CN1029319C - Process and equipment for extracting bay oil by combination of distillation and rectification - Google Patents
Process and equipment for extracting bay oil by combination of distillation and rectification Download PDFInfo
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- CN1029319C CN1029319C CN 92112176 CN92112176A CN1029319C CN 1029319 C CN1029319 C CN 1029319C CN 92112176 CN92112176 CN 92112176 CN 92112176 A CN92112176 A CN 92112176A CN 1029319 C CN1029319 C CN 1029319C
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Abstract
The present invention relates to a process and devices for extracting bay oil by combining the steps of distillation and rectification, which belongs to the technical field of refined chemical industry separation. A distillation kettle, an oil increasing device for rectification, a condenser and an oil water separator are used in the process. The present invention has the advantages of simple process, small devices and easy operation, and the oil yield can be increased to 20% to 60%. The bay oil extracted by the process can be widely applied to fragrant essential oil systems which have water solubility and emulsibility.
Description
The extraction oil of bay technology that the present invention combines for distillation-rectifying belongs to the fine chemistry industry separation field.
Because the solvability and the emulsifying property of oil of bay are strong, and with the density difference of water only be 0.05, thereby make oil of bay leaching process yield low, generally have only the 50%-60% of actual oil length.There is oil about 40% to be deposited in the branches and leaves or is dissolved in the water, or form emulsification with water and get to come out.At present, improve to some extent though extract the technology of oil of bay both at home and abroad, basic ideas are recovery part oil of bays from the distilled water of the emulsification shape that steams.Improved the 1st kind of method is steam distillation and adds emulsion splitter bonded method.Add emulsion splitter and can make the emulsion flocking settling that steams, recovery part oil of bay; The steam distilled equipment of ortho-water mainly contains three parts: 1. still kettle; 2. condenser; 3. oil-water decanter, its schematic flow sheet is shown in figure ().With the cassia twig leaf still kettle 1 of packing into, add 3-4 water doubly again, under normal pressure, be heated to boiling, water vapor is taken the oil of bay in the branches and leaves out of, and the steam that contains oil of bay is through condenser 2 condensations, and the gained phlegma enters the water-and-oil separator layering, oil reservoir is the oil of bay product, still contain a small amount of oil of bay in the water layer, be milky white shape, return in the still kettle.In order to reclaim the oil of bay in the oyster white distilled water, the someone adopts the measure that adds emulsion splitter, and emulsion splitter is added in the water-and-oil separator to alleviate emulsion, emulsified oil of bay is partly condensed separate out, thereby improve the oil yield of oil of bay.But this method is difficult in the selection of emulsifying agent, and demulsification is generally not ideal enough, thereby the oil yield raising is limited.
The 2nd kind of improved method is multistage settlement separate extraction oil of bay flow process.Its major equipment is made up of still kettle, condenser and tens sedimentation cylinders, and its flow process is shown in figure (two).The cassia twig leaf is put into still, still kettle 4(1)-add water again in 4(4), under normal pressure, be heated to boiling then, contain oil vapour and enter condenser 5(1) condensation, phlegma enters 6(1)-6(4) in numbers 4 sedimentation cylinders, sedimentation 48 hours is taken out lower floor's oil of bay and is product.The water of its upper strata emulsification shape is squeezed into still kettle 4(2) in make distilled water and use, put into new branches and leaves in the still, after several hours with 6(5)-6(8) water on cylinder upper strata is squeezed into still 4(3) in, after several hours, with 6(9)-6(12) water on cylinder upper strata is squeezed into still kettle 4(4) in make distilled water and carry out steam distillation with just putting into the cassia twig leaf in turn by these four stills, handle emulsion in turn with 12 cylinders, part emulsification and dissolved oil of bay are reclaimed.
The 3rd kind of improved technology is extracted the oil of bay technology second distillation.This improved technology is that the cassia twig leaf is carried out second distillation, see figure (three), in first still, add the cassia twig leaf, add water again, under normal pressure, be heated to boiling, steam is through condenser condenses, phlegma enters quantizer, quantizer lower floor is that oil of bay product, upper strata are 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.Among the figure (three), 7 is still kettle, and 8 is condenser, and 9 is water-and-oil separator.Entire operation is all carried out under normal pressure.
Though more than several technology can partially recycled oil of bay, and improve the oil yield of oil of bay to a certain extent, it is very complicated that equipment and flow process become, and it is not thorough to reclaim oil of bay.
The objective of the invention is to improve the oil yield of oil, simultaneously simplified apparatus and flow process.
The present invention extracts the oil of bay technical process for distillation-rectifying combines.Equipment comprises still kettle, condenser and water-and-oil separator, and principal character is to have increased the oil increasing device that rectifying is used between still kettle and condenser, and oil increasing device essence mainly is a rectifying tower, and theoretical plate number is the 3-20 piece, and gas speed is 0.2-2.0m/s.
Describe the present invention in conjunction with the accompanying drawings now.Accompanying drawing (four) is technical process of the present invention, and 10 is still kettle among the figure, and 11 is oil increasing device, and 12 is condenser, and 13 is water-and-oil separator.The cassia twig leaf is put into still kettle 10, add 3～4 times water, under normal pressure, heat, make the water boiling, water vapor is taken the oil of bay in the cassia twig leaf out of, and enters oil increasing device 11 and carry out rectifying, and oil of bay is thickened, the oil increasing device bottom temp is 100 ℃～110 ℃, resistance is reduced to 30～100 millimeter water column, and the steam after concentrating enters condenser 12 condensations, and phlegma enters water-and-oil separator 13, upper strata distilled water goes back to oil increasing device 11 tops and refluxes, and lower floor is effusive to be the oil of bay product.
Be embodiments of the invention below, test according to above-mentioned flow process and following processing condition, specific as follows:
1. raw material: autumn leaves, charge amount: 250g, atmospheric operation, 103 ℃ of oil increasing device bottom temps, resistance is reduced to the 40mm water column, 6 of number of theoretical plates, gas speed 0.7m/s～1m/s.
Distillation time (min) oil pump capacity (g) oil yield (%) mean value (%)
180 3.2 1.28
Add oil increasing device
180 3.3 1.32 1.30
180 2.15 0.86
Do not add oil increasing device
180 2.2 0.88 0.87
(1.3-0.87)/0.87=0.49, add and improve oil yield 49% behind the oil increasing device.
2. raw material: the spring leaf, charge amount: 250g, 102 ℃ of oil increasing device bottom temps, resistance is reduced to the 30mm post, 6 of number of theoretical plates, gas speed 0.7m/s
Distillation time (min) oil pump capacity (g) oil yield (%) mean value (%)
180 2.65 1.05
Add oil increasing device
180 2.5 1.00 1.025
180 1.52 0.608
Do not add oil increasing device
180 1.50 0.60 0.604
(1.025-0.604)/0.604=0.697, add that oil yield improves 69.7% behind the oil increasing device.
3. raw material: spring leaf, charge amount: 250g, atmospheric operation, 104 ℃ of oil increasing device bottom temps, resistance drop 50mm post, 10 of number of theoretical plates, gas speed 0.7m/s.
Distillation time (min) oil pump capacity (g) oil yield (%)
180 1.5 0.6
Do not add oil increasing device
180 1.51 0.60
180 2.80 1.12
Add oil increasing device
180 3.00 1.20
(1.16-0.6)/0.6=0.933, add that oil yield improves 93.3% behind the oil increasing device.
The present invention has reached and has given the effect of thinking, owing to added oil increasing device, the flow process that has adopted distillation-rectifying to combine, make and contain oil vapour and concentrated, make the easy layering of profit, reduced simultaneously the oil of bay content in the still liquid, like this, when the vaporization of still liquid enters the bed of material, the concentration of oil reduces in the steam, thereby mass transfer force is increased, in addition, because oil of bay content in the still has also reduced the oil of bay loss that causes owing to pyrolysis, hydrolysis. Here it is adds the main cause that improves oil yield behind the oil increasing device. Compare with the improved technology in front, the present invention need not reclaim a small amount of oil of bay with 12 vats, because it is not to reclaim oil of bay by mechanical sedimentation again after oil of bay emulsification, but the oil in the steam is concentrated, make the easy layering of profit, thereby reduce emulsification. So just save huge equipment investment, also simplified operation.
Compare with aforesaid second distillation technology, also have at 2 than its advanced person. The second distillation technology is that the branches and leaves that first still steamed are moved into second still, and this is the secondary concentrate, and the present invention is multistage concentrate with an oil increasing device, thereby concentrated effect of the present invention is more much better than it. In addition, industrial, the former steams the branches and leaves of going over the first still 500kg to move on to second still again, and this has not only increased labour intensity, and makes the operation complicated, and the present invention need not to carry out such operation.
In sum, the present invention has obvious superiority than existing technology, and its enrichment effect is big, thereby the oil yield height, and easy and simple to handle, equipment is small and exquisite.
We are through up to a hundred experiments, and result's proof adds oil increasing device and can increase substantially oil yield, approximately can increase oil yield 20%-60%.
With the autumn leaves is that raw material compares experiment, after adding oil increasing device, oil yield increases by 49% than former technology, is that raw material is done the contrast experiment with the spring leaf, oil yield increases by 69% than former technology after adding oil increasing device, and oil pump capacity doubled than former technology after the commerical test proof of carrying out in certain perfumery added oil increasing device.
From a series of laboratories lab scale and plant-scale test, prove that all the present invention has advantages such as the high equipment of oil yield is simple, easy to operate.The present invention has high economic benefit, and has broad application prospects, and the volatile oil system of, emulsifying property water-soluble for having is that some essential oil of phenols, alcohols, acids all can adopt this invention for main component.
Claims (2)
1, the method for the extraction oil of bay that combines of a kind of distillation-rectifying comprises: the cassia twig leaf is put into still kettle 10, add 3～4 times of water, under normal pressure, heat, make the water boiling, water vapor is taken the oil of bay in the cassia twig leaf out of, and enter oil increasing device 11 and carry out rectifying, oil of bay is thickened, the oil increasing device bottom temp is 100～110 ℃, resistance is reduced to 30～100 mmhg, and the steam after concentrating enters condenser 12 condensations, and phlegma enters water-and-oil separator 13, upper strata distilled water goes back to oil increasing device 11 tops and refluxes, and lower floor is effusive to be the oil of bay product.
2, the system of the extraction oil of bay that combines of a kind of distillation-rectifying, the water-and-oil separator that contains the method for still kettle, condenser and enforcement claim 1, it is characterized in that having increased between still kettle and the condenser oil increasing device that carries out rectifying, an i.e. rectifying tower, the number of theoretical plate of oil increasing device is 3～20, and gas speed is 0.2 to 2m/s.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 92112176 CN1029319C (en) | 1992-10-21 | 1992-10-21 | Process and equipment for extracting bay oil by combination of distillation and rectification |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 92112176 CN1029319C (en) | 1992-10-21 | 1992-10-21 | Process and equipment for extracting bay oil by combination of distillation and rectification |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1085939A CN1085939A (en) | 1994-04-27 |
| CN1029319C true CN1029319C (en) | 1995-07-12 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 92112176 Expired - Fee Related CN1029319C (en) | 1992-10-21 | 1992-10-21 | Process and equipment for extracting bay oil by combination of distillation and rectification |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1029319C (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1045619C (en) * | 1996-02-16 | 1999-10-13 | 广西农业大学林学院 | Distillating process and apparatus for quick separation of bay oil |
| CN101530674B (en) * | 2009-03-16 | 2015-09-02 | 王艺瑾 | Unit-combination type extracts technique and the device of Effective Component of Chinese Medicine |
| CN109207266A (en) * | 2018-11-09 | 2019-01-15 | 广西科技师范学院 | A kind of extracting method of rose ethereal oil |
| CN110194991A (en) * | 2019-03-06 | 2019-09-03 | 上海市南洋模范中学 | Extracting method, equipment and the application of Bergamot |
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1992
- 1992-10-21 CN CN 92112176 patent/CN1029319C/en not_active Expired - Fee Related
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| Publication number | Publication date |
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| CN1085939A (en) | 1994-04-27 |
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| C15 | Extension of patent right duration from 15 to 20 years for appl. with date before 31.12.1992 and still valid on 11.12.2001 (patent law change 1993) | ||
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| C19 | Lapse of patent right due to non-payment of the annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |