CN102504955B - Processing for extracting and purifying eucalyptus oil - Google Patents
Processing for extracting and purifying eucalyptus oil Download PDFInfo
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- 239000010642 eucalyptus oil Substances 0.000 title claims abstract description 60
- 229940044949 eucalyptus oil Drugs 0.000 title claims abstract description 60
- 229960005233 cineole Drugs 0.000 claims abstract description 70
- 238000000034 method Methods 0.000 claims abstract description 59
- 238000010992 reflux Methods 0.000 claims abstract description 53
- GRWFGVWFFZKLTI-IUCAKERBSA-N 1S,5S-(-)-alpha-Pinene Natural products CC1=CC[C@@H]2C(C)(C)[C@H]1C2 GRWFGVWFFZKLTI-IUCAKERBSA-N 0.000 claims abstract description 50
- GRWFGVWFFZKLTI-UHFFFAOYSA-N α-pinene Chemical compound CC1=CCC2C(C)(C)C1C2 GRWFGVWFFZKLTI-UHFFFAOYSA-N 0.000 claims abstract description 28
- MVNCAPSFBDBCGF-UHFFFAOYSA-N alpha-pinene Natural products CC1=CCC23C1CC2C3(C)C MVNCAPSFBDBCGF-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000000470 constituent Substances 0.000 claims description 24
- 239000007788 liquid Substances 0.000 claims description 20
- 239000012752 auxiliary agent Substances 0.000 claims description 18
- 239000000284 extract Substances 0.000 claims description 12
- 238000009833 condensation Methods 0.000 claims description 9
- 230000005494 condensation Effects 0.000 claims description 9
- 230000000630 rising effect Effects 0.000 claims description 9
- 238000004821 distillation Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000004458 analytical method Methods 0.000 claims description 2
- 238000005070 sampling Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims 1
- WEEGYLXZBRQIMU-UHFFFAOYSA-N 1,8-cineole Natural products C1CC2CCC1(C)OC2(C)C WEEGYLXZBRQIMU-UHFFFAOYSA-N 0.000 abstract description 13
- 238000004519 manufacturing process Methods 0.000 abstract description 9
- WEEGYLXZBRQIMU-WAAGHKOSSA-N Eucalyptol Chemical compound C1C[C@H]2CC[C@]1(C)OC2(C)C WEEGYLXZBRQIMU-WAAGHKOSSA-N 0.000 abstract description 8
- 239000006227 byproduct Substances 0.000 abstract description 5
- 238000011112 process operation Methods 0.000 abstract 1
- 239000000047 product Substances 0.000 description 21
- 244000166124 Eucalyptus globulus Species 0.000 description 10
- 238000011084 recovery Methods 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 239000003921 oil Substances 0.000 description 6
- RFFOTVCVTJUTAD-UHFFFAOYSA-N cineole Natural products C1CC2(C)CCC1(C(C)C)O2 RFFOTVCVTJUTAD-UHFFFAOYSA-N 0.000 description 5
- 235000004692 Eucalyptus globulus Nutrition 0.000 description 4
- 235000019134 Eucalyptus tereticornis Nutrition 0.000 description 4
- 238000002203 pretreatment Methods 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- YKFLAYDHMOASIY-UHFFFAOYSA-N γ-terpinene Chemical compound CC(C)C1=CCC(C)=CC1 YKFLAYDHMOASIY-UHFFFAOYSA-N 0.000 description 4
- 239000000203 mixture Substances 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 2
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- UAHWPYUMFXYFJY-UHFFFAOYSA-N beta-myrcene Chemical compound CC(C)=CCCC(=C)C=C UAHWPYUMFXYFJY-UHFFFAOYSA-N 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000005194 fractionation Methods 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000004615 ingredient Substances 0.000 description 2
- XMGQYMWWDOXHJM-UHFFFAOYSA-N limonene Chemical compound CC(=C)C1CCC(C)=CC1 XMGQYMWWDOXHJM-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229930014626 natural product Natural products 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 239000000341 volatile oil Substances 0.000 description 2
- OGLDWXZKYODSOB-UHFFFAOYSA-N α-phellandrene Chemical compound CC(C)C1CC=C(C)C=C1 OGLDWXZKYODSOB-UHFFFAOYSA-N 0.000 description 2
- WTARULDDTDQWMU-RKDXNWHRSA-N (+)-β-pinene Chemical compound C1[C@H]2C(C)(C)[C@@H]1CCC2=C WTARULDDTDQWMU-RKDXNWHRSA-N 0.000 description 1
- WTARULDDTDQWMU-IUCAKERBSA-N (-)-Nopinene Natural products C1[C@@H]2C(C)(C)[C@H]1CCC2=C WTARULDDTDQWMU-IUCAKERBSA-N 0.000 description 1
- 108010023832 Florigen Proteins 0.000 description 1
- WTARULDDTDQWMU-UHFFFAOYSA-N Pseudopinene Natural products C1C2C(C)(C)C1CCC2=C WTARULDDTDQWMU-UHFFFAOYSA-N 0.000 description 1
- XCPQUQHBVVXMRQ-UHFFFAOYSA-N alpha-Fenchene Natural products C1CC2C(=C)CC1C2(C)C XCPQUQHBVVXMRQ-UHFFFAOYSA-N 0.000 description 1
- VYBREYKSZAROCT-UHFFFAOYSA-N alpha-myrcene Natural products CC(=C)CCCC(=C)C=C VYBREYKSZAROCT-UHFFFAOYSA-N 0.000 description 1
- OGLDWXZKYODSOB-SNVBAGLBSA-N alpha-phellandrene Natural products CC(C)[C@H]1CC=C(C)C=C1 OGLDWXZKYODSOB-SNVBAGLBSA-N 0.000 description 1
- 229930006722 beta-pinene Natural products 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000010960 commercial process Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000000294 eucalyptus globulus labille leaf/twig oil Substances 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 230000001261 florigenic effect Effects 0.000 description 1
- LCWMKIHBLJLORW-UHFFFAOYSA-N gamma-carene Natural products C1CC(=C)CC2C(C)(C)C21 LCWMKIHBLJLORW-UHFFFAOYSA-N 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 229940087305 limonene Drugs 0.000 description 1
- 235000001510 limonene Nutrition 0.000 description 1
- CDOSHBSSFJOMGT-UHFFFAOYSA-N linalool Chemical compound CC(C)=CCCC(C)(O)C=C CDOSHBSSFJOMGT-UHFFFAOYSA-N 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- HFPZCAJZSCWRBC-UHFFFAOYSA-N p-cymene Chemical compound CC(C)C1=CC=C(C)C=C1 HFPZCAJZSCWRBC-UHFFFAOYSA-N 0.000 description 1
- 239000002304 perfume Substances 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000012264 purified product Substances 0.000 description 1
- 238000010898 silica gel chromatography Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 235000013599 spices Nutrition 0.000 description 1
- 238000000194 supercritical-fluid extraction Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
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- Fats And Perfumes (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a process for extracting and purifying eucalyptus oil. High-purity eucalyptus oil is extracted by performing vacuum intermittent rectification under the assistance of an aid; separating efficiency is increased by changing the thermodynamic property of an eucalyptus oil system in a way of adding an aid under the condition of not greatly changing the conventional rectification process, and high-purity eucalyptol and alpha-pinene serving as a byproduct are extracted by adjusting reflux ratio and tower kettle temperature; and the content of the extracted eucalyptol is higher than 90 percent, and can be up to 96.50 percent in maximum, the yield is over 75 percent, the production period is within six hours, process operation is simple, a production process is stable, a byproduct containing about 80 percent of alpha-pinene is obtained simultaneously, and the added value of crude eucalyptus oil is increased.
Description
Technical field
The present invention relates to the isolation technique of natural perfume oils high purity product, more particularly, relate to a kind of eucalyptus
Leaf oil extracts the technique of purifying.
Background technology
Eucalyptus oil is the volatile oil of eucalyptus leaves oil droplet emiocytosis, is the mixture containing multiple organic composition.Eucalyptus oil can be divided three classes according to major ingredient and purposes: medicine, spices and technical oils.Wherein the most important thing is pharmaceutical eucalyptus oil, its major ingredient is 1,8-eucalyptol.
The thick eucalyptus oil impurity of natural product is many, wherein take α-pinene as main, also has a small amount of beta-pinene, myrcene, α-phellandrene, limonene, to poly-loose florigen, γ-terpinene, phantol etc.Plurality of impurities and 1,8-eucalyptol are that isomers or molecular structure and molecular weight are very approaching, have similar physicochemical property, for the purification of eucalyptol has brought very large difficulty.Literature research shows, the method for separated eucalyptol has a variety of, as supercritical extraction, silica gel column chromatography, chemical reaction method, catalytic rectification process, the crystallizing process under low temperature, film-falling crystallization method etc.
Rectificating method, because technique is simple, commercial process is ripe, has become the Main Means of the natural products such as purification eucalyptol.Chinese patent (CN1181415) discloses a kind of volatile oil extracted from eucalyptus' leaves or twigs double tower continuous treating method, the method is first carried out pre-treatment 1 ~ 5 hour to eucalyptus oil under high temperature (100 ~ 250 ℃) and high pressure (2 ~ 10kg/cm2), again pre-treatment eucalyptus oil is carried out to rectifying by continuous rectifying tower, wherein the still raffinate of First tower carries out rectifying as second tower raw material, finally from the light constituent of second, collects cineole content at 70 ~ 83% eucalyptus oil.Although be two tower continuous rectifications, but still belong to batch fractionating, compared with the batch fractionating towers that increase more, and need the pre-treatment step through air lift and fore-distillation early stage, increased production cost, produced unnecessary energy consumption, make the production cycle elongated, cost increases, the product of producing be all cineole content below 80%, and yield is on the low side.
Chinese patent (101899361A) uses a kind of single-tower continuous rectification method of eucalyptus oil, and the Eucalyptus Globulus oil of cineole content 62.5% of take is raw material, takes continuously feeding discharging.At the material such as the continuous extraction light constituent in different products export places, cineole, still be residual.According to the content situation of adopting outlet material, by adjusting reflux ratio, controlling distillation temperature, extract the eucalyptus oil of different eucalyptus oil content.The cineole content gathering reaches as high as 92%, and 10 tons/day of raw material day outputs are produced consume and are less than or equal to 1%, 80% eucalyptus oil yield and reach more than 75%.This method day output is large, and the quality of production is stable, and production loss is less, simple to operate.But this method main product is 80% eucalyptol, though can reach high-content 92%, the in the situation that of limited tower height; single-tower continuous rectification cannot make more highly purified product, and product yield is on the low side, cannot large-scale production; if increase tower height, can produce too much energy consumption.And in continuous rectification process, by adjusting reflux ratio and distillation temperature, control product purity, certainly will cause whole continuous unstablely, make the distillation operation process complexity that becomes.
Chinese patent (CN101307058A) and Chinese patent (CN201276512Y) have been invented a kind of novel separation column, in the situation that keeping former processing condition, by heat interchanging area is set between separation column partial condenser and fractionation tower top, be 50 ~ 70% condensing reflux passage.The heat-exchanging tube bundle consistent with the gas flow of tower be evenly set on tube sheet tower tray.The stringing area of tube bank is tray area 35%.Reach the volatile quantity that reduces γ-terpinene and Paracymene.Expanded the relative volatility of each component in eucalyptus oil.Make a fractionation eucalyptol content reach 80%, stable process conditions.But the product content that this device is produced mostly, between 80% ~ 83%, is not suitable for producing highly purified eucalyptol.
Summary of the invention
The present invention overcomes the deficiencies in the prior art, aim to provide the technique that a kind of eucalyptus oil extracts purifying, this technique is in the situation that little amplitude changes traditional rectification process, synergistic effect by auxiliary agent, the thermodynamic property of change system, thus make production technique simple, shorten preparation cycle, reduce production loss, obtain 1 of high-purity high-yield, 8-eucalyptol; In rectifying, collect by product α-pinene, improve the added value of the thick oil of folium eucalypti.
The present invention adopts following technical scheme to be achieved:
(1) eucalyptus oil stoste and auxiliary agent are evenly mixed by certain ratio;
(2) in tower reactor, add the solution that proportioning is good, open vacuum pump and overhead condensation device, make the vacuum tightness of distillation system reach processing requirement stable;
(3) when setting tower reactor temperature and reach processing requirement, carry out total reflux operation;
(4) eucalyptus oil is collected, and first adopts large reflux ratio to collect in eucalyptus oil system and take α-pinene as main light constituent, after light constituent is collected completely, rising tower reactor temperature, reduces reflux ratio and collects 1,8-eucalyptol, treat 1,8-eucalyptol content is during lower than processing requirement, then improves reflux ratio and collect 1,8-eucalyptol, until cannot reaching processing requirement, product content stops gathering, finally merge containing 1,8-eucalyptol and collect liquid, obtain eucalyptus oil.
The stoste of eucalyptus oil described in the present invention is that 1,8-eucalyptol content is 58%～63%(mass percent,
Eucalyptus oil down together), auxiliary agent is C
2～C
4alcohols, the addition of auxiliary agent accounts for 5～10% of the former liquid measure of eucalyptus oil.
The vacuum tightness of distillation system described in the present invention is 1.0～4.0KPa.
The type of heating of tower reactor described in the present invention is electrically heated or steam indirect heating, and tower reactor temperature is 50 ℃～65 ℃, total reflux 30 minutes.
Eucalyptus oil described in the present invention is collected, and first adopts large reflux ratio to collect in eucalyptus oil system and take α-pinene as main light constituent, and reflux ratio is 20～30, collects light constituent and makes α-pinene content in tower bottoms be less than 5%; Then the tower reactor that raises temperature to 65 ℃～80 ℃, reflux ratio is reduced to 10～15, collects 1,8-eucalyptol, and collect 1,8-eucalyptol content can not be lower than 90.00%, gather after 60～90 minutes, every 15 minutes sampling analysis, treat 1 in sample, 8-eucalyptol content is lower than 90.00% time, improving reflux ratio is 15～20, collects 1,8-eucalyptol, and in collection liquid 1,8-eucalyptol content is not less than 90.00%; Until in collection product 1,8-eucalyptol content cannot reach 90.00% to be stopped gathering when above, finally merge collect containing 1,8-eucalyptol liquid.
The present invention has used the method for auxiliary agent assisted vacuum batch fractionating 1, the 8-eucalyptol of purifying from eucalyptus oil.Eucalyptus oil has strong thermo-sensitivity, and rectification under vacuum can make the boiling point lowering of eucalyptus oil system, guarantees that polymerization does not occur stock liquid.Batch fractionating technique is simple, flexible operation, is applicable to the separation requirement of mixed solution compared with situation high and that feed liquid kind or composition often change.Add auxiliary agent and changed the relative volatility between eucalyptus oil system, improved separation efficiency; And in technique, take varying reflux ratio operation, guaranteed high purity and the high yield of product.
The present invention is with respect to advantage and the technique effect of prior art:
1, the present invention only needs single tower, and stock liquid, without pre-treatment, has been saved production and equipment operation cost, and technique is simple, stable operation, and product purity and yield are far above double tower continuous rectification.
2, the present invention is by adding auxiliary agent, changed the thermodynamic property of separated system, by varying reflux ratio, operate again and the control to still temperature, improved mass-transfer efficiency, having obtained 1,8-eucalyptol content is more than 90% eucalyptus oil, constant product quality, yield is high, reaches as high as 96.50%, and yield reaches more than 75%.
3, the present invention directly changes the relative volatility between eucalyptus oil system by adding auxiliary agent, without interpolation equipment, has reduced capacity consumption, and can obtain high purity product.
4, eucalyptus oil has strong thermo-sensitivity, adopts rectification under vacuum can make eucalyptus oil separating technology move at low temperatures, both guaranteed that polymerization does not occur stock liquid, and temperature controllability is strong.
5, the batch fractionating technique that adopts is simple, flexible operation, can collect the by product α-pinene in eucalyptus oil system simultaneously, can obtain the by product containing 80% left and right α-pinene, increased the added value of the thick oil of folium eucalypti, and in technique, adopt varying reflux ratio operation, guaranteed high purity and the high yield of product.
Embodiment
Embodiment 1: the technique that this eucalyptus oil extracts purifying is to pack rectifying tower reactor into after the blue gum crude eucalyptus oil 1000g containing 63% 1,8-eucalyptol and ethanol 60g are mixed, and wherein the amount of auxiliary agent accounts for 6% of former liquid measure; Open vacuum pump and water of condensation, vacuum tightness is 1.0KPa, after vacustat, open heater switch, be heated to 50 ℃, after total reflux 30 minutes, setting reflux ratio is 20, starts to collect to take α-pinene as main light constituent, and this process continues 60 minutes, treat that in tower bottoms, α-pinene content is less than 5%, stop collecting light constituent; Regulate tower reactor temperature to 65 ℃, reflux ratio is 10, collects 1,8-eucalyptol, and this process continues 70 minutes, rising reflux ratio is 16, collects 1,8-eucalyptol, and this process continues 140 minutes, stop collecting, obtain the product containing 1,8-eucalyptol 96.50%, total recovery is 75.35%.
Embodiment 2: the technique that this eucalyptus oil extracts purifying is to pack rectifying tower reactor into after the straight-bar eucalyptus crude eucalyptus oil 1000g containing 60% 1,8-eucalyptol and ethanol 80g are mixed, and wherein the amount of auxiliary agent accounts for 8% of former liquid measure; Open vacuum pump and water of condensation, vacuum tightness is 2.0KPa, after vacustat, open heater switch, be heated to 55 ℃, after total reflux 30 minutes, reflux ratio is set as 25, starts to collect to take α-pinene as main light constituent, and this process continues 80 minutes, treat that in tower bottoms, α-pinene content is less than 5%, stop collecting light constituent; Regulate tower reactor temperature to 70 ℃, reflux ratio 12, collects 1,8-eucalyptol, and this process continues 70 minutes, and rising reflux ratio 18 is collected 1,8-eucalyptol, and this process continues 150 minutes, stops collecting; Obtain the product containing 1,8-eucalyptol 93.12%, total recovery is 76.75%.
Embodiment 3: the technique that this eucalyptus oil extracts purifying is to pack rectifying tower reactor into after the blue gum crude eucalyptus oil 1000g containing 58% 1,8-eucalyptol and ethanol 100g are mixed, and wherein the amount of auxiliary agent accounts for 10% of former liquid measure; Open vacuum pump and water of condensation, vacuum tightness is 4.0KPa, after vacustat, open heater switch, be heated to 65 ℃, after total reflux 30 minutes, reflux ratio is set as 30, starts to collect to take α-pinene as main light constituent, and this process continues 90 minutes, treat that in tower bottoms, α-pinene content is less than 5%, stop collecting light constituent; Reconcile tower reactor temperature to 80 ℃, reflux ratio is 15, collects 1,8-eucalyptol, and this process continues 90 minutes, and rising reflux ratio is 20, collects 1,8-eucalyptol, and this process continues 150 minutes, stops collecting; Obtain the product containing 1,8-eucalyptol 94.34%, total recovery is 75.85%.
Embodiment 4: the technique that this eucalyptus oil extracts purifying is to pack rectifying tower reactor into after the straight-bar eucalyptus crude eucalyptus oil 1000g containing 63% 1,8-eucalyptol and Virahol 50g are mixed, and wherein the amount of auxiliary agent accounts for 5% of former liquid measure; Open vacuum pump and water of condensation, vacuum tightness is 3.0KPa, after vacustat, open heater switch, be heated to 60 ℃, after total reflux 30 minutes, reflux ratio is set as 20, starts to collect to take α-pinene as main light constituent, and this process continues 60 minutes, treat that in tower bottoms, α-pinene content is less than 5%, stop collecting light constituent; Regulate tower reactor temperature to 75 ℃, reflux ratio is 10, collects 1,8-eucalyptol, and this process continues 70 minutes, and rising reflux ratio is 15, collects 1,8-eucalyptol, and this process continues 150 minutes, stops collecting; Obtain the product containing 1,8-eucalyptol 93.34%, total recovery is 76.05%.
Embodiment 5: the technique that this eucalyptus oil extracts purifying is to pack rectifying tower reactor into after the blue gum crude eucalyptus oil 1000g containing 60% 1,8-eucalyptol and Virahol 70g are mixed, and wherein the amount of auxiliary agent accounts for former liquid measure 7%; Open vacuum pump and water of condensation, vacuum tightness is 1.0KPa, after vacustat, open heater switch, be heated to 50 ℃, after total reflux 30 minutes, setting reflux ratio is 25, starts to collect to take α-pinene as main light constituent, and this process continues 80 minutes, treat that in tower bottoms, α-pinene content is less than 5%, stop collecting light constituent; Regulate tower reactor temperature to 65 ℃, reflux ratio is 12, collects 1,8-eucalyptol, and this process continues 80 minutes, rising reflux ratio is 17, collects 1,8-eucalyptol, and this process continues 160 minutes, stop collecting, obtain the product containing 1,8-eucalyptol 94.50%, total recovery is 75.75%.
Embodiment 6: the technique that this eucalyptus oil extracts purifying is to pack rectifying tower reactor into after the straight-bar eucalyptus crude eucalyptus oil 1000g containing 59% 1,8-eucalyptol and propyl carbinol 90g are mixed, and wherein the amount of auxiliary agent accounts for 9% of former liquid measure; Open vacuum pump and water of condensation, vacuum tightness is 2.0KPa, after vacustat, open heater switch, be heated to 55 ℃, after total reflux 30 minutes, reflux ratio is set as 25, starts to collect to take α-pinene as main light constituent, and this process continues 70 minutes, treat that in tower bottoms, α-pinene content is less than 5%, stop collecting light constituent; Regulate tower reactor temperature to 70 ℃, reflux ratio 15, collects 1,8-eucalyptol, and this process continues 90 minutes, and rising reflux ratio 20 is collected 1,8-eucalyptol, and this process continues 160 minutes, stops collecting; Obtain the product containing 1,8-eucalyptol 93.12%, total recovery is 76.75%.
Embodiment 7: the technique that this eucalyptus oil extracts purifying is to pack rectifying tower reactor into after the blue gum crude eucalyptus oil 1000g containing 63% 1,8-eucalyptol and propyl carbinol 60g are mixed, and wherein the amount of auxiliary agent accounts for 6% of former liquid measure; Open vacuum pump and water of condensation, vacuum tightness is 3.0KPa, after vacustat, steam indirect heating, is heated to 60 ℃, after total reflux 30 minutes, reflux ratio is set as 20, starts to collect to take α-pinene as main light constituent, and this process continues 60 minutes, treat that in tower bottoms, α-pinene content is less than 5%, stop collecting light constituent; Reconcile tower reactor temperature to 75 ℃, reflux ratio is 12, collects 1,8-eucalyptol, and this process continues 80 minutes, and rising reflux ratio is 18, collects 1,8-eucalyptol, and this process continues 150 minutes, stops collecting; Obtain the product containing 1,8-eucalyptol 94.54%, total recovery is 75.25%.
Claims (1)
1. eucalyptus oil extracts a technique for purifying, it is characterized in that carrying out as follows:
(1) eucalyptus oil stoste and auxiliary agent are evenly mixed by certain ratio;
(2) in tower reactor, add the mixing stoste that proportioning is good, open vacuum pump and overhead condensation device, make the vacuum tightness of distillation system reach processing requirement stable;
(3) to tower reactor heating, when tower reactor temperature reaches processing requirement, carry out total reflux operation;
(4) eucalyptus oil is collected, and first adopts large reflux ratio to collect in eucalyptus oil system and take α-pinene as main light constituent, after light constituent is collected completely, rising tower reactor temperature, reduces reflux ratio and collects 1,8-eucalyptol, treat 1,8-eucalyptol content is during lower than processing requirement, then improves reflux ratio and collect 1,8-eucalyptol, until cannot reaching processing requirement, product content stops gathering, finally merge containing 1,8-eucalyptol and collect liquid, obtain eucalyptus oil;
Wherein said eucalyptus oil stoste is the eucalyptus oil containing mass percent 58%～63% 1,8-eucalyptol, and auxiliary agent is C
2～C
4alcohols, the addition of auxiliary agent accounts for 5～10% of the former liquid measure of eucalyptus oil;
The vacuum tightness of described distillation system is 1.0～3.0KPa;
Described tower reactor type of heating is electrically heated or steam indirect heating, and tower reactor temperature is 50 ℃～60 ℃, total reflux 30 minutes;
Described first employing in large reflux ratio collection eucalyptus oil system be take α-pinene as main light constituent, reflux ratio is 20～30, when in tower bottoms, α-pinene content is less than 5%, light constituent has been collected, then the tower reactor that raises temperature to 65 ℃～80 ℃, reducing reflux ratio is 10～15, collect 1, 8-eucalyptol, and in collection liquid 1, 8-eucalyptol content is not less than 90.00%, every 15 minutes sampling analysis, gather after 60～90 minutes, treat 1 in sample, 8-eucalyptol content is lower than 90.00% time, improving reflux ratio is 15～20, collect 1, 8-eucalyptol, and in collection liquid 1, 8-eucalyptol content is not less than 90.00%, until in the product of collecting 1, 8-eucalyptol content cannot reach 90.00% to be stopped when above gathering, finally merge 1 of collection, 8-eucalyptol liquid.
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| CN102850370B (en) * | 2012-07-13 | 2016-05-25 | 北京工商大学 | A kind of method that reclaims 1,8-cineole from eucalyptus oil substandard goods |
| CN103408080B (en) * | 2013-08-28 | 2015-04-15 | 福建森美达生物科技有限公司 | Method for removing peculiar smell of cooling water and recycling cooling water in eucalyptus oil production process |
| CN106554360A (en) * | 2016-11-21 | 2017-04-05 | 四川省林业科学研究院 | A kind of method of 1,8 Cineoles in purification yusho oil |
| CN106800496A (en) * | 2016-12-07 | 2017-06-06 | 广西灏源盛世生物科技有限公司 | It is a kind of to be continuously separated 1,8 cineoles and the dilute method of α pinanes in eucalyptus oil |
| CN108251213A (en) * | 2016-12-29 | 2018-07-06 | 广州华芳烟用香精有限公司 | A kind of natural perfume material distillation and its preparation method and application |
| CN108864126B (en) * | 2018-06-05 | 2021-06-04 | 云南国润香料制造有限公司 | Method for continuously and hierarchically rectifying eucalyptus oil |
| CN108654129B (en) * | 2018-06-05 | 2021-01-05 | 云南国润香料制造有限公司 | Eucalyptus oil rectification device for collecting rectification liquid in sections and processing method |
| CN108586199B (en) * | 2018-06-05 | 2021-11-19 | 云南国润香料制造有限公司 | Method for extracting and separating terpineol from eucalyptus volatile oil |
| CN109293671A (en) * | 2018-09-04 | 2019-02-01 | 中粮德信行健康产业有限公司 | A kind of purification process of Cineole |
| CN109234014A (en) * | 2018-09-05 | 2019-01-18 | 中粮德信行健康产业有限公司 | A kind of folium eucalypti oil producing method |
| CN109554229A (en) * | 2018-11-19 | 2019-04-02 | 江西省林业科学院 | A kind of method of extraction of essential oil and device of high-content linalool |
| CN109320526B (en) * | 2018-12-21 | 2021-06-22 | 广州市博林机械设备有限公司 | Method for separating 1, 8-cineole from eucalyptus globulus leaf oil |
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| CN101899361A (en) * | 2010-08-04 | 2010-12-01 | 厦门百度科技开发有限公司 | Single-tower continuous rectification method of eucalyptus oil |
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