CN105349262A - Method for extraction of plant essential oil aroma component by water jet milling and centrifugation membrane pressure-reduction low-temperature distillation - Google Patents
Method for extraction of plant essential oil aroma component by water jet milling and centrifugation membrane pressure-reduction low-temperature distillation Download PDFInfo
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- CN105349262A CN105349262A CN201510732763.XA CN201510732763A CN105349262A CN 105349262 A CN105349262 A CN 105349262A CN 201510732763 A CN201510732763 A CN 201510732763A CN 105349262 A CN105349262 A CN 105349262A
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/0003—Compounds of unspecified constitution defined by the chemical reaction for their preparation
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/027—Recovery of volatiles by distillation or stripping
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Abstract
The invention relates to a method for extraction of a plant essential oil aroma component by water jet milling and centrifugation membrane pressure-reduction low-temperature distillation. The method comprises S1, adding crushed plant essential oil aroma component extraction raw materials into a stirring tank, adding water into the stirring tank, carrying out stirring, and feeding the mixture into a centrifuge, S2, conveying the separated heavy substances into a water jet mill, and carrying out water jet milling, S3, conveying the light substances obtained by the step S2 into an upper feeding inlet of a multilayer disc-type centrifugation and gravity film-forming and differential pressure reduction low-temperature evaporator, wherein the low-temperature evaporator comprises rotary conical surface discs and fixed conical surface discs coaxially stacked at intervals and the rotary conical surface discs are fixed to a central shaft and rotate, and S4, sucking a gas phase fragrant oily substance and steam together into a condenser, condensing the gas phase fragrant oily substance and water steam together to obtain a liquid, and separating the gas phase fragrant oily substance and the condensate water by a separator so that the plant essential oil aroma component is obtained. The method realizes milling and distillation extraction of a high-quality plant essential oil aroma component by a pure physical method.
Description
Technical field
The present invention relates to scented plants processing technique field, more particularly, relate to a kind of method of nappe flip length and centrifugal film decompression low-temperature distillation extraction plants essential oil fragrance.
Background technology
Along with the raising of modern society's health level, and people are to the approval of " back to nature " theory, be raw-material medicine with natural phant, food, health care and skin care product etc. are more and more paid attention to, wherein, plant-derived essential oil is except having pleasant aroma component, mostly there is extremely strong seepage force, enter skin, assistance body circulates, the curative effects such as calm nerves, also have anti-oxidant, scavenging free radicals, soft skin, antibacterial bacteriostatic, the effects such as delaying senility, advocating the today of " green consumption ", people are enjoyed to favor, therefore, in medical health care, food-drink, the industry such as makeup and daily-use chemical industry is used widely.
Essential oil, also known as volatile oil, is the general name that the class contained in plant has the oily composition of aromatic odour, take from the flower of scented plants, really, organ containing essential oil of leaf, branch, skin, root or subterraneous stem, seed etc. and resinous secretion.Essence main body of oil is fatty compounds and aromatics, comprises alcohols, ester class, phenols, aldehydes, ketone, ethers, terpene hydrocarbons, arene etc.In the cell of these fragrant oily species distribution in the glandular hairs of plant, grease chamber, oil pipe, the various tissue such as secretory cavity or resin canal, epidermis, parenchyma and vascular bundle and organ and in intercellular substance.When stripping, must first could discharge through cell walls and cytolemma.But the cell tissue of plant is tight usually, and cell walls is also very thick, makes solvent not easily permeate and spread, effective constituent or solvend are difficult to by derect seething out.
Therefore, in order to effectively extract the fragrant oily mater that these content are generally only 0.001% ~ 10%, first pulverization process should be carried out to scented plants, so that the stripping smoothly enough in a solvent of these fragrant oily substances.
In the art, various known method of extraction of essential oil comprises:
Milling process: the fragrant oily mater in plant tissue organ is fully squeezed out by pressure effect.This method avoid essential oil to be heated the change of the chemical composition that may cause and function, essential oil quality can be ensured, and simple to operate, with strong points, but shortcoming to be oil yield lower.
Distillation method: be extract one of the most frequently used method of essential oil, raw material is put into water distilling apparatus, bottom-heated or pass into water vapor, the oil storage cell making essential oil break through plant discharges, then is cooled to liquid by condenser, last oily water separation.The method is applicable to not react with water, indissoluble or water insoluble, and volatility is good, the extraction of essential oil that composition is not easily destroyed at still-process, and shortcoming is that water temperature over-high easily destroys some thermally sensitive compositions in essential oil.
Solvent extraction method: under infiltration, diffusion, solvent penetration enters scented plants organization internal, form the inside and outside solute concentration difference of cell and produce osmotic pressure, under the effect of osmotic pressure, extracellular solvent constantly enters in plant tissue, dissolves soluble components, the inside and outside formation concentration difference of cell, make liquid constantly to external diffusion, namely complete once extract until the inside and outside strength of solution of cell reaches running balance.Leach solution, then add novel solvent, until the whole or most of stripping of required composition.Solvent can be the water of strong polarity, also can be wetting ability or lipophilic organic solvent.Compare with milling process with distillation method, solvent extraction complex procedures, essential oil yield is fewer and possibility residual solvent usually.Therefore, in the extraction of the multiplex plant petals of easily degrading in thermo-labile, effective constituent of solvent extration or resin.Solvent extraction method specifically comprises: pickling process, percolation, decocting method, reflux extraction and continuous circumfluence extraction method.
Supercritical CO
2fluids extraction: the superpower dissolving power utilizing supercutical fluid to have, makes fragrant oily substance dissolves, and by the control of pressure and temperature, makes CO
2solvent reaches stagnation point in extraction process, completes the hypercritical transition of liquid phase to gas phase, and obtains the fragrant oily mater of liquid phase.The method purity is high, no solvent residue, is suitable for the extraction of the fragrant oily mater of nonpolar or low-pole mostly, therefore has more application in this area.But the method treatment capacity is lower, facility investment is comparatively large, cost is higher, low to the aromatoising substance extraction yield of low volatility.
Subcritical abstraction method: utilize subcritical fluids as extraction agent, in the container of airtight, anaerobic, low pressure, according to the similar principle that mixes of organism, the molecular diffusion in immersion process by raw material and extraction agent, the fat-soluble component reached in scented plants is transferred in liquid extraction agent, then by the process of reduction vaporization by extraction agent and fragrant oily separating substances.
Aqueous enzymatic method: fully ground by scented plants raw material, destroy the cell walls of raw material, be then soaked in water and make the abundant water-swelling of scented plants, enzyme-added further destruction cell walls, makes the essential oil in cell discharge, then centrifugation obtains essential oil.
Ultrasonic-assisted extraction method: utilize hyperacoustic cavatition, destroy the cell of plant tissue, solvent is made to be easy to infiltrate in cell, simultaneously due to hyperacoustic many secondary actions, as mechanical movement, emulsification, spread, smash, diffusion that chemical effect etc. can also accelerate effective constituent in cell, release and dissolving, thus accelerate the extraction of essential oil.Because ultrasonic extraction is applicable to all kinds of SOLVENTS, extraction rate is fast, and method is simple, and yield is higher, very suitable to the extraction of some case of thermal instability compositions.Possible problem is limited to ultrasonic transducer power, and processing power is large not.
Using microwave-assisted: when utilizing the plant medium microwave energy absorbing in microwave field, because intracellular molecular polarization produces dipole Action of Superhigh Frequency Vibration, friction and heat-dissipating, when after the latent heat gasification that liquid phase scrubbing is enough, break through cell walls disengaged vapor and reach pulverizing object.This is applied widely, and extraction time is short, and percentage extraction is high.Possible problem is that fragrant oily mater is because of overheated and deteriorated.Using microwave-assisted specifically comprises: microwave-assisted wet distillation method, microwave accelerate distillation method, microwave-assisted organic solvent method and Microwave Water diffusion gravity method etc.
In the extracting method of above known various aromatic essential oil, except aqueous enzymatic method, ultrasonic-assisted extraction method and using microwave-assisted relate to except the pulverizing to scented plants, other method does not all carry out pulverization process, to contribute to the stripping smoothly enough in a solvent of fragrant oily substance.
On the other hand, research shows, if by plant superfine grinding to median size about 5 ~ l0 μm, makes its granularity be less than the diameter 10 ~ 100 μm of general vegetable cell, can make degradation rate reach >=95%, realize so-called pulverizing.Therefore, utilize superfine grinding method, the particle size of plant can be made greatly to reduce, and specific surface area significantly increases, and dissolution rate and the extraction yield of fragrant oily mater significantly improve, and also improve the effective rate of utilization of scented plants simultaneously.
In the art, to the solution being dissolved with fragrant oily mater, carry out the vaporization temperature control aspect of gas phase conversion, in known method described above, supercritical carbon dioxide extraction is comprised although take, ultrasonic-assisted extraction, the novel methods such as microwave auxiliary extraction, but " material of the same race has different saturation vapour pressures under not synthermal, and increase along with the rising of temperature, saturation vapour pressure value is higher, more be conducive to liquid phase and become gas phase " evaporating principle and fragrant oily mater " temperature is too high causes deterioration " this to the coordination aspect of contradiction, mostly belong to conventional technological balance, the principle of relative shortage method and apparatus aspect breaks through.
The patent below quoted from wherein some method and apparatus aspect obtains certain success, but this can not to be interpreted as these existing technology be inevitably suitable.
Liu Yu waits by force the Chinese patent CN200510014973.1 of people, disclose a kind of extraction edible volatile plant essence oil Processes and apparatus, technique is: the Plant Powder containing ethereal oil is broken to certain particle size, puts into container, through solvent soaking or without after immersion, put into solvent with certain proportion; Be evaporated in membrane extraction water cooler with extraction solvent at a certain temperature, volatile oil component is concentrated in extraction solvent simultaneously, and the volatile oil after concentrated obtains volatile plant oil finished product after rectification and purification.Equipment comprises: the heating container that plant is soaked and distills, extraction solvent distillation heating container, the thermal insulation of delivery of steam or heating tube, the cooling of liquid film extraction or the liquid film extraction device of condensation, reclaim the partial condenser of condensed fluid, the condenser of cooling extraction solvent and volatile oil, the well heater of accurate control temperature.
Clear Chinese patent application publication No. CN102651978A and the CN103783626A waiting people of hair large bamboo hat with a conical crown and broad brim show, disclose a kind of preparation method and flavouring agent of flavouring agent, by aroma materials and the solvent demonstrating specific solubility parameter, under elevated pressure, extract the operation of the flavour ingredient that aroma materials contains, solvent is be selected from least one solvent in water, alcohols, ketone and ester class.It is excellent and can pay the flavouring agent of the fragrance that diet product etc. have with aroma materials that this preparation method can be extracted in economy aspect high-titer.
The Chinese patent CN201210117126.8 of the people such as Sun great Wen, disclose the extracting method that peel essential oil taken out by a kind of ice crystal broken wall, choose fresh swab exodermis, thickness is 1.5 ~ 2.5mm; To skin oil vacuole layer slow freezing under the environment of-15 ~-30 DEG C be taken out, form ice slag; To tuck inside the sleeve skin ice slag crusher in crushing; Ice slag after fragmentation thaws, and then adopts screw press squeezing, obtains squeezing mixed solution; In squeezing mixed solution, add the salt of 3% ~ 4% quality, decompression stratification, obtains oil-water mixture; Mixed solution underpressure distillation, collects distillate, obtains oil-water mixture, oil-water mixture natural layering, obtain taking out peel essential oil.
The Chinese patent CN201310303360.4 of the people such as Wang Juan, disclose a kind of extracting process of plants essential oil, comprise the techniques such as allotment, expanded, extraction, puffing technique is utilized to combine with other techniques, improve the textural property of plant material, derived essential oil is easily overflowed, the overcritical or subcritical abstraction of follow-up employing intensified by ultrasonic wave, obtain plants essential oil.
The Chinese patent CN201310080571.6 of the people such as Yu Xinhai, disclose a kind of extraction element of effective ingredients in plant, comprise the end cap of homogenate equipment tank body and the setting of its upper end, end cap and homogenate equipment tank body are by C-type clamp and gasket seal, end cap is provided with loading hopper, anchor stirrer, high shear agitation device and ultrasonic generator; The probe of the stirring rake of anchor stirrer, high shear agitation device and ultrasonic generator all stretches into from described end cap in the working chamber of homogenate equipment tank body; Anchor stirrer comprises for it provides the motor of power, rotation axis and stirring rake, and high shear agitation device and ultrasonic generator are popped one's head between stirring rake and transmission shaft; Rotation axis is provided with dismountable blade.
The Chinese patent application publication No. CN103740467A of Lu Yan, discloses a kind of extracting method of plants essential oil, comprises step: by plant material freezing 1 ~ 8 day of subzero less than 10 degrees Celsius temperature; Plant material under freezing state is crushed to the particulate of below 1 mm dia; Particulate is added in the liquid normal butane of subzero 4 degrees Celsius to subzero 0.5 degree Celsius and fully stir, and keep this temperature 0.5 ~ 3 hour; At the temperature of subzero 4 degrees Celsius to subzero 0.5 degree Celsius, pass into ultrasonic wave, and regulate hyperacoustic power to normal butane boiling, and keep 1 ~ 5 hour; Filter and leave standstill, after solution layering, extracting supernatant liquid.
The Chinese patent application publication No. CN103897805A of Wei Weihong, disclose a kind of Solventless Extraction Process of lemon quintessence oil, comprise step: pulverized by clean Fresh Lemon pericarp, or pulverize after clean lemon dry fruit skin water-wet, obtain lemon pericarp fragment; Lemon pericarp fragment is placed in microwave extracting apparatus, microwave radiation is applied to lemon pericarp fragment, collect the essential oil steam condensation that produce, obtain thick lemon quintessence oil; Applying the mode of microwave radiation is intermittent type, and its process is: carry out interval after a microwave radiation processing, then carry out microwave radiation processing next time, repeat operation; Isolate the impurity in thick lemon quintessence oil, obtain lemon quintessence oil.
The Chinese patent application publication No. CN103897806A of the people such as Wei Weihong, discloses a kind of microwave auxiliary extracting method of lemon quintessence oil, comprises step: cleaned up by lemon pericarp, then carries out drying treatment and pulverize, and obtains lemon fruit peel powder; Lemon fruit peel powder is placed in non-metallic container, and adds water and salt in non-metallic container, be placed in microwave extracting apparatus, then by the extremely boiling of the heating material in non-metallic container; After material boiling, microwave radiation is applied to the material in non-metallic container, collect the steam condensation that produce, obtain thick lemon quintessence oil; The mode applying microwave radiation is intermittent type; Isolate the water in thick lemon quintessence oil and impurity, obtain lemon quintessence oil.
Known based on above analysis, in the art, still there is no a kind of wet grinding technique at present, its force mechanism pulverized not only has mill stripping and smashes effect, have the direct broken cells of stretching action simultaneously concurrently, and realize by the saturation vapour pressure value improving solution rete the method that low-temperature distillation extracts fragrant oily mater.Therefore, expecting to provide a kind of by adopting the pulverizing force mechanism suitable to scented plants raw material, making scented plants cell obtain abundant broken wall, to improve the solubleness of fragrant oily mater, on this basis, the solution of fragrant oily mater will be dissolved with, be dispersed into uniform thin film layer, to utilize Clausius-carat amber dragon (ClausiusClapeyron) equation principle, improve the saturation vapour pressure value of thin film layer solution, and pass through the collaborative depressurization of the decompression of fluid speedup and vacuum take-off, the solution making to be dissolved with fragrant oily mater is gas phase by liquid-phase conversion at a lower temperature, realize the high-efficiency evaporating of fragrant oily mater, finally by efficient condenser and separator, prepare the high-quality plants essential oil fragrance realizing pulverizing and distillation extraction with pure physical method.
Summary of the invention
The technical problem to be solved in the present invention is, provides a kind of nappe flip length and centrifugal film decompression low-temperature distillation to extract the method for plants essential oil fragrance, realizes the high-quality plants essential oil fragrance of pulverizing and distillation extraction with pure physical method.
The technical solution adopted for the present invention to solve the technical problems is: a kind of method constructing nappe flip length and centrifugal film decompression low-temperature distillation extraction plants essential oil fragrance, comprises the following steps:
S1, the extraction raw material of plants essential oil fragrance after pulverizing is joined in stirred pot, add after water stirs and deliver to separating centrifuge;
S2, the heavies after being separated is delivered to water fluid jet grind and carries out nappe flip length;
S3, the light materials solution that described step S2 obtains is delivered to the low-temperature evaporation device upper end charging opening that multilayer disc-stack centrifuge and gravity film forming and differential reduce pressure, described low-temperature evaporation device comprises cone of revolution video disc and the fixed axoid video disc of coaxial alternate lamination setting, wherein, cone of revolution video disc is fixing rotates on center shaft; Light materials solution, from the cone of revolution video disc of the superiors, successively flow to undermost fixed axoid video disc; The lower end sidepiece of the low-temperature evaporation device that hot gas flow then reduces pressure from described multilayer disc-stack centrifuge and gravity film forming and differential enters, and with lightweight thing solution stream to doing countercurrent flow, successively rise, period flows through the tapered annular gap that cone of revolution video disc and fixed axoid video disc are formed, with solution rete generation heat exchange, the fragrant oily mater of liquid phase is evaporated to gas phase;
S4, gas phase fragrance oily mater, with steam, is sucked and enters condenser, and be condensed into liquid together with water vapor; Again by separator make fragrant oily mater and condensed moisture from, obtain liquid plants essential oil fragrance.
In such scheme, for the water fluid jet grind of plant superfine grinding, by the impact of high-pressure water jet, water wedge tension force, cavitation abtragung, make flower, really, the superfine grinding granularity of leaf, branch, skin, root or the scented plants such as subterraneous stem, seed raw material reaches median size and be about < 5 ~ l0 μm, the polar component being beneficial to fragrant oily mater is soluble in water, simultaneously, under the turbulent flow emulsifying effect that high-pressure water jet is violent, nonpolar (oiliness or the fat) composition being also conducive to fragrant oily mater is soluble in water.
In such scheme, described a kind of water fluid jet grind for plant superfine grinding, closed-circuit pulverization and separating circuit is formed with separating centrifuge, high pressure plunger pump and transferpump, the heavies (containing coarse particles) that separating centrifuge is separated is returned the described water fluid jet grind for plant superfine grinding, carries out continuous circulation pulverizing; By lightweight thing solution (containing fragrant oily mater and the fine scented plants particle) high pressure plunger pump of making a gift to someone that separating centrifuge is separated, recycle as working medium, until the subparticle in the described lightweight thing solution of separating centrifuge separation, granularity reaches median size when being about < 5 ~ l0 μm, described lightweight thing solution is switched out closed-circuit pulverization and separating circuit, and is transported to next stage and carries out vaporize draw.
In such scheme, at the cone of revolution video disc of described lightweight thing solution from the superiors, alternately flow in the process of undermost fixed axoid video disc, successively form even rete, and with rise hot gas flow generation heat exchange, fragrant oily mater in described lightweight thing solution is evaporated to gas phase, and described heat exchange temperature within the scope of 25 ~ 95 DEG C, and adjusts by hot gas flow flow.
In such scheme, described lightweight thing solution, is first transported into evaporation slip preheater, is preheated within the scope of 25 ~ 55 DEG C, and adjust by hot gas flow flow, then be transported to the low-temperature evaporation device that described multilayer disc-stack centrifuge and gravity film forming and differential reduce pressure and carry out vaporize draw.
In such scheme, by vacuum pump set, the gas phase fragrance oily mater evaporated by the low-temperature evaporation device that described multilayer disc-stack centrifuge and gravity film forming and differential reduce pressure, with water vapor, is sucked and enters condenser, and be condensed into liquid together with water vapor; Again by separator, make fragrant oily mater and condensed moisture from, obtain liquid plants essential oil fragrance, the vacuum tightness of vacuum pump set is 0.035 ~ 0.095MPa.
In such scheme, described lightweight thing solution, after the evaporation concentration of the low-temperature evaporation device reduced pressure by described multilayer disc-stack centrifuge and gravity film forming and differential, then is cooled to normal temperature via enriching slurry water cooler, the cooled solution of evaporation concentration, makes foodstuff additive etc. by processing purification.
In such scheme, to the branch in scented plants raw material, skin, root or subterraneous stem, seed, granularity < 6 order (3.35mm) is crushed to by plant pulverizer, to the flower in scented plants raw material, really, leaf, size < 2 order (8mm) is become by cutting and grinding powder mode size degradation, join in stirred pot, again by solid-to-liquid ratio 1:(2 ~ 8) add water, impregnated raw material 20 ~ 120min at normal temperatures, period agitator with linear velocity 0.2 ~ 1m/s continuously or intermittent stirring; By the swelling good raw material of dipping, by slurry transferring pump delivery to described separating centrifuge, the heavies after separation is transported to the described water fluid jet grind for plant superfine grinding; Lightweight thing solution after separation, is transported to high pressure plunger pump, recycles as working medium.
In such scheme, in discharge adapter place of the described water fluid jet grind for plant superfine grinding, separator is set, by the aromatic plant volatility aroma component produced in nappe flip length process, directly be delivered to the condenser and separator that are arranged in the low-temperature evaporation device back segment that described multilayer disc-stack centrifuge and gravity film forming and differential reduce pressure, trap in the lump with fragrant oily mater.
In such scheme, when lightweight thing solution switches out closed-circuit pulverization and separating circuit, described heavies after separating centrifuge is separated, switch out closed-circuit pulverization and separating circuit simultaneously, be delivered to filter dehydration device, dehydration obtains the slag charge be made up of scented plants fibrous particle afterwards and can be fully utilized, as feed, or as the starting material etc. of stacte goods.
Implement the method for nappe flip length of the present invention and centrifugal film decompression low-temperature distillation extraction plants essential oil fragrance, there is following beneficial effect:
The present invention carries out pulverizing by water fluid jet grind to plant and pulverizes, to improve the solubleness of fragrant oily mater; And utilize the cryogenic distillation that multilayer disc-stack centrifuge and gravity film forming and differential reduce pressure, the Solution Dispersion uniformly thin film layer of fragrant oily mater will be dissolved with, to improve the saturation vapour pressure value of thin film layer solution, and by fluid differential decompression and the collaborative depressurization of vacuum take-off, make the solution high-efficiency evaporating being at a lower temperature dissolved with fragrant oily mater, finally by efficient condenser and separator, prepare the plants essential oil fragrance realizing pulverizing and distillation extraction with pure physical method.
Accompanying drawing explanation
Below in conjunction with drawings and Examples, the invention will be further described, in accompanying drawing:
Fig. 1 is the method technical process exemplary schematic illustration that a kind of nappe flip length and centrifugal film decompression low-temperature distillation extract plants essential oil fragrance;
Fig. 2 is the main pseudosection of the low-temperature evaporation device that multilayer disc-stack centrifuge and gravity film forming and differential reduce pressure;
Fig. 3 is the part sectioned view of cone of revolution disc stack;
Fig. 4 is the upward view of cone of revolution disc stack;
Fig. 5 is the part sectioned view of fixed axoid disc stack;
Fig. 6 is the upward view of fixed axoid disc stack;
Fig. 7 is the main pseudosection of water fluid jet grind for plant superfine grinding;
Fig. 8 is the vertical view of the water fluid jet grind for plant superfine grinding;
Fig. 9 is the A-A sectional view in Fig. 7;
Figure 10 is the main pseudosection of top charging hierarchy;
Figure 11 is the C direction view in Figure 10;
Figure 12 is the main pseudosection that lower nozzle pulverizes structure;
Figure 13 is the B direction view in Figure 12.
Embodiment
In order to there be understanding clearly to technical characteristic of the present invention, object and effect, now contrast accompanying drawing and describe the specific embodiment of the present invention in detail.
As shown in Figure 1, a kind of nappe flip length provided by the invention and centrifugal film decompression low-temperature distillation extract the method for plants essential oil fragrance, its technical process and set device comprise: stirred pot 0101, plant pulp material conveying pump 0102, high pressure plunger pump 0103, for the water fluid jet grind 0104 of plant superfine grinding, pulverize slurry transferring pump 0105, pulverize slip separator 0106, flowrate control valve 0107, separating centrifuge 0108, filter dehydration device 0109, evaporation slip preheater 0110, enriching slurry water cooler 0111, the low-temperature evaporation device 0112 that multilayer disc-stack centrifuge and gravity film forming and differential reduce pressure, condenser 0113, separator 0114, vacuum pump set 0115, handpiece Water Chilling Units 0116, hot gas device 0117.
Processing step and the main technologic parameters of the method for described a kind of nappe flip length and centrifugal film decompression low-temperature distillation extraction plants essential oil fragrance are as follows:
Step 1: to the branch in scented plants raw material, skin, root or subterraneous stem, seed, granularity < 6 order (3.35mm) is crushed to by plant pulverizer, to the flower in scented plants raw material, really, leaf, size < 2 order (8mm) is become by cutting and grinding powder mode size degradation, join in stirred pot 0101, again by solid-to-liquid ratio 1:(2 ~ 8) add water, impregnated raw material 20 ~ 120min at normal temperatures, period agitator with linear velocity 0.2 ~ 1m/s continuously or intermittent stirring; By the swelling good raw material of dipping, be delivered to separating centrifuge 0108 by plant pulp material conveying pump 0102, the heavies (containing raw material coarse particles) after separation is transported to the described water fluid jet grind 0104 for plant superfine grinding; Lightweight thing (containing fragrant oily mater and fine scented plants particle) solution after separation, is transferred people's high pressure plunger pump 0103, recycles as working medium.
Step 2: the heavies after separation is taken over via charging, enters the described tubular crushiing chamber of flat ring for the water fluid jet grind 0104 of plant superfine grinding, carries out nappe flip length, slurry after pulverizing, by pulverizing slurry transferring pump 0105, is sucked via discharge adapter and discharges the described water fluid jet grind 0104 for plant superfine grinding, then is delivered to separating centrifuge 0108 and is separated, by this process, heavies after separating centrifuge 0108 is separated, by high pressure plunger pump 0103, the described water fluid jet grind 0104 for plant superfine grinding, separating centrifuge 0108 is with in the closed-circuit pulverization pulverizing the formation of slurry transferring pump 0105 and separating circuit, acquisition continuous circulation is pulverized, until the subparticle in lightweight thing solution after being separated by separating centrifuge 0108, granularity reaches median size when being about the setting index of < 5 ~ l0 μm, by flowrate control valve 0107, lightweight thing solution is switched out closed-circuit pulverization and separating circuit, and be transported into evaporation slip preheater 0110.
The pulverizing pressure of the nozzle of the described water fluid jet grind 0104 for plant superfine grinding is 5 ~ 20MPa, preferably, 7 ~ 12MPa, the back pressure of the tubular crushing chamber of flat ring within the scope of 0.010 ~ 0.040MPa, preferably, 0.02 ~ 0.03MPa.
By pulverizing slip separator 0106, will directly be delivered to the condenser 0113 and separator 0114 trapping that are arranged in evaporation unit back segment at the described aroma volatile being used for producing in water fluid jet grind 0104 crushing process of plant superfine grinding.
When lightweight thing solution being switched out closed-circuit pulverization and separating circuit by flowrate control valve 0107, heavies after separating centrifuge 0108 is separated, switch out closed-circuit pulverization and separating circuit simultaneously, be delivered to filter dehydration device 0109, dehydration obtains the slag charge be made up of scented plants fibrous particle afterwards, can be fully utilized, as feed, or as the starting material etc. of stacte goods.
Step 3: the lightweight thing solution obtained by step 2, be transported into evaporation slip preheater 0110, make lightweight thing solution be preheated to 25 ~ 55 DEG C, the temperature within the scope of this is adjustable; Lightweight thing solution after preheating, then the low-temperature evaporation device 0112 upper end charging opening being transported to that described multilayer disc-stack centrifuge and gravity film forming and differential reduce pressure, from the cone of revolution video disc of the superiors, successively flow to undermost fixed axoid video disc; The lower end sidepiece of the low-temperature evaporation device 0112 that hot gas flow then reduces pressure from described multilayer disc-stack centrifuge and gravity film forming and differential enters, and with lightweight thing solution stream to doing countercurrent flow, successively rise, period flows through the tapered annular gap that cone of revolution video disc and fixed axoid video disc are formed, with solution rete generation heat exchange, temperature controls, within the scope of adjustable 25 ~ 95 DEG C, the fragrant oily mater of liquid phase to be evaporated to gas phase.
The fragrant oily mater of gas phase is with steam, under the suction function of vacuum pump set 0115, discharge via upper end pump orifice the low-temperature evaporation device 0112 that described multilayer disc-stack centrifuge and gravity film forming and differential reduce pressure, the vacuum tightness of vacuum pump set 0115 is 0.035 ~ 0.095MPa.
The gas phase fragrance oily mater of discharging the low-temperature evaporation device 0112 that described multilayer disc-stack centrifuge and gravity film forming and differential reduce pressure, with steam, is sucked and enters condenser 0113, and be condensed into liquid together with water vapor; Again by separator 0114, make fragrant oily mater and condensed moisture from, obtain liquid plants essential oil aroma component.
Solution after evaporation concentration, the lower end of the low-temperature evaporation device 0112 reduced pressure via described multilayer disc-stack centrifuge and gravity film forming and differential is discharged, normal temperature is cooled to again by enriching slurry water cooler 0111, the cooled solution of evaporation concentration, there is containing some the non-volatile plants essential oil component of low saturation vapour pressure value, make foodstuff additive etc. by processing purification.
Handpiece Water Chilling Units 0116 provides cooling fluid, cooling temperature scope 0.5 ~ 8 DEG C for condenser 0113 and enriching slurry water cooler 0111.
The low-temperature evaporation device 0112 that hot gas device 0117 reduces pressure for evaporation slip preheater 0110 and described multilayer disc-stack centrifuge and gravity film forming and differential provides hot gas flow, temperature range 85 ~ 110 DEG C.
The low-temperature evaporation device that the described water fluid jet grind for plant superfine grinding and described multilayer disc-stack centrifuge and gravity film forming and differential reduce pressure, and in extraction system, be configured with situ cleaning CIP device and the measure of steam high-temperature sterilization.
As shown in Figure 2, the low-temperature evaporation device 0112 that multilayer disc-stack centrifuge and gravity film forming and differential reduce pressure, its structure comprises: feed liquid feed socket 1201, head bearing assembly 1202, upper set ring 1203, feed liquid nozzle 1204, cone of revolution disc stack 1205, fixed axoid disc stack 1206, cylindrical shell 1207, lower location fixed axoid video disc 1208, support cylindrical shell 1209, concentrated solution collection bucket 1210, concentrated solution discharge adapter 1211, lower bearing component 1212, vaporised gas derives adapter 1213, cylinder top cover 1214, temperature sensor 1215, tightening round nut 1216, upper positioning shaft sleeve 1217, central shaft 1218, hot gas flow imports adapter 1219, lower positioning shaft sleeve 1220, dish 1221 shed by concentrated solution, steam condensate outlet connection 1222, drive pulley 1223.
As shown in Figure 3 and Figure 4, cone of revolution disc stack 1205 is made up of cone of revolution video disc 12051, cone of revolution video disc blade 12052 and cone of revolution video disc set ring 12053, the quantity of cone of revolution video disc blade 12052 is 4 ~ 16, in the present embodiment preferably, and 6.
As shown in Figure 5 and Figure 6, fixed axoid disc stack 1206 is made up of fixed axoid video disc 12061, fixed axoid video disc blade 12062 and fixed axoid video disc set ring 12063, the quantity of fixed axoid video disc blade 12062 is 6 ~ 24, in the present embodiment preferably, and 8.
As shown in Fig. 2 ~ Fig. 6, the outside diameter of the fixed axoid video disc set ring 12063 on fixed axoid disc stack 1206 is D0; Interior Circular Aperture on fixed axoid video disc 12061 on fixed axoid disc stack 1206 is D1; The height of fixed axoid disc stack 1206 is GH; The height of fixed axoid video disc set ring 12063 is Gh; Cone of revolution video disc 12051 upper end outside diameter on cone of revolution disc stack 1205 is D2; End outside diameter bored by cone of revolution video disc 12051 on cone of revolution disc stack 1205 is D3, and the height of cone of revolution disc stack 1205 is ZH, and the height of cone of revolution video disc set ring 12053 is Zh; Cylindrical shell 1207 height is H with the thickness sum of cylinder top cover 1214, and the height of support cylindrical shell 1209 is h; The angle of cone of revolution video disc 12051 and fixed axoid video disc 12061 conical surface and central shaft 1218 axis is β.
As shown in Fig. 2 ~ Fig. 6, feed liquid feed socket 1201 is welded on the eccentric position of cylinder top cover 1214, and feed liquid feed socket 1201 lower end is connected by pipe thread seal with feed liquid nozzle 1204; Head bearing assembly 1202 axis and cylinder top cover 1214 axis coaxle are arranged, and are connected by bolt seal, and central shaft 1218 upper end is nested in head bearing assembly 1202 in dynamic cooperation assembling mode; Cone of revolution video disc 1205 passes through cone of revolution video disc set ring 12053 with central shaft 1218 with splined, and located vertically by cone of revolution video disc set ring 12053, cone of revolution disc stack 1205 forms integrative-structure by cone of revolution video disc 12051, cone of revolution video disc blade 12052 and cone of revolution video disc set ring 12053 by welding process; Fixed axoid disc stack 1206 passes through fixed axoid video disc set ring 12063 kink in cylindrical shell 1207 inwall, neighbouring fixed axoid disc stack 1206 is with the locator means of steady brace, make the axis of all fixed axoid disc stacks 1206 of lamination coaxial with central shaft 1218, and locate vertically by fixedly turning conical surface video disc set ring 12063, fixed axoid video disc 1206 forms integrative-structure by fixed axoid video disc 12061, fixed axoid video disc blade 12062 and fixed axoid video disc set ring 12063 by welding process; Cylindrical shell 1207 can be divided into 2 ~ 4 sections, is connected by flange and bolt seal; Vaporised gas is derived adapter 1213 and is welded on the eccentric position of cylinder top cover 1214, and cylinder top cover 1214 is connected by bolt seal with the upper flange of cylindrical shell 1207; Concentrated solution collection bucket 1210 and concentrated solution discharge adapter 1211 form integrative-structure with support cylindrical shell 1209 by welding process; Hot gas flow imports adapter 1219 and is welded on support cylindrical shell 1209 sidewall, and steam condensate outlet connection 1222 is welded on bottom support cylindrical shell 1209; Lower bearing component 1212 axis and support cylindrical shell 1209 axis coaxle are arranged, and be connected in bottom support cylindrical shell 1209 by bolt seal, central shaft 1218 lower end is nested in lower bearing component 1212 in dynamic cooperation assembling mode, and drive pulley 1223 is by the axle head of Flat dey joint at central shaft 1218.
As shown in Figure 2, assemble successively in the following order: central shaft 1218 lower end is nested in lower bearing component 1212 in dynamic cooperation assembling mode; Concentrated solution is shed dish 1221 to be inserted in central shaft 1218 spline keyway, be pressed in lower center axle 1218 shaft shoulder place; Lower positioning shaft sleeve 1220 is inserted in central shaft 1218 spline keyway, is pressed in concentrated solution and sheds on dish 1221; Lower location fixed axoid video disc 1208 is pressed in the flange seam of support cylindrical shell 1209 and locates; Cone of revolution disc stack 1205 is inserted in central shaft 1218 spline keyway, is pressed on lower positioning shaft sleeve 1220; Fixed axoid disc stack 1206 is pressed on lower location fixed axoid video disc 1208, again another cone of revolution disc stack 1205 is inserted in central shaft 1218 spline keyway, be pressed on cone of revolution disc stack 1205 below, alternately assemble each cone of revolution disc stack 1205 and fixed axoid disc stack 1206 in this way; Be inserted in central shaft 1218 spline keyway until be assembled to upper positioning shaft sleeve 1217 topmost, will all parts lockings in central shaft 1218 spline keyway be inserted in by tightening round nut 1216; Fixed axoid disc stack 1206 is topmost compressed by upper set ring 1203 and cylinder top cover 1214, and central shaft 1218 upper end is nested in head bearing assembly 1202 in dynamic cooperation assembling mode.
As shown in Fig. 2 ~ Fig. 6, when the outside diameter of the fixed axoid video disc set ring 12063 on fixed axoid disc stack 1206 is D0, interior Circular Aperture on fixed axoid video disc 12061: D1=(0.150 ~ 0.450) × D0, in the present embodiment preferably, D1=0.314D0; The height of fixed axoid disc stack 1206: GH=(0.150 ~ 0.350) × D0, in the present embodiment preferably, GH=0.265D0; The height of fixed axoid video disc set ring 12063: Gh=(0.080 ~ 0.250) × D0, in the present embodiment preferably, Gh=0.149D0; Cone of revolution video disc 12051 upper end outside diameter: D2=(0.550 ~ 0.980), in the present embodiment preferably, D2=0.843D0; End outside diameter bored by cone of revolution video disc 12051: D3=(0.140 ~ 0.550) × D0, in the present embodiment preferably, and D3=0.0.299D0; The height of cone of revolution disc stack 1205: ZH=(0.120 ~ 0.380) × D0, in the present embodiment preferably, ZH=0.243D0; The height of cone of revolution video disc set ring 12053: Zh=(0.090 ~ 0.240) × D0, in the present embodiment preferably, Zh=0.138D0; Cylindrical shell 1207 height and the thickness sum of cylinder top cover 1214: H=(2.00 ~ 4.00) × D0, in the present embodiment preferably, H=2.97D0; The height of support cylindrical shell 1209 is h=(0.500 ~ 2.00) × D0, in the present embodiment preferably, and h=0.838D0; The angle of cone of revolution video disc 12051 and fixed axoid video disc 12061 conical surface and central shaft 1218 axis is β=30 ° ~ 60 °, in the present embodiment preferably, and β=47 °.
Central shaft 1218 speed range 200 ~ 1450r.p.m., by variable-frequency motor or servomotor speed regulating control; The temperature range that temperature sensor 1215 measures is 25 ~ 120 DEG C, and the hot stream temperature passed into by hot gas flow importing adapter 1219 and Flow-rate adjustment control; The vacuum tightness that vaporised gas derives adapter 1213 place is 0.035 ~ 0.095MPa, is controlled by vacuum pump set adjustment.
As shown in Figure 7, water fluid jet grind 0104 for plant superfine grinding comprises: top charging hierarchy 041, structure 042 is pulverized with lower nozzle, top charging hierarchy 041 and lower nozzle are pulverized structure 042 and are connected by bolt seal, and form the tubular crushing chamber 0424 of flat ring and blade classification impact ring 0414 structure, wherein, the tubular crushing chamber 0424 of flat ring comprises multi-nozzle and converges disintegrating area, and uniform nozzle multiple spot tangential impact disintegrating area.
As shown in Fig. 7 ~ Figure 13, the outer diameter of the tubular crushing chamber 0424 of flat ring is D0, the inner diameter of the tubular crushing chamber 0424 of flat ring is D1, feed opening 0415 center circle diameter is D2, lower substrate outside diameter is D3, it is D4 that ring 0414 internal diameter is impacted in blade classification, and charging adapter 0411 internal diameter is Din, and discharge adapter internal diameter is Dout.
As shown in Fig. 7 ~ Figure 11, top charging hierarchy 041, by charging adapter 0411, discharge adapter 0412, upper matrix 0413, ring 0414 is impacted in blade classification and feed opening 0415 is formed, wherein, blade classification impact ring 0414 is made up of convergence jet impact wall 0414a, uniform jet impact wall 0414b and tangential vane 0414c.
As shown in Figure 10 and Figure 11, charging adapter 0411 is connected by bolt seal with upper matrix 0413, and charging adapter 0411 position is determined by feed opening 0415 center circle diameter D2, D2=(0.80 ~ 0.87) × D0, preferably, and D=0.84D0; Charging adapter 0411 diameter Din=(0.2 ~ 0.4) × (D0-D1), preferably, Din=0.23 × (D0-D1), D0 span 300 ~ 1160mm.
As shown in Fig. 7, Figure 12 and Figure 13, the inner diameter of the tubular crushing chamber 0424 of flat ring is D1 is D1=(0.55 ~ 0.75) × D0, preferably, and D1=0.64D0.
As shown in Figure 10 and Figure 11, discharge adapter 0412 is positioned at the center of matrix 0413 circle, and with upper matrix by being welded to connect, discharge adapter 0412 diameter Dout=(0.12 ~ 0.16) × D0, preferably, Dout=0.13D0.
As shown in Fig. 9, Figure 10 and Figure 11, it is one-piece construction that blade classification impacts ring 0414 with upper matrix 0413, and ring 0414 internal diameter D4=(0.45 ~ 0.65) × D0 is impacted in blade classification, preferably, and D4=0.54D0; The arc length angle 40 ° ~ 54 ° of the convergence jet impact wall 0414a on ring 0414 is impacted in blade classification, preferably, 48 °, and from there is the axis of different convergence nozzle 0423a, 0423b, 0423c and 0423d of cutting angle, touch low-angle tangent with wide-angle; The uniform jet impact wall 0414b that blade classification is impacted on ring 0414 is corresponding tangent with uniform nozzle 0423 axis, uniform jet impact wall 0414b arc length angle 16 ° ~ 20 °, preferably, and 18 °; Tangential vane 0414c on blade classification impact ring 0414 cuts angle 25 ° ~ 50 °, preferably, 30 °, tangential vane 0414c setting area arc length angle 42 °, the tangential vane 0414c setting area arc length angle 72 ° of next-door neighbour's feed opening 0415; Tangential vane 0414c height h=(2.8 ~ 3.5) × (D0-D1), preferably, h=3.1 × (D0-D1); The blade passage wavelength width of a slit of two alternate formations of tangential vane 0414c is 3 ~ 6mm, preferably, and 4mm.
As shown in Fig. 9, Figure 12 and Figure 13, lower nozzle pulverizes structure 042, by nozzle plug 0421, annular high voltage water distribution room 0422, converge nozzle 0423a, 0423b, 0423c and 0423d, uniform nozzle 0423, and the tubular crushing chamber 0424 of flat ring, pressure transmitter 0425, lower substrate 0426 and high pressure water access tube 0427 are formed.
As shown in Figure 9, converging nozzle 0423a and horizontal axis angle is 10 ° ~ 20 °, preferably, 15 °, the neighbour angle between convergence nozzle 0423b, 0423c and 0423d be 17 ° ~ 25 ° preferably, 20 °; The β that cuts angle of uniform nozzle 0423 is 50 ° ~ 75 °, preferably, and 62 °; Converge nozzle and uniform nozzle, be connected in lower substrate 0422 by thread seal; High pressure water access tube 0427 is welded on lower substrate 0426 cylindrical sidewall, and communicates with annular high voltage water distribution room 0422.
As shown in figs. 7 and 13, the cross section of fluid channel size of the tubular crushing chamber 0424 of flat ring: width B=0.5 × (D0-D1), height H=(0.15 ~ 0.35) × (D0-D1), preferably, H=0.2 (D0-D1).
Convergence nozzle is 3 ~ 7 throat diameters is 0.7 ~ 2.5mm High pressure water jet nozzle, and preferably, convergence nozzle is 4 throat diameters is the High pressure water jet nozzle of 1mm; Multiple uniform nozzle is 4 ~ 9 throat diameters is the High pressure water jet nozzle of 0.7 ~ 2.5mm, and preferably, convergence nozzle is 4 throat diameters is 1mm High pressure water jet nozzle.
The pulverizing pressure of High pressure water jet nozzle is 5 ~ 30MPa, preferably, and 7 ~ 12MPa.
The present invention utilizes the water fluid jet grind being used for plant superfine grinding to carry out pulverizing to scented plants and pulverizes, to improve the solubleness of fragrant oily mater; And utilize the low-temperature evaporation device that multilayer disc-stack centrifuge and gravity film forming and differential reduce pressure, the Solution Dispersion uniformly thin film layer of fragrant oily mater will be dissolved with, to improve the saturation vapour pressure value of thin film layer solution, and by fluid differential decompression and the collaborative depressurization of vacuum take-off, make the solution high-efficiency evaporating being at a lower temperature dissolved with fragrant oily mater; Configured by the coupling technique of the special low-temperature evaporation apparatus design reduced pressure for the described water fluid jet grind for plant superfine grinding and described multilayer disc-stack centrifuge and gravity film forming and differential and supplementary unit, form a set of plants essential oil fragrance extraction system.
By the described water fluid jet grind for plant superfine grinding, by the extraction raw material of plants essential oil fragrance, the i.e. flower of scented plants, really, leaf, branch, skin, root or subterraneous stem, seed etc., under the impact of high-pressure water jet and water wedge tension force and cavitation abtragung, superfine grinding to median size is about < 5 ~ l0 μm, make diameter about the cell wall damage of the various scented plants cells of 10 ~ 100 μm of size ranges, the polar component being not only conducive to fragrant oily mater is soluble in water, and under the violent turbulent flow emulsifying effect of high-pressure water jet, also nonpolar (oiliness or the fat) composition being conducive to fragrant oily mater is soluble in water.
Because the described water fluid jet grind for plant superfine grinding is working medium with water, if in crushing process, from extraction system, supplement work Jie water continuously by high pressure plunger pump, then can cause the too dilution of fragrant oily mater and affect distillation efficiency.To this, extraction system is configured with separating centrifuge, high pressure plunger pump, the described water fluid jet grind for plant superfine grinding, separating centrifuge and transferpump is made to form closed-circuit pulverization and separating circuit, the heavies (containing coarse particles) that separating centrifuge is separated is returned the described water fluid jet grind for plant superfine grinding, carries out continuous circulation pulverizing; By lightweight thing (containing fragrant oily mater and the fine scented plants particle) high pressure plunger pump of making a gift to someone that separating centrifuge is separated, recycle as working medium, until the granularity of lightweight thing that separating centrifuge is separated reaches median size when being about < 5 ~ l0 μm, be transported into interchanger preheating with the form of wet colloidal sol, then be admitted to the low-temperature evaporation device upper end charging opening that multilayer disc-stack centrifuge and gravity film forming and differential reduce pressure and carry out evaporation process.
Because vegetable particle size contained in work Jie water is small, and almost without abrasiveness, therefore the supercharging push rod wearing and tearing that high pressure plunger pump is principle of work with simple linear re-ciprocating motion can not be caused, and doping contact scar is produced to solution.Water fluid jet grind heats up very little in crushing process, can not produce heat affecting to fragrant oily mater.
In nappe flip length process, some in scented plants are easy to the fragrant molecule of escaping from liquid phase, volatilization is produced due to the impact of high-pressure water jet and cavatition, therefore gas-liquid separator is set in discharge adapter place of the described water fluid jet grind for plant superfine grinding, this part aroma volatile is directly delivered to the condensation and gas-liquid separation device that are arranged in evaporation unit back segment, traps in the lump with plants essential oil fragrance.
Extract as fragrant oily mater the flower of the scented plants of raw material, really, leaf, branch, skin, root or subterraneous stem, seed etc., before the described water fluid jet grind for plant superfine grinding is pulverized, first in stirred pot, use water retting, vegetable fibre is produced certain swelling, the pulverizing so that water fluid jet grind is efficiently loosened.
By the flower to scented plants, really, for some time of leaf, branch, skin, root or the raw material such as subterraneous stem, seed pulverizes and the stripping process of fragrant oily mater, the heavies (containing coarse particles) be separated via separating centrifuge is admitted to filter dehydration device and carries out solid-liquid separation, the slag charge of gained can be fully utilized, as as feed, or as the starting material etc. of stacte goods.
The low-temperature evaporation device that described multilayer disc-stack centrifuge and gravity film forming and differential reduce pressure, has revolution and the fixing coaxial alternate lamination of two groups of conical surface video discs arranges structure, and wherein, cone of revolution video disc is fixing to rotate on center shaft.When on solution to be injected into the cone of revolution video disc of the superiors internal surface by upper end charging opening, under centrifugal action, solution sprawls uniformly thin film layer on an internal surface, and is thrown to cone of revolution video disc cylindrical in the mode of continuous flow; Flow under the influence of gravity into the cylindrical place of the lower one deck fixed axoid video disc internal surface alternate with it, and collect along the conical surface and flow to fixed axoid video disc inner circle, in the process, solution under gravity, still in the mode of continuous flow at the uniform thin film layer of fixed axoid video disc internal surface upper berth generate; Collect the solution flowing to fixed axoid video disc inner circle, continue the inner circle fallen on the internal surface of lower one deck cone of revolution video disc alternate with it, in this way, solution, under centrifugal force and weight effect, alternately forms even rete in revolution and two groups of fixing conical surface video disc internal surfaces.
According to Clausius-Clapeyron equation principle, liquid rete is thinner, and film temperature gradient is less, is heated more even, more level off to evaporitic environment temperature, therefore relative to thick film layers, the saturation vapour pressure value of its liquid improves, and namely thin film layer solution is more easily evaporated into gas, simultaneously, rete quantity is more, and specific surface area is larger, and steam output is larger.Therefore, the low-temperature evaporation device that described multilayer disc-stack centrifuge and gravity film forming and differential reduce pressure, by alternately forming even rete in revolution and two groups of fixing a fairly large number of conical surface video disc internal surfaces, improves the vaporization efficiency of fragrant oily mater.
On the outside surface of revolution and two groups of fixing conical surface video discs, be respectively provided with one group of uniform blade; When cone of revolution video disc rotates with central shaft, blade on cone of revolution video disc outside surface, because of the viscous force effect of gas, the gas that fixed axoid video disc internal surface contacts with solution film layer is driven to do swirling motion, make the gas on the solution film layer surface on fixed axoid video disc internal surface, produce a slip speed relative to the blade on cone of revolution video disc outside surface; Simultaneously, when cone of revolution video disc rotates with central shaft, the gas that cone of revolution video disc internal surface contacts with solution film layer, because being subject to the stagnation effect of the blade on the fixed axoid video disc outside surface alternate with it, make the gas on the solution film layer surface on cone of revolution video disc internal surface, also produce a slip speed relative to the blade on fixed axoid video disc outside surface.
According to bernoulli (Bernoulli) equation principle, fluid velocity is higher, and pressure is lower, is namely more conducive to the saturation vapour pressure value of evaporitic environment pressure lower than rete solution.Therefore, the low-temperature evaporation device that described multilayer disc-stack centrifuge and gravity film forming and differential reduce pressure, by forming this two slip speeds, making the stream pressure contacted with rete lower than the saturation vapour pressure value of rete solution, improving the vaporization efficiency of fragrant oily mater.Meanwhile, by increasing the specific surface area of solution rete, the steam output of fragrant oily mater is strengthened.
Be dissolved with the cone of revolution video disc of solution from the superiors of fragrant oily mater, successively flow in the process of undermost fixed axoid video disc, the lower end sidepiece of the low-temperature evaporation device that hot gas flow then reduces pressure from described multilayer disc-stack centrifuge and gravity film forming and differential enters, and with solution stream to doing countercurrent flow, successively rise, period flows through the tapered annular gap that cone of revolution video disc and fixed axoid video disc are formed, with solution rete generation heat exchange, the fragrant oily mater of liquid phase is evaporated to gas phase, with steam, discharge via upper end pump orifice the low-temperature evaporation device that described multilayer disc-stack centrifuge and gravity film forming and differential reduce pressure by vacuum pump set.The saturation vapour pressure value lower due to solution thin layer and the depressurization of slip speed, and the suction synergy of vacuum pump set, make vaporization temperature lower, temperature operating ranges is adjustable in 25 ~ 95 DEG C.
Discharge the gas phase fragrance oily mater of the low-temperature evaporation device that described multilayer disc-stack centrifuge and gravity film forming and differential reduce pressure, be sucked and enter condensing works and gas-liquid separation device, make fragrant oily mater and condensed moisture from, obtain the plants essential oil fragrance of liquid state.Condensation and gas-liquid separation can adopt high-efficiency condensation well known in the art and tripping device, as screw pipework condensation device, membrane separation apparatus, chromatography column separator, macroporous resin separator etc.
Solution after evaporation concentration, the low-temperature evaporation device lower end of reducing pressure via described multilayer disc-stack centrifuge and gravity film forming and differential is discharged, owing to having the non-volatile plants essential oil component of low saturation vapour pressure value in concentrated solution containing some, make foodstuff additive etc. by processing purification.
By reference to the accompanying drawings embodiments of the invention are described above; but the present invention is not limited to above-mentioned embodiment; above-mentioned embodiment is only schematic; instead of it is restrictive; those of ordinary skill in the art is under enlightenment of the present invention; do not departing under the ambit that present inventive concept and claim protect, also can make a lot of form, these all belong within protection of the present invention.
Claims (10)
1. nappe flip length and centrifugal film decompression low-temperature distillation extract a method for plants essential oil fragrance, it is characterized in that, comprise the following steps:
S1, the extraction raw material of plants essential oil fragrance after pulverizing is joined in stirred pot, add after water stirs and deliver to separating centrifuge;
S2, the heavies after being separated is delivered to water fluid jet grind and carries out nappe flip length;
S3, the light materials solution that described step S2 obtains is delivered to the low-temperature evaporation device upper end charging opening that multilayer disc-stack centrifuge and gravity film forming and differential reduce pressure, described low-temperature evaporation device comprises cone of revolution video disc and the fixed axoid video disc of coaxial alternate lamination setting, wherein, cone of revolution video disc is fixing rotates on center shaft; Light materials solution, from the cone of revolution video disc of the superiors, successively flow to undermost fixed axoid video disc; The lower end sidepiece of the low-temperature evaporation device that hot gas flow then reduces pressure from described multilayer disc-stack centrifuge and gravity film forming and differential enters, and with lightweight thing solution stream to doing countercurrent flow, successively rise, period flows through the tapered annular gap that cone of revolution video disc and fixed axoid video disc are formed, with solution rete generation heat exchange, the fragrant oily mater of liquid phase is evaporated to gas phase;
S4, gas phase fragrance oily mater, with steam, is sucked and enters condenser, and be condensed into liquid together with water vapor; Again by separator make fragrant oily mater and condensed moisture from, obtain liquid plants essential oil fragrance.
2. nappe flip length according to claim 1 and centrifugal film decompression low-temperature distillation extract the method for plants essential oil fragrance, it is characterized in that, in described step S2, high pressure plunger pump, water fluid jet grind, separating centrifuge and pulverizing slurry transferring pump are connected to form closed-circuit pulverization and separating circuit, raw material in stirred pot, be delivered to separating centrifuge by plant pulp material conveying pump, the heavies after separation is transported to water fluid jet grind; Lightweight thing solution after separation, is transferred people's high pressure plunger pump, recycles as working medium.
3. nappe flip length according to claim 2 and centrifugal film decompression low-temperature distillation extract the method for plants essential oil fragrance, it is characterized in that, when granularity reaches the setting index of median size, heavies after separating centrifuge is separated switches out closed-circuit pulverization and separating circuit, and heavies is delivered to filter dehydration device.
4. nappe flip length according to claim 2 and centrifugal film decompression low-temperature distillation extract the method for plants essential oil fragrance, it is characterized in that, slurry after pulverizing obtains continuous circulation and pulverizes in closed-circuit pulverization and separating circuit, until when the subparticle granularity in lightweight thing solution after being separated by separating centrifuge reaches the setting index of median size, by flowrate control valve, lightweight thing solution is switched out closed-circuit pulverization and separating circuit, and be transported into evaporation slip preheater, lightweight thing solution after preheating, be transported to the low-temperature evaporation device upper end charging opening that multilayer disc-stack centrifuge and gravity film forming and differential reduce pressure again.
5. nappe flip length according to claim 4 and centrifugal film decompression low-temperature distillation extract the method for plants essential oil fragrance, it is characterized in that, the low-temperature evaporation device that described evaporation slip preheater reduces pressure with multilayer disc-stack centrifuge and gravity film forming and differential is connected with hot gas source.
6. nappe flip length according to claim 1 and centrifugal film decompression low-temperature distillation extract the method for plants essential oil fragrance, it is characterized in that, the aroma volatile produced in described water fluid jet grind crushing process is delivered to the condenser being arranged in evaporation unit back segment and traps.
7. nappe flip length according to claim 1 and centrifugal film decompression low-temperature distillation extract the method for plants essential oil fragrance, it is characterized in that, solution after evaporation concentration, the lower end of the low-temperature evaporation device reduced pressure via described multilayer disc-stack centrifuge and gravity film forming and differential is discharged, then is cooled to normal temperature by enriching slurry water cooler.
8. nappe flip length according to claim 7 and centrifugal film decompression low-temperature distillation extract the method for plants essential oil fragrance, and it is characterized in that, described condenser is connected with handpiece Water Chilling Units with water cooler.
9. nappe flip length according to claim 1 and centrifugal film decompression low-temperature distillation extract the method for plants essential oil fragrance, it is characterized in that, in described step S1, to the branch in scented plants raw material, skin, root or subterraneous stem, seed, granularity < 6 order is crushed to by plant pulverizer, to the flower in scented plants raw material, really, leaf, size < 2 order is become by cutting and grinding powder mode size degradation, join in stirred pot, again by solid-to-liquid ratio 1:(2 ~ 8) add water, impregnated raw material 20 ~ 120min at normal temperatures, period agitator with linear velocity 0.2 ~ 1m/s continuously or intermittent stirring.
10. nappe flip length according to claim 1 and centrifugal film decompression low-temperature distillation extract the method for plants essential oil fragrance, it is characterized in that, in described step S3, the temperature of the hot gas flow generation heat exchange of lightweight thing solution and rising in low-temperature evaporation device is within the scope of 25 ~ 95 DEG C.
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| CN108499151A (en) * | 2017-12-27 | 2018-09-07 | 温州市日中轻工机械有限公司 | A kind of centrifugal thin-film Distallation systm |
| CN109745444A (en) * | 2017-11-07 | 2019-05-14 | 甘肃省金羚集团药业有限公司 | A kind of Traditional Chinese medicine compound composition for treating deficient qi and blood |
| WO2020146053A1 (en) * | 2019-01-07 | 2020-07-16 | Tropicana Products, Inc. | Process and system for enhancing recovery of essential oil |
| CN111821764A (en) * | 2019-04-19 | 2020-10-27 | 吉林碳谷碳纤维股份有限公司 | Method and device for cleaning disc of precision filter |
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| CN109745444A (en) * | 2017-11-07 | 2019-05-14 | 甘肃省金羚集团药业有限公司 | A kind of Traditional Chinese medicine compound composition for treating deficient qi and blood |
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| WO2020146053A1 (en) * | 2019-01-07 | 2020-07-16 | Tropicana Products, Inc. | Process and system for enhancing recovery of essential oil |
| US10995300B2 (en) | 2019-01-07 | 2021-05-04 | Tropicana Products, Inc. | Process and system for enhancing recovery of essential oil |
| CN111821764A (en) * | 2019-04-19 | 2020-10-27 | 吉林碳谷碳纤维股份有限公司 | Method and device for cleaning disc of precision filter |
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| CN105349262B (en) | 2019-03-05 |
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