CN101358157B - Method for extracting cinnamon oil using fluidized-bed and apparatus thereof - Google Patents
Method for extracting cinnamon oil using fluidized-bed and apparatus thereof Download PDFInfo
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Abstract
The present invention discloses a method for abstracting cassia oil by using a fluidized bed and a device thereof. The method uses steam as fluidizing agent, cinnamon leaves are fiercely stirred in the fluidized bed, so that the cinnamon leaves contacted with steam can be constantly refreshed, thus the oil yield of the cinnamon leaves is increased. The device mainly comprises a steam generator, the fluidized bed, a condenser and an oil-water separator; wherein, the steam generator is connected with an air inlet on the lower side of the fluidized bed; an outlet on the top of the fluidized bed is connected with the input end of the condenser; the output end of the condenser is connected with the inlet of the oil-water separator; a distribution plate, which is used to uniformly distribute gas, is mounted on the bottom of the fluidized bed and positioned over the air inlet. The present invention, which has the advantages of short operation time, high oil yield, low unit energy consumption, etc., is applicable to the abstraction of substances such as vegetable oils.
Description
Technical field
The present invention relates to the technical field that a kind of forest chemical trees inclusion is extracted, particularly by branch, the leaf extracted Gui oil of cassia tree or extract the Processes and apparatus of other plant fragrance wet goods extract.
Background technology
Oil of bay has very high utility value aspect food and medicine, and becomes one of important source of natural perfume.Oil of bay is the essential oil that extracts the branch, leaf or bark, seed from cassia tree, is the main converted products of xylocinnamomum.China is the big producing country of oil of bay, and wherein the oil of bay of Guangxi and Guangdong production accounts for 80% of world wide production.The annual export volume of China oil of bay is more than 1000 tons, mainly is on sale to America, country such as France, and demand constantly increases, the domestic market to the oil of bay product consumption also in continuous increase.At present, oil of bay product international market demand is 6000 tons, and the annual production of main product state China is only about 1500 tons.Therefore the production efficiency and the output that improve oil of bay are crucial for China's oil of bay industry.
Generally adopt methods such as steam distillation, volatile solvent extraction and supercritical extraction method for the extraction of oil of bay.Compare with steam distillation, volatile solvent extraction solvent residual amount height, the oil of bay product of extraction has lost natural characteristic; And also just at the experimental stage for the supercritical carbon dioxide extraction Oleum Cinnamomi, and production cost is higher, is not easy to suitability for industrialized production.So continue to use the method that water distillation stripping is got oil of bay so far always,
The principle of steam distillation: under the ebullient temperature condition, by the cinnamon leaf of boiling under thermodynamic activity, its lower boiling oil of bay composition at first blendes together one with the water that penetrates into cell and becomes steam, sees through the expansible cell walls by osmosis then, reaches the surface at last and evaporates.In order to remedy the composition of these evaporations, another part oil of bay begins to mix with water, and steams through cell walls, and moisture is from extravasating into, to remedy inner moisture loss simultaneously.This effect goes round and begins again, up to because of till improving that temperature is oozed out the whole free expansions of high boiling oil of bay composition and being taken away by water vapour.
When extracting oil of bay,, must solve two problems if will improve its oil yield with steam distillation: the one, the derived essential oil in the cassia twig leaf is as far as possible fully taken out of by steam; The 2nd, with the separated and collected as far as possible fully of the oil of bay in the phlegma.In order to improve oil yield, done the improvement of many technologies as domestic and international researchist.The oil yield of steam distillation from the fs 0.3%, develops into the present phase III, brings up to 1.0%.But still fail so far to find a kind of oil yield height and equipment is simple, the operating time is short again extraction process.
Produce by indigenous method the oil of bay device relatively with traditional, the technology of extracting oil of bay at present mainly contains following several improved technology.
1. make profit before emulsification, realize automatic oily water separation, improve the rate of recovery of oil of bay.Adopt the method for condenser upside-down mounting as Chinese patent CN1133877A, the inlet of profit steam is exactly the outlet of phlegma, guarantee that phlegma has higher temperature, emulsification does not take place in profit, under the effect of partial condenser, oil is sharp separation from phlegma soon, and oil yield reaches more than 1.2%, improves 1.5 times than common water distilling apparatus.But distillation time needs 3 hours, and the operating time, long problem was not improved.
2. change two pot series connection steam oils into by single pot of steam oil, increase water oil ratio.A kind of is that the osmanthus leaf is respectively charged into two still pots, water vapor sprays into the bottom of first still pot then, mixing steam is exported the bottom that is input to second still pot again through the top of first still pot, and then mixing steam outputs to the thermal source that the first step is heated up in a steamer do distillation distillate again through the top of second still pot.As Chinese patent CN1347971A, CN1528871A is exactly two pot series connection distillations of adopting two still pots, and oil yield reaches 1.2～1.4% like this, has improved 70～90%, has made full use of the waste heat of steam again, has improved working efficiency and has reduced power consumption.But the whole process operating time once is 80～100 minutes, and the time is still long.Another kind is the osmanthus leaf to be carried out second distillation extract oil of bay.In first still, add the osmanthus leaf, under normal pressure, be heated to boiling, steam is through condenser condenses, phlegma enters quantizer, quantizer lower floor is the oil of bay product, the upper strata is the emulsus distillate that steams, and return in the still, and the cassia twig leaf that will steam hangs out, move on in second still, second still adds clear water and carries out second distillation.The emulsus distillate that steams in first still adds new cassia twig leaf again and carries out steam distillation as part distilled water, and the branches and leaves that steamed move on to second still again, so finishes the extraction work of whole flow process with two stills.This technology has been carried out second distillation to the osmanthus leaf, but owing to after isolating oil of bay, water layer is returned still pot as the distillation water, these water layers that return still pot are saturated by perfume oil, it is slack-off to make the oil content of raw material inside be diffused into the speed on surface, oil yield is greatly reduced, so the oil yield raising is limited.
3. distillation-rectifying combines.This technology is to set up a rectifying tower between still pot and condenser, and profit steam is entered before the condenser, and the oil in the steam is concentrated, and makes the easier layering of profit, reduces emulsification.As Chinese patent CN1085939A, adopt distillation-rectifying to combine and reach 1.0～1.3% than traditional technology oil yield, improved 40～60% than not setting up rectifying tower.But not reducing the distillation procedure time, still is 3 hours, and used rectifying tower cost height is promoted relatively difficulty.
4.. adopt means such as pressure distillation, adding additive.Because the effect of additive, making oil of bay be subjected to suitable water looses and water-soluble effect, forming under the azeotrope temperature condition, phenylacroleins in the Cortex Cinnamomi powder etc. form steam with composition and the water that infiltrates oil cell, see through the expansible cell walls by osmosis, reach the surface at last and be evaporated out.Make cinnamon leaf steam to such an extent that more oil of bay comes out as far as possible like this, the cinnamic aldehyde content that records the oil of bay that this method produces through ultraviolet spectrophotometer is up to more than 95%, and the oil yield of raw material is the highest can bring up to 1.52%.
Though above several method improves the oil yield of oil of bay to a certain extent, the operating time is long and the extraction oil of bay is not thorough.Because the still pot that adopts is a fixed bed, all osmanthus leaves that water vapor can not touch, even feed water vapor for up to 2～3 hours, part osmanthus leaf is also arranged owing to can't not extract oil of bay well with water vapor acting well.Therefore, lower with traditional still pot extraction yield, time-consuming, waste energy and resource.
Summary of the invention
The objective of the invention is to overcome the prior art above shortcomings, a kind of method and device thereof that extracts oil of bay with fluidized-bed is provided, by using fluidizer to improve the oil yield of oil of bay, the specific productivity of raising extraction element is striven for more economic benefits.The present invention is achieved through the following technical solutions.
With the method for fluidized-bed extraction oil of bay, this method comprises the steps:
(1) the osmanthus leaf is joined in the fluidized-bed from injection port D;
(2) make the inlet mouth A feeding fluidized-bed of the water vapour of water vapor generating unit output from the fluidized-bed bottom; Regulate the output pressure of water vapor generation device, make Gui Ye keep fluidized state;
(3) steam with water vapor after the osmanthus leaf the contacts oil of bay with Gui Yezhong, mixing steam is transported to condenser and carries out condensation through the top exit E of fluidized-bed, and phlegma enters water-and-oil separator again to be separated, and the oil of bay of separating is positioned at the separator bottom.
In the aforesaid method, the described fluidized state of step (2) is meant: Gui Ye contacts with water vapor under suspended state, and the generation disturbance, thereby the renewal speed of the osmanthus leaf surface of quickening water vapor contact, the easier whole free expansions of the oil of bay composition of Gui Yezhong are oozed out and are taken away by water vapour.
In the aforesaid method, in the step (2), just begun when fluidized-bed input water vapour, to open the non-condensable gases in the vertical T-valve F discharge of the fluidized-bed fluidized-bed; Open the valve B of bottom again, eject the water of condensation of the pipeline between water vapor generation device and fluidized-bed.
In the aforesaid method, the granular size of the described osmanthus of step (1) leaf is 0.45～30mm, and the described water vapor generation device of step (2) is a boiler.
In the aforesaid method, regulating boiler pressure in the step (2) is 0.11～0.12MPa, and making steam flow is 17～24m
3/ h reaches the fluidizing velocity of Gui Ye, and the osmanthus leaf keeps fluidized state.
In the aforesaid method, when the osmanthus leaf was in fluidized state, the fluidized-bed bottom temp was 100～108 ℃.After the osmanthus leaf fluidized state hold-time is 20～40 minutes, and the oil of bay content mass percent of phlegma is lower than at 0.0158% o'clock, finishes to extract.
Be used to realize the device of aforesaid method, this device comprises water vapor generation device 1, fluidized-bed 4, condenser 5 and water-and-oil separator 6, described water vapor generation device 1 links to each other with the bottom inlet mouth A of fluidized-bed 4 by pipeline, the outlet E at fluidized-bed 4 tops is connected by the input terminus of pipeline with condenser 5, and the output terminal of condenser 5 is connected by the input aperture of pipeline with water-and-oil separator 6; The bottom of described fluidized-bed 4 is equipped with the grid distributor that is used for uniform distribution gas, and this grid distributor is positioned at the top of described inlet mouth A; Pipeline between described water vapor generation device 1 and the fluidized-bed 4 also is provided with under meter 2.
Described under meter 2 is provided with flow control valve, and the outside of fluidized-bed 4 also is provided with differential manometer 3, and fluidized-bed 4 also is provided with injection port D, discharge port C and top exit E, and the bottom also is provided with valve B.
Advantage of the present invention has: the present invention is the technical process of fluidized-bed water vapour distillation oil of bay, and major equipment comprises boiler, fluidizer, partial condenser and water-and-oil separator, and principal character is to be equipped with in the fluidized-bed bottom grid distributor of uniform distribution gas.As fluidizing medium, make Gui Ye that the intensive disturbance take place with water vapor, mutual friction and collision are accelerated the renewal speed of the solid surface of water vapor contact.When fluidisation under some lower fluidization gas velocity, bubble constantly changed gas by the osmanthus leaf flow state and cause particle motion, guarantee so constantly to change the osmanthus leaf that contacts, thereby make water vapor to contact with the osmanthus leaf fully rapidly with water vapor.After the osmanthus leaf reached stable fluidized state in addition, Gui Ye contacted with water vapor under suspended state, has increased the area that water vapor contacts with the osmanthus leaf greatly, and the temperature uniformity of bed.Like this when extracting oil of bay, can not make the bed local superheating and portion burns, or the low excessively extraction temperature that do not reach of local temperature.Improve the oil yield of oil of bay, improve the specific productivity of extraction element, have high economic benefit, for also general being suitable for of the extraction of vegetables oil.Heat up in a steamer technology again with existing oil of bay production and compare, the present invention can also reduce by a still kettle, has saved huge facility investment, simplifies the operation, the labour intensity that has significantly reduced.
Description of drawings
Fig. 1 is the formation synoptic diagram of apparatus of the present invention.
1 is steam-generating installation among the figure, and 2 is under meter, 3 differential manometers, and 4 is fluidized-bed, 5 condensers, 6 water-and-oil separators.A in the fluidized-bed is that inlet mouth, B are that valve, the C of bottom is that discharge port, D are that injection port, E are top exit, and F is a T-valve.
Embodiment
In conjunction with the accompanying drawings concrete enforcement of the present invention is described in detail now.
As shown in Figure 1, this device comprises water vapor generation device 1, fluidized-bed 4, condenser 5 and water-and-oil separator 6, described water vapor generation device 1 links to each other with the bottom inlet mouth A of fluidized-bed 4 by pipeline, the outlet E at fluidized-bed 4 tops is connected by the input terminus of pipeline with condenser 5, and the output terminal of condenser 5 is connected by the input aperture of pipeline with water-and-oil separator 6; The bottom of described fluidized-bed 4 is equipped with the grid distributor that is used for uniform distribution gas, and this grid distributor is positioned at the top of described inlet mouth A; Pipeline between described water vapor generation device 1 and the fluidized-bed 4 also is provided with under meter 2.Described under meter 2 is provided with flow control valve, and the outside of fluidized-bed 4 also is provided with differential manometer 3, and fluidized-bed 4 also is provided with injection port D, discharge port C and top exit E, and the bottom also is provided with valve B.
Concrete extracting method comprises following operation steps: 1. the osmanthus leaf of pulverizing is added fluidized-bed 4 device the insides from injection port.2. start steam-generating installation 1 (boiler) and discharging non-condensable gases wherein, after boiler reached setting pressure, water vapor entered from the bottom end side mouth of fluidized-bed, opened the non-condensable gases that the vertical T-valve emptying of fluidized-bed is come out from fluidized-bed then; Open the water of condensation that the threeway discharge line of bottom is come again.3. the cooling water inlet valve of open cold condenser 5 and reach and regulate the phlegma generation by regulating cooling water inflow.Regulating boiler pressure simultaneously is 0.11～0.12MPa, and making steam flow is 17～24m
3/ h reaches the fluidizing velocity of Gui Ye, makes osmanthus leaf fluidisation and keeps fluidized state.This moment, the fluidized-bed bottom temp was 100～108 ℃.4. with the water vapor after the osmanthus leaf contacts oil of bay is taken out of, and entered condenser 5 and carry out condensation, phlegma enters water-and-oil separator 6 and isolates oil of bay.5. leaf fluidized state in osmanthus kept after 30 minutes, when phlegma contains oil of bay amount less (the quality percentage composition is less than 0.0158%), but just end operation.6. the liquid that reclaims in the fluidized-bed is opened in the threeway of fluidized-bed bottom.
Compare with present fixed bed distillation technique, extract oil of bay with fluidization and have following several advantage:
(1) extraction time is short.Extraction time about present relatively wet distillation 2.5h, because fluidization technique increases particle and fluidic contact area, the collision of fierceness between particle has reduced the time that oil of bay extracts, by measuring oil yield over time, determine that the fluidization technique optimal operations time is 0.5h.Handle the osmanthus leaf of same weight, the operating time that fluidization technique extracts oil of bay shortens greatly, has improved the efficient of producing.
(2) the extraction composition is more.The oil of bay main component that fluidized-bed and bed technology are extracted all is by phenylacrolein, 2,4,5-trimethoxy-1-propenylbenzene, o-methoxy cinnamic aldehyde, 2,4,5-trimethoxy-1-propenylbenzene, 20 carbon saturated fatty acids, tonka bean camphor, o-methoxy cinnamic aldehyde are formed.The wherein difficult evaporable material of oil of bay that extracts with fluidization is as 2,4, and the content of 5-trimethoxy-1-propenylbenzene is many, and extracts multiple difficult evaporable material.This is that the service temperature of fluidized-bed is 104～105 ℃ because the service temperature of fixed bed is 100 ℃.Higher service temperature from the angle analysis of mass transfer, more helps the diffusion of oil of bay, makes some difficult evaporable compositions of Gui Yezhong extract the percentage composition that increases difficult evaporable composition.
(3) oil yield height.Relatively fixed bed and fluidization are at the oil yield that extracts oil of bay, and the oil yield of fixed bed is 1.363%, and the oil yield of fluidized-bed is 2.336%, and oil yield has improved 70% on original basis.A medium-sized factory produces 40 tons of oil of bays per year, and pressing oil yield increases by 70% calculating, can increase by 28 tons of oil of bays every year.The price of oil of bay is 120,000 yuan/ton at present, utilizes fluidization technique can have a net increase of 3,360,000 yuan of benefits.
Be case study on implementation of the present invention below, test according to above-mentioned flow process and following processing condition, specific as follows:
1. osmanthus leaf charge amount: 200g, granular size 0.45～0.9mm, osmanthus leaf water content are 6.872%.During osmanthus leaf critical fluidization velocity, the flow 18m of water vapor
3/ h, other parameter is as shown in table 1.
Table 1
| Extract the device of oil of bay | Charge amount (g) | Pressure (MPa) | Temperature (℃) | Distillation time (min) | Oil pump capacity (g) | Oil yield (%) |
| Fixed bed device | 200 | 0.101 | 100 | 50 | 2.62 | 1.31 |
| Fluidizer | 200 | 0.111 | 103 | 30 | 5.08 | 2.54 |
2. osmanthus leaf charge amount: 200g, granular size 0.9～2mm.During osmanthus leaf critical fluidization velocity, the flow 23m of water vapor
3/ h, other parameter is as shown in table 2.
Table 2
| Extract the device of oil of bay | Charge amount (g) | Pressure (MPa) | Temperature (℃) | Distillation time (min) | Oil pump capacity (g) | Oil yield (%) |
| Fixed bed device | 200 | 0.101 | 100 | 50 | 2.84 | 1.42 |
| Fluidizer | 200 | 0.116 | 104 | 30 | 4.28 | 2.14 |
| Fluidizer | 200 | 0.121 | 105 | 30 | 4.66 | 2.33 |
3. osmanthus leaf charge amount: 200g, granular size 2～30mm.During osmanthus leaf critical fluidization velocity, the flow 25m of water vapor
3/ h, other parameter is as shown in table 3.
Table 3
| Extract the device of oil of bay | Charge amount (g) | Pressure (MPa) | Temperature (℃) | Distillation time (min) | Oil pump capacity (g) | Oil yield (%) |
| Fixed bed device | 200 | 0.101 | 100 | 50 | 1.50 | 0.75 |
| Fluidizer | 200 | 0.111 | 103 | 30 | 2.70 | 1.35 |
From embodiment 1, be the osmanthus leaf of 0.45～0.9mm as can be seen for granular size, improve oil yield 93% behind the use fluidization technique.In theory, the easy more composition Gui Yezhong of the more little water vapor of particle extracts, but its oil yield of water vapor extracting method under fixed bed device is not high, mainly be because particle is more little, requirement for charging is high more, because particle Xiao Gui leaf is more piled up closely more, be unfavorable for that water vapor contacts with the osmanthus leaf to extract oil of bay.Then for the not bigger requirement of short grained charging method, in fluid mapper process, can eliminate the osmanthus leaf with fluidization technique because the tight formed dead band that can not contact of the little accumulation of particle with water vapor.
From embodiment 2, the document record uses fluidization technique also can improve oil yield 51%～64% than the particle 0.9～2mm of high oil recovery as can be seen.
From embodiment 3, granular size 2～30mm mainly is vein and the leaf branch of Gui Ye, also can reach oil yield preferably.
Therefore, the present invention has reached the effect of anticipation, after using fluidization technique that the osmanthus leaf is extracted oil of bay (particular flow sheet is seen appendix), its oil yield is improved greatly.Owing to use fluidizer, all osmanthus leaves can both contact with water vapor, and temperature is even, has reduced the too high oil of bay pyrolysis that causes of local temperature, the loss of hydrolysis.Here it is extracts the high major cause of oil of bay oil yield with fluidization technique.
Claims (9)
1. extract the method for oil of bay with fluidized-bed, it is characterized in that comprising the steps:
(1) from injection port, join the osmanthus leaf in the fluidized-bed;
(2) make the inlet mouth feeding fluidized-bed of the water vapour of water vapor generating unit output from the fluidized-bed bottom; Regulate the output pressure of water vapor generation device, make Gui Ye keep fluidized state;
(3) steam with water vapor after the osmanthus leaf the contacts oil of bay with Gui Yezhong, mixing steam is transported to condenser through the top exit of fluidized-bed and carries out condensation, and phlegma enters water-and-oil separator again to be separated, and the oil of bay of separating is positioned at the separator bottom.
2. method according to claim 1, it is characterized in that the described fluidized state of step (2) is meant: Gui Ye contacts with water vapor under suspended state, and disturbance takes place.
3. method according to claim 1 is characterized in that in the step (2), has just begun to open the non-condensable gases in the vertical T-valve discharge of the fluidized-bed fluidized-bed when fluidized-bed input water vapour; Open the valve of bottom again, eject the water of condensation of the pipeline between water vapor generation device and fluidized-bed.
4. according to each described method of claim 1～3, it is characterized in that the granular size of the described osmanthus of step (1) leaf is 0.45～30mm, the described water vapor generation device of step (2) is a boiler.
5. method according to claim 4 is characterized in that in the step (2), the adjusting boiler pressure is 0.11～0.12MPa, and making steam flow is 17～24m
3/ h reaches the fluidizing velocity of Gui Ye, makes Gui Ye keep fluidized state.
6. method according to claim 5 is characterized in that when the osmanthus leaf is in fluidized state the fluidized-bed bottom temp is 100～108 ℃.
7. method according to claim 5, it is characterized in that the osmanthus leaf fluidized state hold-time is 20～40 minutes after, and the oil of bay content mass percent of phlegma is lower than at 0.0158% o'clock, finishes to extract.
8. device that is used to realize the described method of claim 1, it is characterized in that this device comprises water vapor generation device (1), fluidized-bed (4), condenser (5) and water-and-oil separator (6), described water vapor generation device (1) links to each other by the bottom inlet mouth of pipeline with fluidized-bed (4), the outlet at fluidized-bed (4) top is connected by the input terminus of pipeline with condenser (5), and the output terminal of condenser (5) is connected by the input aperture of pipeline with water-and-oil separator (6); The bottom of described fluidized-bed (4) is equipped with the grid distributor that is used for uniform distribution gas, and this grid distributor is positioned at the top of described inlet mouth; Pipeline between described water vapor generation device (1) and the fluidized-bed (4) also is provided with under meter (2).
9. device according to claim 8 is characterized in that described under meter (2) is provided with flow control valve, and the outside of fluidized-bed (4) also is provided with differential manometer (3), and fluidized-bed (4) also is provided with injection port, discharge port and top exit, and the bottom also is provided with valve.
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| CN102295992B (en) * | 2010-06-23 | 2012-11-07 | 新疆天然芳香农业科技有限公司 | Plant essence gradient extraction device |
| CN102978001B (en) * | 2012-12-06 | 2013-09-25 | 广西京桂香料有限公司 | Natural cassia oil condenser |
| CN103215137B (en) * | 2013-05-08 | 2014-11-05 | 宜宾学院 | Method for continuously distilling aromatic oil by subsectional temperature control |
| CN116179266B (en) * | 2023-04-26 | 2023-07-18 | 烟台南山学院 | Whale oil extraction equipment and extraction method for stranded whales |
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Non-Patent Citations (1)
| Title |
|---|
| 高福成.固体颗粒的流化态原理.《现代食品工程高新技术》.中国轻工业出版社,1997,(第1版),528-531. * |
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