CN208008751U - A kind of agilawood essential oil decompression fractionation unit - Google Patents

Abstract

The utility model provides a kind of agilawood essential oil fractionating device, including raw material tank, distiller, blade applicator and condenser pipe；Raw material tank outer cover is equipped with pre- hot jacket, and the bottom of raw material tank is connected to distiller；The inner barrel of the distiller is divided into epicoele and cavity of resorption two parts, and one end of blade applicator connects scraping blade motor, and the other end, which is connected with, scrapes diaphragm, scrapes diaphragm and stretches into the upper intracavitary；It is also enclosed outside the cylinder of distiller corresponding to epicoele equipped with chuck, forms an oil bath chamber between chuck and cylinder；Lower intracavitary is provided with the internal collecting pipe for cavity structure, and the lower end of collecting pipe is connected to condenser pipe；The other end of condenser pipe connects essential oil receiving flask by an essential oil diversion pipe；The essential oil diversion pipe is connected to a cold-trap by a vacuum tube, the vacuum system of distiller described in the other end piping connection of cold-trap；The bottom of distiller also connects fraction collection bottle by a residue diversion pipe.The utility model fractionation is high-quality, and essential oil fractionating efficiency is high, has preferable practical value.

Description

A kind of agilawood essential oil decompression fractionation unit

Technical field

The utility model is related to essential oil fractionating technology fields, and in particular to a kind of agilawood essential oil decompression fractionation unit.

Background technology

Agalloch eaglewood contains the timber of resin for Isolated From Thymelaeaceae Species suspension culture of Aquilaria sinensis Aquilaria sinensis (Lour.) Gilg.Point It is distributed in the ground such as Guangdong, Hainan, Guangxi, Fujian.With promoting qi circulation and relieving pain, the effect of warming middle energizer to arrest vomiting, gas of receiving is relievingd asthma.It is swollen to be usually used in chest and abdomen Bored pain, gastrofrigid vomiting hiccup, the asthma of the kidney deficiency circulation of vital energy in the wrong direction are anxious.

The extractive of volatile oil of agilawood essential oil, that is, agalloch eaglewood, fragrance is elegant, is the important originals such as manufacture highclass perfumes, cosmetics Material.The extracting method of agilawood essential oil is more in the market, there is steam distillation, supercritical extraction, solvent method, Microwave-assisted Extraction Follow the example of etc., open source literature also reports the extracting method of some agilawood essential oils, such as：

(1) application No. is 201310630694.2 Chinese patents to disclose a kind of extracting method of agilawood essential oil, the party Method selects entrainer of the ethyl alcohol as supercritical carbon dioxide extracting agilawood essential oil, by supercritical carbon dioxide extraction method and essence Technology combined use is evaporated, the solubility and soluble end of extractant is effectively increased, agilawood essential oil recovery rate is made to be increased, Gained agilawood essential oil uniform color is limpid, strong flavor.(2) application No. is 201410028499.7 Chinese patents to disclose one The method that agilawood essential oil is extracted kind from agalloch eaglewood sawdust, this method be after agalloch eaglewood sawdust is first beaten powder, relatively low at 30~60 DEG C At a temperature of extract using ethyl alcohol as solvent extraction or by solvent continuous microwave of ethyl alcohol, then by the first extract of gained at -7 DEG C ~-18 times 5~20h of freezing, take advantage of cold suction filtration, solvent are recovered under reduced pressure and obtains medicinal extract, 0.5~2 (w of its weight is added into medicinal extract:w) Times adsorbent, the two is uniformly mixed to the glass chromatography column for being splined on that draw ratio is 5~15 for dry-eye disease, uses mixed solvent Column is rushed, eluent is collected, in 40~65 DEG C of water-baths, mixed solvent is evaporated in the case where vacuum degree is 0.02~0.09MPa, is sunk Essential oil.The obtained agilawood essential oil product of the invention is in light brown, and appearance uniform is transparent, good fluidity, and the technique is maximum Limit it is enriched with and protects heat-sensitive ingredients fragrant in agalloch eaglewood, aroma of pure and complete.(3) application No. is 201410180768.1 Chinese patent also provides a kind of extracting method of agilawood essential oil, and this method crushes agalloch eaglewood raw material simultaneously Water is added to stir into slurries, slurries cross colloid mill；The slurries after colloid mill are completed through ultrasonication, then use cellulase water Solution；Enzyme-deactivating after hydrolysis filters, and the first filtrate of gained is extracted with 95% ethyl alcohol, takes organic phase to filter again, the second filtrate of gained Ethyl alcohol is distilled off, obtains agilawood essential oil.The invention carries out economic benefits and social benefits extraction using ultrasonic wave and enzymatic isolation method to agilawood essential oil, effectively Raising agilawood essential oil recovery rate, so that the agilawood essential oil extraction yield of the agalloch eaglewood raw material of the layer containing whitewood is improved to 0.4% or more, Extraction time is reduced simultaneously, is suitable for the extraction of the agilawood essential oil of natural agilawood and artificial agilawood；(4) application No. is The Chinese patent of 201610212220.X then provides a kind of distillation production method and equipment of agilawood essential oil, by that will distill original Material steam boiler is heated into steam, and then condensation fractionation within the condenser, obtains required agilawood essential oil.

It has been investigated that in the document of report disclosed above, document 1 to 3 is all added to second in the extraction of agilawood essential oil Alcohol influences whether the quality of agilawood essential oil using a series of operation, the extracting method；Document 4 is in the extraction side of agilawood essential oil Face extracts essential oil by the way of distillation, and addition enzyme or ethyl alcohol can effectively be avoided to have an impact agilawood essential oil, but It is that this method device structure is more complicated, cost is higher, while also lacking the collection measure to residue, to being fractionated the matter of essential oil There is certain influence in amount.

Therefore, it is based on above-mentioned, the utility model provides that a kind of cost is relatively low, the higher agilawood essential oil fractionation dress of fractionating efficiency It sets, second-rate to solve agilawood essential oil fractionation of the existing technology, fractionating efficiency is relatively low and cost is higher insufficient and scarce It falls into.

Utility model content

The purpose of this utility model is that：For presently, there are the above problem, provide a kind of cost it is relatively low, fractionation effect The higher agilawood essential oil decompression fractionation unit of rate, second-rate to solve agilawood essential oil fractionation of the existing technology, fractionation is imitated Rate is relatively low and the higher problem of cost.

The utility model provides a kind of agilawood essential oil decompression fractionation unit, including raw material tank, distiller, blade applicator and cold Solidifying pipe；The raw material tank outer cover be equipped with it is internal be cavity structure pre- hot jacket, the bottom of the raw material tank by mother tube with The distiller connection；The inner barrel of the distiller is divided into epicoele and cavity of resorption two parts, one end connection of the blade applicator Scraping blade motor, the other end, which is connected with, scrapes diaphragm, and the diaphragm of scraping stretches into the upper intracavitary；Distiller corresponding to the epicoele It is also enclosed outside cylinder equipped with chuck, forms an oil bath chamber between the chuck and the cylinder；The lower intracavitary is provided with inside For the collecting pipe of cavity structure, the collecting pipe is located at the lower section for scraping diaphragm；The upper end of the collecting pipe and tube wall surrounding Several pores are provided with, and the lower end of the collecting pipe is connected to the condenser pipe；The other end of the condenser pipe passes through an essence Oily diversion pipe connects essential oil receiving flask；The essential oil diversion pipe is connected to a cold-trap, the other end of the cold-trap by a vacuum tube The vacuum system of distiller described in piping connection；The bottom of the distiller also connects residue by a residue diversion pipe and receives Collect bottle.

Preferably, it is described scrape diaphragm be helical blade shape, and it is described scrape be between diaphragm and the inner wall of the epicoele between Gap coordinates；The quantity for scraping diaphragm is 3 or 3 or more.

Preferably, the pore size of the pore is 0.3mm-0.5mm；The pore is circular through hole structure, ellipse The polygonal through hole structure of through-hole structure or rule, and the pore surrounds the axle center array arrangement of collecting pipe.

Preferably, the vacuum system includes diffusion pump and vacuum pump, the cold-trap can respectively with the diffusion pump vacuum Pump line road is connected to；A switch valve V7 is equipped on the pipeline that diffusion pump is connected to cold-trap, the other end of diffusion pump connects tap water Slot is equipped with a switch valve V11 on the pipeline that diffusion pump is connected to originally sink；Connecting line between cold-trap and vacuum system Further include first pipe and second pipe, first pipe is equipped with a pressure gauge, and pressure gauge is respectively arranged on the left side and the right side switch Valve V5 and switch valve V6；There is first pipe the first end and second end being oppositely arranged, first end to be located at cold-trap and switch valve V7 Between pipeline on, the second end of first pipe is between diffusion pump and switch valve V11；One end of second pipe is located at pressure On pipeline between table and switch valve V6, the other end is connect with vacuum pump, and second pipe is equipped with switch valve V3.

Preferably, it is provided with the circulation port of spiral through-hole structure on the tube wall of the condenser pipe, the entrance of circulation port and goes out Mouth is connected to thermostatic water bath by hose and forms closed circulation respectively.

Preferably, the end of the mother tube is extend into the distiller, and close to the tube wall of the distiller.

Preferably, the mother tube outer cover is equipped with economizer bank, the upper end of the pre- hot jacket and the lower end of economizer bank point It is not connected to preheater.

Preferably, oil bath chamber top and bottom are connected to oil heater by oil bath pipe respectively, form oil bath heating and return Road.

Preferably, be between the raw material tank and preheater it is closed be connected to, form closed air preheat circuit, and raw material The switch valve V8 for control channel open or close is provided between slot and distiller.

Preferably, it is both provided with switch valve V2 on 2 pipelines that the oil heater is connected to oil bath chamber, oil heater Right end is provided with switch valve V10, and originally sink, the originally sink are used to be oil heater for the other end connection of switch valve V10 Cooling tap water is provided.

By adopting the above-described technical solution, the beneficial effects of the utility model are：

The utility model preheats the pipeline of raw material tank and connection raw material tank by preheater, passes through and preheats increase The mobility of the larger extraction raw material of viscosity, is distilled to be flowed rapidly into distiller conducive to extraction of essential oil object；It will sink Essence oil extract, downstream in distiller, is provided with the knifing being connect with blade applicator lower end along distiller tube wall in distiller Piece；The blade applicator that extraction of essential oil object is rotated scrapes from tube wall and is dispersed in the knifing on piece of preheating；Agilawood essential oil is set to extract Essential oil fractionation component in object is evaporated, and essential oil is fractionated component under pull of vacuum effect after inflow collecting pipe, condensed pipe It cools down and flows into essential oil receiving flask；And the residual component detached is fallen from blade applicator, enters essential oil along residue diversion pipe Fraction collection bottle.This fractionation mode can be protected effectively by the lower agilawood essential oil of boiling point and the effective separate collection of residue The collection purity of agilawood essential oil is demonstrate,proved.In addition, the utility model is carried in fractional distillation process without adding ethyl alcohol and various enzymes auxiliary Essential oil is taken, therefore the fractional method of the utility model is extracted relative to addition auxiliary reagent for the method for essential oil, fractionation is sunk Essential oil better quality can effectively avoid the pollution of ethyl alcohol and auxiliary enzymes.

On the other hand, utility model is heated relative to existing boiler and is fractionated by the use of scraping blade motor and blade applicator For mode, fractionating efficiency higher, fractionating effect is more preferable；Carrying for distiller tube wall can will be flowed to by scraping the quick rotation of diaphragm It takes raw material to be disperseed, forms liquid dispersed film, the flash distillation for extracting raw material can be accelerated；Again by adjusting knifing The temperature of piece and the vacuum degree of distiller can be fractionated the agilawood essential oil of heterogeneity, the fractionation components control side of essential oil Just, conducive to meeting the use demand of different clients；Meanwhile the fractionating device structure of the utility model is relative to existing boiler point For distillation unit, equipment cost is relatively low.

In another aspect, utility model is arranged by the collecting pipe of porous structure, the impurity quilt outside collecting pipe can be avoided It sucks in collecting pipe, ensures the material of distillation essential oil, also avoid the impurity of sucking from resulting in blockage or destroy pipeline, pore Structure plays the role of filtering protection；In conjunction with the condensation of condenser pipe, it can realize that the essential oil steam of evaporation passes through vacuum system Enter collecting pipe under the action of system, and flow into and be condensed into drop in condenser pipe, flowing into essential oil then along essential oil diversion pipe collects It is stored in bottle；And residue is fractionated then under the action of scraping diaphragm, it falls in cavity of resorption, finally along residue diversion pipe It flows into fraction collection bottle and collects, this fractionation mode can be protected effectively by agilawood essential oil and the effective separate collection of residue The collection purity of agilawood essential oil is demonstrate,proved；And cold-trap is set between condenser pipe and diffusion pump, it can be to completely cold not in condenser pipe Solidifying essential oil steam carries out time condensation, and essential oil steam is avoided to be made with safe by the performance that vacuum pump sucks and influences vacuum system With the safeguard protection tool of raising and equipment hence for fractionating efficiency has very great help.

Finally, the use of the oil heater can facilitate in fractional distillation process and distiller is preheated and heated, to The rapid evaporation of extraction of essential oil raw material is effectively facilitated, improves the fractionating efficiency of essential oil energetically, is also conducive to avoid agilawood essential oil Loss and waste.

Through examining, the agilawood essential oil that is refining to obtain is fractionated using the utility model, purity is higher, persticide residue and again Tenor detection level exists《Chinese Pharmacopoeia》In bound requirements as defined in versions in 2015.This illustrates the technology of the utility model The agilawood essential oil fractionating effect that scheme is obtained is good, and purity is preferable, and persticide residue and impurity content disclosure satisfy that user's Requirement.

Description of the drawings

Fig. 1 is the structural schematic diagram of the agilawood essential oil decompression separation device of the utility model；

Fig. 2 is the distiller internal structure schematic diagram of the utility model；

Fig. 3 scrapes diaphragm mounting structure schematic diagram for the utility model；

Fig. 4 is the collecting pipe structural schematic diagram of the utility model；

Fig. 5 is the ion of the gas chromatography-mass spectrum (GC-MS) of gained agilawood essential oil sample in the utility model embodiment 1 Flow graph.

Fig. 6 is the ion flow graph of the GC-MS of gained agilawood essential oil sample in the utility model embodiment 2.

In figure：1, raw material tank；2, preheater；3, diffusion pump；4, vacuum pump；5, water ring vacuum pump；6, oil heater；7, cold Trap；8, fraction collection bottle；9, essential oil receiving flask；10, thermostatic water bath；11, hose；12, distiller；13, scraping blade motor；14, Blade applicator；15, vacuum tube；16, diaphragm is scraped；17, epicoele；18, cavity of resorption；19, collecting pipe；20, condenser pipe；21, circulation port；22, Essential oil diversion pipe；23, residue diversion pipe；24, pressure gauge；25, originally sink；26, oil bath chamber；27, oil bath pipe；28, it connects Axis；29, pore；30, pre- hot jacket；31, economizer bank；32, chuck；33, first pipe；34, second pipe；35 third pipelines.

Specific implementation mode

It is new below in conjunction with this practicality to keep the purpose, technical scheme and advantage of the utility model embodiment clearer Attached drawing in type embodiment, the technical scheme in the utility model embodiment is clearly and completely described, it is clear that is retouched The embodiment stated is the utility model a part of the embodiment, instead of all the embodiments, based on the implementation in the utility model Example, the every other embodiment that those of ordinary skill in the art are obtained without creative efforts belong to The range of the utility model protection.

Embodiment 1

As shown in Figs 1-4, it is a kind of agilawood essential oil decompression fractionation unit used in the utility model embodiment.The device Including raw material tank 1, distiller 12, blade applicator 14 and condenser pipe 20；Raw material tank 1 is located at storage, default agilawood essential oil extract.It is former The outer cover of hopper 1 is equipped with the internal pre- hot jacket 30 for cavity structure, and the bottom of raw material tank 1 passes through mother tube and distiller 12 connects It is logical；The inner barrel of the distiller 12 is divided into 18 two parts of epicoele 17 and cavity of resorption；One end of the blade applicator 14 connects scraping blade Motor 13, the other end, which is connected with, scrapes diaphragm 16, scrapes diaphragm 16 and stretches into the epicoele 17.Further, it scrapes diaphragm 16 and passes through company Spindle 28 is connected with the lower end of blade applicator 14.Outside the cylinder of distiller 12 corresponding to epicoele 17, also enclose equipped with chuck 32, An oil bath chamber 26 is formed between the chuck 32 and cylinder, for being filled with conduction oil.In the cavity of resorption 18 of distiller 12 is internally provided with Portion is the collecting pipe 19 of cavity structure, and collecting pipe 19 is located at the lower section for scraping diaphragm 16；The upper end of collecting pipe 19 and tube wall surrounding are equal Several pores 29 are provided with, and 19 lower end of collecting pipe is connected to condenser pipe 20；The lower end of condenser pipe 20 passes through an essential oil water conservancy diversion The closing connection essential oil of pipe 22 receiving flask 9；Essential oil diversion pipe 22 passes through 15 closed communication cold-trap 7 of a vacuum tube, the other end of cold-trap 7 The vacuum system of piping connection distiller 12；The bottom of distiller 12 is connected with residue by a residue diversion pipe 23 closing Receiving flask 8.

Preferably, the diaphragm 16 of scraping is helical blade shape, and the inner wall for scraping diaphragm 16 and the epicoele 17 it Between be clearance fit；The quantity for scraping diaphragm 16 is 3 or 3 or more.

Preferably, the pore size of the pore 29 is 0.3mm-0.5mm；The pore 29 is circular through hole structure, ellipse The polygonal through hole structure of circular through hole structure or rule, and the pore 29 surrounds the axle center array arrangement of collecting pipe 19.

Preferably, the vacuum system includes diffusion pump 3 and vacuum pump 4, the cold-trap 7 can respectively with the diffusion pump 3 4 pipeline of vacuum pump is connected to；A switch valve V7 is equipped on the pipeline that diffusion pump 3 is connected to cold-trap 7, the other end of diffusion pump 3 connects Be connected to and carry out sink 25, diffusion pump 3 on the pipeline that originally sink 25 is connected to be equipped with a switch valve V11；Cold-trap 7 and vacuum system Between connecting line further include first pipe 33 and second pipe 34, first pipe 33 is equipped with a pressure gauge 24, pressure gauge 24 are respectively arranged on the left side and the right side switch valve V5 and switch valve V6；First pipe 33 has the first end and second being oppositely arranged End, for first end on the pipeline between cold-trap 7 and switch valve V7, the second end of first pipe 33 is located at diffusion pump 3 and switch Between valve V11；One end of second pipe 34 is on the pipeline between pressure gauge 24 and switch valve V6, the other end and vacuum pump 4 Connection, second pipe 34 are equipped with switch valve V3.

Preferably, the circulation port 21 of spiral through-hole structure is provided on the tube wall of the condenser pipe 20, circulation port 21 enters Mouth and outlet are connected to thermostatic water bath 10 by hose 11 and form closed circulation respectively.

Preferably, the end of the mother tube is extend into the distiller 12, and close to the tube wall of the distiller 12.

Preferably, the mother tube outer cover is equipped with economizer bank 31, the upper end of the pre- hot jacket 30 and economizer bank 31 Lower end is connected to preheater 2 respectively.

Preferably, 26 top and bottom of oil bath chamber are connected to oil heater 6 by oil bath pipe 27 respectively, form oil bath and add Hot loop.

Preferably, be between the raw material tank 1 and preheater 2 it is closed be connected to, form closed air preheat circuit, and former The switch valve V8 for control channel open or close is provided between hopper 1 and distiller 12.

Preferably, switch valve V2, oil heating are both provided on 2 pipelines that the oil heater 6 is connected to oil bath chamber 26 The right end of device 6 is provided with switch valve V10, and the other end of switch valve V10 connects originally sink 25, and the originally sink 25 is for being Oil heater 6 provides cooling tap water.

In the utility model other embodiment, raw material tank 1 is not used yet, at this point it is possible to entering the distiller Mouth is connected to the outlet conduit of the extraction equipment of agilawood essential oil extract.Extraction, the decompression point of agilawood essential oil may be implemented in this way The continuous operation evaporated.

In the utility model embodiment, the end of the mother tube extend into the upper intracavitary of distiller 12, and close to stating steaming Evaporate the tube wall of device 12.

Further, the outer cover of mother tube is equipped with economizer bank 31；For being filled with heat medium in economizer bank 31.Further Ground, pipeline is connected between one end of pre- hot jacket 30, one end of economizer bank 31, the other end of pre- hot jacket 30, economizer bank 31 it is another End is connected to 2 pipeline of a preheater respectively；Preheater 2 into the pre- hot jacket 30, economizer bank 31 for providing heat medium.Add Thermal medium can return to preheater after flowing through pre- hot jacket 30, economizer bank 31, form warm-up cycle circuit；A preheating is used in this way Device 2 can realize the preheating to agilawood essential oil extract in raw material tank 1 simultaneously, and the agilawood essential oil extract after preheating is in raw material Preheating temperature is kept in pipe, additionally it is possible to the mobility for increasing the larger extraction raw material of viscosity by preheating, to promote essence Oil extract carries out rapid evaporation in inflow distiller, improves the fractionating efficiency of essential oil energetically, is also conducive to avoid agalloch eaglewood smart The loss and waste of oil.

Optionally, heat medium can be vapor, hot-air etc..

Further, it is provided with switch valve V1 in the connecting pipe between the pre- hot jacket 30 and economizer bank 31, for controlling The warm-up cycle circuit of raw material tank processed.

Further, it is additionally provided with switch valve V8 on the mother tube.The switch valve V8 is for controlling the raw material tank 1 The open or close of pipeline between distiller 12.

Wherein, oil bath chamber 26 is connected to by oil bath pipe 27 with 6 pipeline of oil heater, and oil heater 6 is used to export heating It encloses in the chuck 32 set on the top of conduction oil to distiller 12.It is apparent that being respectively arranged on the chuck 32 and oil bath chamber 26 Heat conducting oil inlet, the conduction oil outlet of connection.Oil bath pipe 27 is connected at heat conducting oil inlet, conduction oil outlet respectively.It in this way can be real Now in distiller 12, and it extend into distiller 12 and scrapes preheating of the diaphragm 16 before fractionation, the heating in fractional distillation process, The rapid evaporation of extraction of essential oil raw material is effectively facilitated, improves the fractionating efficiency of essential oil energetically, is also conducive to avoid agilawood essential oil Loss and waste.

In the utility model embodiment, in scraping blade motor 13 under the driving of blade applicator 14, drive is scraped diaphragm 16 and quickly revolved Turn, the extraction raw material for flowing to distiller tube wall can be disperseed, form liquid dispersed film, extract original can be accelerated The flash distillation of material；The temperature of diaphragm and the vacuum degree of distiller are scraped by adjusting again, the agalloch eaglewood essence of heterogeneity can be fractionated The fractionation components control of oil, essential oil is more convenient, conducive to the use demand of different clients is met.

Further, it is helical blade shape to scrape diaphragm 16, and is scraped between diaphragm 16 and 17 inner wall of epicoele of distiller 12 For clearance fit；The quantity for scraping diaphragm 16 is 3 or 3 or more；The material for scraping diaphragm 16 is metal material.

In the utility model embodiment, switch valve is additionally provided on the pipeline that the oil heater 6 is connected to oil bath chamber 26 V2；The other end of the oil heater 6 with one originally sink 25 connect, connect with originally sink 25 in the oil heater 6 Switch valve V10 is additionally provided on pipeline.Originally sink 25 is used to provide cooling tap water for oil heater 6.

In the utility model embodiment, the vacuum system of distiller 12 includes diffusion pump 3, vacuum pump 4 and water ring vacuum pump 5, cold-trap 7 is connected with diffusion pump 3, vacuum pump 4 and water ring vacuum pump 5 respectively.Diffusion pump 3, vacuum pump 4 and water ring vacuum pump 5 Etc. compositions vacuum system, can be before fractionation starts, to provide required vacuum environment in distiller 12；In distillation fractional distillation process In, under the action of the vacuum system, the essential oil that evaporates fractionation component can the vacuum systems such as diffusion pump, vacuum pump pumping it is true Sky effect is lower to enter collecting pipe, and flows into condenser pipe, is condensed into drop.

For the vacuum system, specifically, it is equipped with a switch valve V7 on the pipeline that diffusion pump 3 is connected to cold-trap 7, expands Other end connection originally sink 25 for dissipating pump 3, diffusion pump 3 on the pipeline that originally sink 25 is connected to equipped with a switch valve V11； Connecting line between cold-trap 7 and vacuum system further includes first pipe 33, second pipe 34 and third pipeline 35, first pipe 33 are equipped with a pressure gauge 24, and pressure gauge 24 is respectively arranged on the left side and the right side switch valve V5 and switch valve V6；First pipe 33 has There is the first end and second end being oppositely arranged, on the pipeline between cold-trap 7 and switch valve V7, second end is located to expand first end It dissipates between pumping 3 and switch valve V11；One end of second pipe 34 connects water ring vacuum pump 5, and the other end of second pipe 34 is located at pressure On pipeline between power table 24 and switch valve V6, second pipe 34 is equipped with switch valve V4；The other end of water ring vacuum pump 5 connects Originally sink 25；One end of third pipeline 35 connects vacuum pump 4, and the other end of third pipeline is located at the other end of second pipe 34 Between switch valve V4, third pipeline 35 is equipped with switch valve V3.

In the utility model, the vacuum system of the compositions such as diffusion pump 3 and vacuum pump 4 can be distiller before fractionation starts Vacuum environment needed for being provided in 12；In fractional distillation process, under the action of the vacuum system, the essential oil fractionation component evaporated can Enter collecting pipe under the vacuum action of the vacuum systems such as diffusion pump, vacuum pump, and flow into condenser pipe, is condensed into drop.

The cold-trap 7 is arranged in the utility model between diffusion pump 3 and the essential oil diversion pipe 22 for being connected to condenser pipe lower end； In distilling fractional distillation process, cold-trap 7 can be to not carrying out time condensation, later stage in the essential oil of condenser pipe total condensation fractionation steam It can mutually merge with the liquid in essential oil receiving flask 9, reduce the waste to agilawood essential oil extract；The presence of cold-trap 7 may be used also Essential oil steam is avoided to be sucked and influenced performance and the safe handling of vacuum system by vacuum systems such as vacuum pump 4, diffusion pumps 3, from And the safeguard protection tool of the raising and equipment for fractionating efficiency has very great help.

It should be noted that in vacuumizing before fractionation and fractional distillation process, the water ring vacuum pump 5 is not used；Water Ring vacuum pump 5 can be used for before experiment starts, and is dehydrated to agilawood essential oil extract, reduce containing for agilawood essential oil extract Water.Detailed process is as follows：Water ring vacuum pump 5 is opened, switch valve V4 and V9 are then turned on, by water ring vacuum pump 5 to distiller Agilawood essential oil extract, is then added in distiller 12, slightly adds to it by interior offer vacuum environment (being usually 2.0-3.8Pa) Heat, the vapor in agilawood essential oil extract are just distilled out of, and it is condensed after flow into essential oil receiving flask 9, after dehydration, Water in essential oil receiving flask 9 is outwelled, and is collected the liquid in fraction collection bottle 8, is just obtained dewatered agilawood essential oil extract. After dehydration, turn off water ring vacuum pump 5 and switch valve V4, V9.Subsequently in fractionation, dewatered agilawood essential oil can be extracted It is added in distiller 12 after object preheating.

In the embodiment of the utility model, the collecting pipe 19 of porous structure, pore 29 are set in the lower section for scraping diaphragm 16 The substance (such as residual component of the extraction of essential oil object of knifing on piece, fractionation) outside collecting pipe can be avoided to be inhaled into collecting pipe In, ensure the material of distillation essential oil, also avoids the impurity of sucking from resulting in blockage or destroy the pipeline of collecting pipe 19, pore Structure can play the role of filtering protection.

Preferably, the circulation port 21 of spiral through-hole structure is provided on the tube wall of the condenser pipe 20, circulation port 21 enters Mouth and outlet are connected to thermostatic water bath 10 by hose 11 and form closed circulation respectively.Can be in this way agilawood essential oil point The condensation for evaporating component in condenser pipe 20 creates conditions.

Agilawood essential oil decompression fractionation unit provided by the utility model, by the agilawood essential oil extract that will preheat along steaming It evaporates 12 tube wall of device to flow down, is provided in the epicoele 17 of distiller 12 and scrapes diaphragm 16, scrape diaphragm 16 and be connected to and can be motor driven 14 lower end of blade applicator, extraction of essential oil object scrape from tube wall and are dispersed in the scraping on diaphragm 16 of preheating by blade applicator 14, and essential oil carries The essential oil in object is taken to be fractionated component evaporation；Distiller 12 is provided by diffusion pump 3, vacuum pump 4 and water ring vacuum pump 5 etc. Vacuum environment, after essential oil fractionation group is diverted into collecting pipe 19, condensed pipe 20 cools down and flows into essential oil receiving flask 9；Residual component It is then fallen from blade applicator 14, enters essential oil fraction collection bottle 8 along residue diversion pipe 23.Provided by the utility model point Evaporating technique can ensure that the collection of agilawood essential oil is pure effectively by the lower agilawood essential oil of boiling point and the effective separate collection of residue Degree, enriches its ingredient.

The yield for the agilawood essential oil sample that the present embodiment 1 obtains is 75% or so.The agilawood essential oil that the present embodiment 1 is obtained Sample carries out composition detection, and analyzing detecting method is：After agilawood essential oil sample is dissolved with chromatographically pure n-hexane solvent, use Gas chromatograph-mass spectrometer (GC-MS) (GC-MS) analyzes its chemical composition to analyze.Chromatographic column is 5%Phenyl Methyl 0.25 μm of the μ m of Silox, 30m × 250；240 DEG C of injector temperature；50 DEG C of holding 1min of column temperature, 140 DEG C are risen to 15 DEG C/min And keep 1min, then rise to 160 DEG C with 1 DEG C/min and keep 2min, finally 250 DEG C are risen to 18 DEG C/min；Carrier gas is helium Gas, flow velocity 1mL/min, 1 μ L of sample size, split ratio 50:1.Mass Spectrometry Conditions：EI-MS, 230 DEG C of ion trap temperature, level four bars temperature 150 DEG C of degree, 260 DEG C of interface temperature, mass range 40-300amu.Using NIST mass spectrum picture libraries confrontation modal data carry out retrieval with It is qualitative, and calculate by areas of peak normalization method the relative amount of each compound, wherein the ion flow graph of gas chromatography-mass spectrum See Fig. 5.The retention time, title of the larger ingredient of content and percentage contents are as shown in table 1 in sample.

The fractions testing result of the agilawood essential oil sample of 1 embodiment 1 of table

Wherein, 155 ingredients, wherein agalloch eaglewood characteristic sesquiterpenoids ingredient-are detected altogether from the agilawood essential oil sample The percentage contents of agalloch eaglewood spiral alcohol (Agarospirol) are 1.799%.Meanwhile it being detected through gaschromatographic mass spectrometry, agalloch eaglewood essence Persticide residue and content of beary metal testing result content exist in oil samples《Chinese Pharmacopoeia》Limit is wanted as defined in versions in 2015 In asking.This illustrates that the agilawood essential oil fractionating effect that the technical solution of the utility model is obtained is good, and purity is preferable, persticide residue It disclosure satisfy that the requirement of user with impurity content.

Embodiment 2

As shown in Figs 1-4, another embodiment operation of the utility model includes the following steps：

(1) early-stage preparations：

Agalloch eaglewood timber is ground into the Chinese Eaglewood Wood that grain size is 60 mesh, then supercritical fluid extraction obtains agilawood essential oil Extract；Agilawood essential oil extract is placed with raw material tank 1, and is preheated to 60 DEG C；

Distiller 12 is preheated to 122 DEG C, diaphragm 16 is scraped and is preheated to 122 DEG C, condenser pipe 20 is cooled to 30 DEG C in advance；Then pass through Vacuum degree in distiller 12 is reached 3.2Pa by vacuum pump 4；The vacuum degree in distiller 12 is reached by diffusion pump 3 1.2Pa；

(2) fractional distillation process：

Agilawood essential oil extract after preheating is flowed out from raw material tank 1, and with the speed of 90mL/s along the pipe of distiller 2 Wall is added in distiller 1；Control blade applicator 14 is scraped diaphragm 16 with the rotating speed drive of 400r/min and is rotated, and blade applicator 14 is smart by agalloch eaglewood Oil extract is scraped from the tube wall of distiller 12, and is dispersed in and is preheated to 122 DEG C and scrapes on diaphragm 16, and agilawood essential oil is made to carry It takes the essential oil in object to be fractionated component to be evaporated；

Essential oil is fractionated component steam and is pre-cooled to 30 DEG C of condenser pipe 20 by the inflow of collecting pipe 19 under pull of vacuum It is interior；Essential oil is fractionated component steam cooled essential oil that condenses into condenser pipe 20 and is fractionated component fluids, and along essential oil diversion pipe It is collected in 22 inflow essential oil receiving flasks 9；And not in condenser pipe 20, the essential oil of total condensation is fractionated steam, then can be true Time condensation is carried out in cold-trap 7 from essential oil diversion pipe 22, via vacuum tube 15 under suction power；The essential oil that will be collected in cold-trap 7 It is merged to get the agilawood essential oil sample refined to fractionation with the essential oil in essential oil receiving flask 9；

And be not easy to evaporate residual component after being fractionated in agilawood essential oil extract, then from scraping on diaphragm 16 and distiller 12 Tube wall on fall, and entered in fraction collection bottle 8 by residue diversion pipe 23 and be collected.

The yield for the agilawood essential oil sample that the present embodiment 2 obtains is 68% or so.Using GC-MS similar to Example 1 Method carries out composition detection, wherein the ion flow graph of gas chromatography-mass spectrum is shown in the agilawood essential oil sample that the present embodiment 2 obtains Fig. 6；The retention time, title of the larger each ingredient of content and percentage contents are as shown in table 2 in sample.

The fractions testing result of the agilawood essential oil sample of 2 embodiment 2 of table

Detect 171 ingredients, wherein agalloch eaglewood characteristic sesquiterpenoids ingredient-agalloch eaglewood spiral shell altogether from agilawood essential oil sample The percentage contents for revolving alcohol (Agarospirol) are 0.595%.Meanwhile it being detected through gaschromatographic mass spectrometry, agilawood essential oil sample Middle pesticide residue and heavy metal are detection, are met《Chinese Pharmacopoeia》Bound requirements as defined in versions in 2015.This illustrates this practicality The agilawood essential oil fractionating effect that novel technical solution is obtained is good, and purity is preferable, and persticide residue and impurity content can Meet the requirement of user.

Above description is only a specific implementation of the present invention, but the scope of protection of the utility model is not limited to In this, any one skilled in the art can readily occur in variation in the technical scope that the utility model discloses Or replace, it should be covered within the scope of the utility model.Therefore, the scope of protection of the utility model should be wanted with right Subject to the protection domain asked.

Claims (10)

1. a kind of agilawood essential oil decompression fractionation unit, which is characterized in that including raw material tank (1), distiller (12) blade applicator (14) With condenser pipe (20)；Raw material tank (1) outer cover is equipped with the internal pre- hot jacket (30) for cavity structure, the raw material tank (1) Bottom be connected to the distiller (12) by mother tube；The inner barrel of the distiller (12) be divided into epicoele (17) and under Chamber (18) two parts, one end connection scraping blade motor (13) of the blade applicator (14), the other end, which is connected with, scrapes diaphragm (16), described Diaphragm (16) is scraped to stretch into the epicoele (17)；It also encloses and is equipped with outside the cylinder of distiller (12) corresponding to the epicoele (17) Chuck (32) forms an oil bath chamber (26) between the chuck (32) and the cylinder；It is provided with inside in the cavity of resorption (18) For the collecting pipe (19) of cavity structure, the collecting pipe (19) is located at the lower section for scraping diaphragm (16)；The collecting pipe (19) Upper end and tube wall surrounding be provided with several pores (29), and the lower end of the collecting pipe (19) with the condenser pipe (20) even It is logical；The other end of the condenser pipe (20) connects essential oil receiving flask (9) by an essential oil diversion pipe (22)；The essential oil diversion pipe (22) cold-trap (7) is connected to by a vacuum tube (15), distiller (12) described in the other end piping connection of the cold-trap (7) Vacuum system；The bottom of the distiller (12) also connects fraction collection bottle (8) by a residue diversion pipe (23).

2. agilawood essential oil decompression fractionation unit as described in claim 1, which is characterized in that the diaphragm (16) of scraping is helical-blade Plate shape, and described scrape between diaphragm (16) and the inner wall of the epicoele (17) is clearance fit；The number for scraping diaphragm (16) Amount is 3 or more.

3. agilawood essential oil decompression fractionation unit as described in claim 1, which is characterized in that the pore size of the pore (29) For 0.3mm-0.5mm；The pore (29) is the polygonal through hole knot of circular through hole structure, ellipse hole structure or rule Structure, and the pore (29) surrounds the axle center array arrangement of collecting pipe (19).

4. agilawood essential oil decompression fractionation unit as described in claim 1, which is characterized in that the vacuum system includes diffusion pump (3) it can be connected to respectively with the diffusion pump (3) vacuum pump (4) pipeline with vacuum pump (4), the cold-trap (7)；In diffusion pump (3) The pipeline being connected to cold-trap (7) is equipped with a switch valve V7, and the other end of diffusion pump (3) connects originally sink (25), spreading The pipeline that pump (3) is connected to originally sink (25) is equipped with a switch valve V11；Connecting tube of the cold-trap (7) between vacuum system Road further includes first pipe (33) and second pipe (34), and first pipe (33) is equipped with a pressure gauge (24), pressure gauge (24) Be respectively arranged on the left side and the right side switch valve V5 and switch valve V6；First pipe (33) has the first end and second being oppositely arranged End, first end are located on the pipeline between cold-trap (7) and switch valve V7, and the second end of first pipe (33) is located at diffusion pump (3) Between switch valve V11；One end of second pipe (34) is located on the pipeline between pressure gauge (24) and switch valve V6, the other end It is connect with vacuum pump (4), second pipe (34) is equipped with switch valve V3.

5. agilawood essential oil decompression fractionation unit as described in claim 1, which is characterized in that on the tube wall of the condenser pipe (20) It is provided with the circulation port (21) of spiral through-hole structure, the entrance and exit of circulation port (21) passes through hose (11) and thermostatted water respectively Slot (10) is connected to and forms closed circulation.

6. agilawood essential oil decompression fractionation unit as described in claim 1, which is characterized in that the end of the mother tube is extend into In the distiller (12), and close to the tube wall of the distiller (12).

7. agilawood essential oil decompression fractionation unit as described in claim 1, which is characterized in that the mother tube outer cover is equipped with pre- Heat pipe (31), the upper end of the pre- hot jacket (30) and the lower end of economizer bank (31) are connected to preheater (2) respectively.

8. agilawood essential oil decompression fractionation unit as described in claim 1, which is characterized in that oil bath chamber (26) upper end is under End is connected to oil heater (6) by oil bath pipe (27) respectively, forms oil bath heating circuit.

9. agilawood essential oil decompression fractionation unit as claimed in claim 8, which is characterized in that the oil heater (6) and oil bath It is both provided with switch valve V2 on 2 pipelines of chamber (26) connection, the right end of oil heater (6) is provided with switch valve V10, switch valve Originally sink (25), the originally sink (25) are used to provide cooling tap water for oil heater (6) for the other end connection of V10.

10. agilawood essential oil decompression fractionation unit as described in claim 1, which is characterized in that the raw material tank (1) and preheater (2) it is closed connection between, forms closed air preheat circuit, and is arranged between raw material tank (1) and distiller (12) useful In the switch valve V8 of control channel open or close.