separation of essential oil, water solution and lipid of fresh peony flowers |
| CN105001667A (en) * | 2014-08-10 | 2015-10-28 | 王选明 | System for rapidly extracting natural plant pigments |
| CN105062123A (en) * | 2014-08-10 | 2015-11-18 | 王选明 | Equipment for rapidly extracting pigments from rhododendron simsii planch |
| CN105392545A (en) * | 2012-12-28 | 2016-03-09 | 科莱恩国际有限公司 | Method for obtaining aromatics |
| CN106675085A (en) * | 2014-08-10 | 2017-05-17 | 王选明 | System for quickly extracting pigment from azalea flowers |
| CN111849632A (en) * | 2020-07-24 | 2020-10-30 | 云南养瑞科技集团有限公司 | Deep processing method of natural tobacco flavor raw material and application of natural tobacco flavor raw material in novel tobacco |
| CN112094697A (en) * | 2020-09-04 | 2020-12-18 | 北京中科环通工程科技有限公司 | Extraction method of citrus essential oil |
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| CN102876455A (en) * | 2010-12-13 | 2013-01-16 | 云南瑞升烟草技术（集团）有限公司 | Three-step preparation method of vanillic spices for tobacco |
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| CN103122277A (en) * | 2013-01-23 | 2013-05-29 | 兰州大学 | Method for extracting natural flavor with dimethyl ether |
| CN103602522A (en) * | 2013-12-04 | 2014-02-26 | 中山鼎晟生物科技有限公司 | Extraction method for plant aromatic stock solution and preparation method for solidified essence from aromatic stock solution |
| CN104087424A (en) * | 2014-08-04 | 2014-10-08 | 安阳市晶华油脂工程有限公司 | Method for one-step extraction and separation of essential oil, water solution and lipid of fresh peony flowers |
| CN104087424B (en) * | 2014-08-04 | 2016-06-29 | 安阳市晶华油脂工程有限公司 | The method that one step extracts, separates fresh peony flower quintessence oil, aqueous solution, lipid |
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| CN106675085A (en) * | 2014-08-10 | 2017-05-17 | 王选明 | System for quickly extracting pigment from azalea flowers |
| CN105001667A (en) * | 2014-08-10 | 2015-10-28 | 王选明 | System for rapidly extracting natural plant pigments |
| CN106675085B (en) * | 2014-08-10 | 2019-01-15 | 三门华迈化工产品有限公司 | A kind of system for from the middle rapidly extracting pigment of azalea |
| CN111849632A (en) * | 2020-07-24 | 2020-10-30 | 云南养瑞科技集团有限公司 | Deep processing method of natural tobacco flavor raw material and application of natural tobacco flavor raw material in novel tobacco |
| CN112094697A (en) * | 2020-09-04 | 2020-12-18 | 北京中科环通工程科技有限公司 | Extraction method of citrus essential oil |
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