CN1964637A - Preparation of tobacco extract - Google Patents
Preparation of tobacco extract Download PDFInfo
- Publication number
- CN1964637A CN1964637A CNA2005800181966A CN200580018196A CN1964637A CN 1964637 A CN1964637 A CN 1964637A CN A2005800181966 A CNA2005800181966 A CN A2005800181966A CN 200580018196 A CN200580018196 A CN 200580018196A CN 1964637 A CN1964637 A CN 1964637A
- Authority
- CN
- China
- Prior art keywords
- wood tar
- extract
- solvent
- tar
- reaction vessel
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Extraction Or Liquid Replacement (AREA)
Abstract
A method for preparation of smoke extract from wood tar for flavouring and colouring of food products is disclosed. The smoke extract is with the present method produced by means of supercritical extraction of fractions of the wood tar. The extractions solvent, such as carbon dioxide, has very good properties of entraining and resolving the required fractions of the wood tar, and it is relatively simple to separate the resolved components in the retrieving process, as the different components have different solubility at different supercritical and subcritical conditions. Thus, a smoke extract containing less than 10 ppb (parts per billion) of benzo (a) pyrene and less than 20 ppb of benzo (a) athracene may be obtained. In one embodiment, the wood tar is subject to a separation process prior to the supercritical extraction to remove a substantial part of the unwanted components.
Description
Technical field
The present invention relates to be used for the preparation of foodstuff flavouring and painted tobacco extract.
Background technology
Food carried out sootiness is used to preserve and the seasoning of food is very ancient and well-known practice, wherein make food stand to come from the cigarette of combustion of wood, in this process since lack enough oxygen or since combustion process in temperature, the gas that discharges in the timber is unburnt.Therefore, this tobacco bale contains the material that required feature is provided for food in a large number.
For numerous food product, preferably do not make the traditional sootiness process of product experience and obtain the sootiness seasoning, and for this purpose, developed polytype tobacco extract.
US 3,106, disclose a kind of method for preparing the liquid smoke extract in 473, and the water-soluble portion that water and timber cigarette adverse current is passed extract cigarette is with as timber cigarette seasoning water solution.In same document, the water-soluble fraction of product of the wood distillation product also being discussed or having been come from the partially combusted condensation cigarette of timber is as the application of liquid smoke extract.
For completing combustion, do not having oxygen to exist or existing when heating under the situation of amount of oxygen deficiency, for example, distillation or pyrolysis, timber produces the gas that contains water, water-soluble component and water-msoluble ingredients, and wherein said water-msoluble ingredients is exactly a wood tar.Residue in the process is ash and charcoal, and it mainly contains carbon and some heavy tar components.Yet the product that is called as wood tar that the condensation by cigarette obtains can also comprise some water-soluble components except insoluble component.
Water-soluble component constitutes the only sub-fraction of thermal decomposition of wood process product, and has attempted extracting from other product of pyrolytic process the appropriate liquid smoke product that is used to prepare food.
Among the WO 02/00040, timber is carried out pyrolytic process, utilize the extraction solvent of supercriticality to make the charcoal experience leaching process that is produced.Supercritical solvent has the characteristic that well penetrates in charcoal and the extraction component thereof, and described charcoal and extraction component thereof regain by the pressure that reduces supercritical solvent.
Charcoal constitutes the largest portion of thermal decomposition of wood process product, but because it comprises a large amount of carcinogenic compounds, especially polynuclear aromatic hydrocarbons (PAH) is such as benzo (a) pyrene and benzo (a) anthracene (benzo (a) athracenc), therefore is commonly referred to be not to be suitable for food.
Attempted obtaining from tar the appropriate liquid cigarette, US 5,681, disclose in 603 a kind ofly, wherein wood tar are dissolved in the alkaline aqueous solution that contacts with nonionic, aryl resin, to remove multi-nucleus aromatic compound.Yet this method need be handled or regenerating resin, is the process of a complexity therefore, also needs the careful quality of controlling and supervising the liquid smoke that is produced, because the content of known timber and the wood tar that is produced has very big changing naturally.
US 4,154, disclose another kind of method in 866, wherein with wood tar and mixed with propylene glycol, are heated to about 140 ℃, and distill by about 100mmHg that reduces pressure, and make the evaporation of propane diols and part wood tar thus.After the devaporation, need utilize powdered activated carbon that coagulation is handled, obtaining the mixture of propane diols and wood, described mixture contains " can not detection limit 3,4-BaP ".
Summary of the invention
The object of the present invention is to provide a kind of production method that is used for foodstuff flavouring and painted tobacco extract, described tobacco extract does not have above-mentioned shortcoming, and described method can be used for the tobacco extract of safe, the low PAH level of manufacture amount.
Because the PAH of high-load and can cause bitter taste or the component of burning taste, wood tar is considered to not to be suitable for food usually, but the inventor finds, in fact the supercritical extraction method similar to disclosed method among the WO 02/00040 can be used on the wood tar rather than be used on the charcoal, and produce high-quality tobacco extract, the PAH of described tobacco extract is low and can produce in a large number and chemicals is not incorporated in the process, and this can cause that tobacco extract handles the consumer's of food new safety concerns.
This purpose realizes by the method according to this invention, wherein produces tobacco extract by the means of supercritical extraction wood.Extract ratio of solvent such as carbon dioxide, have good conveying and dissolve the characteristic of required wood, and it is simple relatively separating the component of being dissolved in removal process, because different component has different dissolubilities under different overcritical and subcritical states.Therefore, can obtain containing benzo (a) pyrene that is less than 10ppb (part per billion) and the tobacco extract that is less than benzo (a) anthracene of 20ppb.
In particularly preferred embodiments, before means of supercritical extraction, make the separation process of wood tar experience to remove the undesirable component of the overwhelming majority, the viscosity that is used for the wood tar of super critical extraction process thus can reduce greatly and wood tar will be more sticking, and this provides the easier conductibility in the super critical extraction process.And super critical extraction process can be carried out under the situation of recovery fraction quality being carried out supervision still less, and the content of the described quality that reclaims fraction and PAH and possible other undesirable ratio of component such as heavy metal is relevant.
The specific embodiment
According to the present invention and these and other advantage of the method for preferred embodiment will become more obvious by following description of the present invention.
Therefore, the present invention relates to the method that a kind of preparation is used for the tobacco extract of foodstuff flavouring, comprise the leaching process that relates to following steps:
Be basically supercriticality extraction solvent extraction wood tar one or more fractions and
In one or more fractions of the wood tar that recovery is extracted at least some obtain tobacco extract thus.
The term wood tar is interpreted as and obtains from timber and mainly comprise the tar of water-fast component basically, but also can have the water-soluble component of fraction.
Extract the mixture that solvent is preferably selected from carbon dioxide, methane, ethane, propane, ethene, propylene, ammonia, methyl alcohol, water and these solvents one or more.Yet, can use other within the scope of the invention and extract solvent, preferably, can adopt critical-temperature and pressure to be respectively 1-400 ℃ of those solvents that cling to 20-500 as extracting solvent.
The timber that obtains tar can be preferably selected from Oak Tree, dragon spruce, pine tree, beech tree, cherry tree, mahogany, ash, maple, alder, elm, birch, hickory and white poplar.In principle, the timber of all kinds all can be suitable for according to the present invention, and the selection between the different timber only is a problem of handling the taste of prepared tobacco extract.The instantiation that can preferably obtain the timber of wood tar is maple (Acer negundo L.), white birch (Betula pendula Roth-comprises subspecies B.alba L. and B.verrucosa Ehrh), European birch (Betula pubescensEhrh), hornbeam (Carpinus betulus L.), hickory (Carya ovata (Mill.) Koch (C.alba (L.) .Nutt.)), chestnut (Castanea sativa Mill.), eucalyptus (Eucalyptus sp.), beech tree (Fagus grandifolia Ehrh. and Fagus sylvatica L.), common ash (Fraxinus excelsior L), walnut tree (Junglans regia L.), apple (Malus pumilaMill.), mesquite (Prosopis juliflora DC.), cherry tree (Prunus avium L.), roble (Quercus alba L.), live-oak (Querqus ilex L.), common yellow jacket tree (Quercusrobur L.), root-bark of Glossy Buckthorn (Rhamnus frangula L.), locust tree (Robinia pseudoacacia), red elm (sweet elm) (Ulmus fulva Michx) and elm (Ulmus rubra M ü hlenb.).
In a preferred embodiment of the invention, the leaching process circulation comprises step
A) the part wood tar is fed in the reaction vessel,
B) with the extracting section solvent supply in reaction vessel,
C) make extraction solvent under the supercriticality acting on wood tar given time of contact, extracting one or more fractions of wood tar,
D) will extract solvent and the wood tar component extracted and from reaction vessel, guide in second Room, and the not extraction unit branch of wood tar is retained in the reaction vessel and
E) reduce at least a of tar fraction that the pressure in second Room extracted to condense from extract solvent, reclaim the component that forms described tobacco extract thus.
Can control temperature and/or pressure in the reaction vessel in the described process, in given time of contact, keep postcritical basically state, thereby extract one or more fractions of wood tar so that extract solvent.
Above-mentioned leaching process can carry out with batch process, wherein extracts solvent to keep postcritical basically state given time of contact in reaction vessel, to extract one or more fractions of wood tar.Reaction vessel should be suitable for keeping the high pressure of means of supercritical extraction solvent, such as 250 crust.
In batch process, to extract solvent is provided in the reaction vessel, increase to supercritical pressure up to container inner pressure, make the solvent and the wood tar reaction of supercriticality, continue predetermined time of contact, remove from reaction vessel then, the pressure in the reaction vessel is brought down below the overcritical level of this solvent usually.The step b) of extraction circulation-e) can repeat the multiple fraction that one or many extracts wood tar, all be extracted out up to all fractions that can be used for predetermined purpose basically, and extract solvent and can when the tar fraction that will be extracted therefrom removes, recycle.
For the temperature at inner control reaction vessel content time of contact, reaction vessel can be equipped with cooling and/or heater.
Join wood tar part in the reaction vessel should preferably account for the reaction vessel interior volume preferred 40% or still less, more preferably 30% or still less, most preferably 20% or still less, with the contact area that guarantees to be enough to effectively extract between wood tar and the solvent.
Scheme as an alternative, extraction can be carried out with continuous process.Particularly, this continuous leaching process circulation comprises step
A) the part wood tar is fed in the reaction vessel,
B) Continuous Flow that the extraction solvent under the supercriticality basically is provided is by reaction vessel, promoting to extract the contact between solvent and the wood tar, thereby extracts one or more fractions of wood tar,
C) the extraction solvent streams that will comprise the wood of being extracted is guided in second Room from reaction vessel continuously, and the not extraction unit branch of wood tar is retained in the reaction vessel,
D) reduce at least a of tar fraction that the pressure in second Room extracted to condense from extract solvent, reclaim thus the component that forms described tobacco extract and
E) make and extract solvent streams by reaction vessel and keep time enough, to extract the fraction surveyed of wood tar.
Wood tar can be fed in the reaction vessel in batches, so that a certain amount of wood tar is arranged in reaction vessel, and keep the extraction solvent Continuous Flow of supercriticality, be extracted out up to all or all basically tar fractions that can be used for this purpose, remaining afterwards wood tar is by new a certain amount of substituting, perhaps the wood tar in the reaction vessel can supply in the container, and the remainder of tar also can be removed continuously.
In a preferred embodiment of the invention, the wood of being extracted reclaims by the pressure that progressively reduces in described second Room, described second Room can be made up of a plurality of chambers that form cascade in this case, extracting solvent at this is fed to from reaction vessel in the chamber, and therefrom be fed to chamber subsequently or the like, wherein each chamber pressure is subsequently reduced.In each step that pressure reduces the condense wood tar that a part extracted, for example 2,3 or 4 steps.
In the wood tar that is extracted some reduce in the step at each pressure condenses, and reduces the wood tar that condenses in the step at each pressure and can collect respectively, is extracted one or more fractions of wood tar to obtain.Use the various combination of gained fraction that the aromatic substance with different smokes road, local flavor and color can be provided thereafter.Concrete trend is can reduce undesirable carcinogenic compound by this way, especially PAH that condenses in specific pressure step and the content thereof in the tobacco extract of gained.
The step that reclaims the component that forms tobacco extract from extract solvent is that the technical staff is known, has for example provided suitable example among the WO 02/00040.
With extract before solvent contacts, make wood tar reach the approaching temperature of temperature with used extraction solvent, preferably in 30 ℃ of described temperature, most preferably in 20 ℃ of described temperature, make the temperature of extracting solvent when contacting, can not be reduced to below the supercritical phase with wood tar.
Wood tar is diluted in solvent or suspending agent or suspending.Make wood tar as follows with the various objectives that solvent or suspending agent mix: protection equipment, extract the high molecular weight component of major part in the wood tar and when using countercurrent extraction method, adjust the shipping time.Randomly, can also add inorganic acid or alkaline constituents.On the one hand, the purpose of dilution or suspension wood tar is that protection equipment is in order to avoid adherence of wood tar.Otherwise the low water content in the wood tar can cause tar to adhere and stick on the equipment.For fear of this problem, preferably dilution or suspension wood tar are 10-95wt%, preferably 20-80wt%, more preferably 40-80wt%, 50-75wt% most preferably to the average tree tar-concentration.Second aspect, the dilution or the purpose of suspension wood tar are when extracting in the adverse current method, adjust the shipping time of wood tar.Shorten the shipping time by adding relatively large solvent or suspending agent.
Generally speaking, solvent or suspending agent should be nontoxic to the mankind, because some solvents or suspending agent can pass through to extract solvent extraction, and therefore will be present in the final products.The solvent or the suspending agent that are suitable for above-mentioned two purposes can be preferably selected from vegetable oil, animal oil, ethanol, water or its mixture.
The third aspect, solvent or suspending agent are to extract the reinforcing agent of fraction from wood tar.In this article, reinforcing agent is defined as a kind of component, and it improves supercritical solvent extracts high molecular weight component from wood tar ability.Reinforcing agent according to the present invention is preferably selected from methyl alcohol, ethanol, water or its mixture.Reinforcing agent or before leaching process, add, or inject respectively the reaction vessel that extracts takes place.The consumption of reinforcing agent is preferably the 0.1%v/v at least of wood tar, more preferably 1%v/v at least.Generally speaking, there is not the upper limit, because when the amount of the reinforcing agent that adds is above above about 5%v/v of wood tar, effect will no longer increase.
In addition or as an alternative scheme before or after wood tar is fed to reaction vessel, can make wood tar and carrier mix before leaching process.The use of carrier can be shortened time of contact required in the extraction.Carrier preferably is insoluble to the extraction solvent of supercriticality basically.Carrier is preferably selected from diatomite, C salt (celite), bentonite, perlite or its mixture.Yet in principle, the carrier of any kind can use.The volume ratio of wood tar and carrier is advantageously 1: 0.1-1: in 10 scopes, and preferred 1: 0.5-1: 2.
In preferred embodiments, extract amount that solvent comprises carbon dioxide and be 85wt% at least, preferred 90wt% at least, more preferably 95wt% at least.The remainder that extracts solvent can be a water, and perhaps carbon dioxide can constitute basically to extract about 100% of weight of solvent.
In leaching process, the temperature of extracting solvent preferably maintains in the 20-100 ℃ of scope, and preferred 30-70 ℃, more preferably 40-60 ℃.In particularly preferred embodiments, in leaching process, the temperature of extracting solvent maintains about 50 ℃ basically.Pressure in the reaction vessel maintains in the 75-500 crust scope, preferred 100-250 crust, and more preferably 120-180 clings to, for example about 150 crust.
The composition that has been found that the tobacco extract that is extracted depends primarily on the pressure in the leaching process, and therefore, the taste of the product that extracts and quality can be adjusted by the pressure condition that changes leaching process.
In preferred embodiments, the tobacco extract when leaching process finishes comprises to join wood tar weight 1-60wt% in the reaction vessel, preferred 5-40wt%, the more preferably fraction of the wood tar that extracted of 5-20wt%.The reason that stops leaching process in this level is to avoid having in the tobacco extract the carcinogenic of excessive concentrations and/or bitter taste component.
According to the present invention, should preferably avoid extracting more than the 60wt% in the wood tar from join this process.Desirable extraction level depends on undesirable carcinogenic and/or bitter taste component concentrations in the tobacco extract that forms in this process.Usually, surpass the extraction level and can cause too much extracting that undesirable component concentrations exceeds more than the acceptable level in the product.
Wood tar and the preferable range of extracting between solvent time of contact are 5-120min, preferred 15-90min, most preferably 20-60min.Be to obtain the important factor in order that high-quality is extracted product time of contact.By keeping reducing bitter taste and/or carcinogenic components best time of contact, therefore improved the taste and the health of the wood of being extracted.
In preferred embodiments, extract its as food with before one or more fractions of tobacco extract, prepare wood tar by the separation process that undressed wood tar product is carried out.
Undressed wood tar product is carried out, can carry out with the known many steps in this area itself in order to the separation process of the wood tar that obtains to carry out super critical extraction process, main purpose is to produce more low viscous wood tar, also have undesirable component, the especially PAH of lower content and possible heavy metal if possible.This separation process of one or more fractions of undressed wood tar can utilize liquid flux to carry out, and utilizes this liquid flux, extracts the fraction of undressed tar and recovery once more, obtains being used for the wood tar of further leaching process thus.Solvent can be the mixture of oil or nonpolar basically solvent or these materials.Solvent can for example comprise alcohols, aldehydes or the ketone with at least two carbon atoms, alkanes, alkene class or alkynes class with at least five carbon atoms, ethers, ester class or the like, but preferred its is selected from ether, ethanol, propyl alcohol, butanols, diethyl ether, hexane, methyl acetate and any mixture thereof.
Scheme or in addition as an alternative, the separation process that undressed wood tar product being used to of carrying out prepared wood tar can comprise by machinery and separates for example centrifugal one or more fractions of separating undressed wood tar, to obtain being used for the wood tar of further leaching process.
The separation process that undressed wood tar product being used for of carrying out is prepared wood tar can also be formed or be may further comprise the steps by following steps: distill undressed wood tar to obtain being used for the wood tar of further leaching process from distillate.Distillation particularly can be carried out in the device that comprises a plurality of positions of condensing with different thickening temperatures and/or pressure, wherein the distillate fraction is collected in each position of condensing, and the wood tar that is used for further leaching process comprises one or more of described fraction.
As another replacement scheme, also can use together with any one aforesaid process, the separation process that undressed wood tar product being used to of carrying out is prepared wood tar can comprise one or more fractions of separating undressed wood tar by electrophoresis, to obtain being used for the wood tar of further leaching process.
The embodiment of embodiment of the present invention
The following example that is used for the tobacco extract of food by means of supercritical extraction production can be based on undressed wood tar, perhaps based on the wood tar that from the separation process that undressed wood tar product is carried out, obtains, such as the wood tar that from undressed wood tar product, separates by the liquid extraction of using diethyl ether, assign to obtain wood tar by reclaiming the level of being extracted subsequently, this wood tar has the viscosity lower than undressed wood tar product.
Batch process according to the present invention is undertaken by following steps: the part wood tar is mixed with the diatomite of similar volume, and this mixture is placed in the suitable reaction vessel, wherein mixture occupies about 40% of internal tank volume.Container is heated to 50 ℃, and keeps this temperature and reach 15min, reach roughly the same temperature to guarantee mixture wherein.Then, by high-pressure pump carbon dioxide is fed in the container from memory.Supply along with carbon dioxide, pressure in the container increases, and beginning at filling step, the temperature of container is regulated by heater and is maintained at about 50 ℃, but in the decline of filling step, the compression of carbon dioxide causes temperature to increase, the temperature when container is equipped with cooling device to be used to regulate the filling step end, pressure in container reaches 150 crust, finishes during about 50 ℃ of temperature.Under these conditions, adopt the time of contact of 30min, the extraction unit of carbon dioxide and wood tar is divided in inflow second Room, described second Room is made up of 3 containers that are connected in series.Described stream at first directly arrives first of these containers, and wherein pressure drops to about 100 crust, and makes temperature drop to about 40 ℃.Condense this first time that causes extracting part, and collect from container.Then carbon dioxide and wood tar are extracted the second and the 3rd container that remainder is partly guided to second Room, wherein pressure drops to 80 crust and 55 crust respectively, but temperature is maintained at about 40 ℃ by heater, collects the second and the 3rd coagulation from corresponding container.Carbon dioxide is recycled in the memory then.For the wood tar of giving certain portions, extract circulation and repeats altogether 3 times, from reaction vessel, remove together with diatomite then and with new wood tar and the replacement of diatomite mixture, and can whole process repeated.Before discharging, can detect the PAH content of the fraction of in the first and the 3rd container of second Room, condensing in order to be used as tobacco extract, but the coagulation most probable in second container has the very PAH of low content.
In continuous leaching process, it is reaction vessel that wood tar and diatomaceous mixture are placed the cylindrical reactor of elongation, and in the whole leaching process, this reaction vessel is kept the pressure that are lower than 150 crust.A terminal inlet supplying carbon dioxide at reactor, flow through reactor, make time of contact with wood tar and diatomaceous mixture at 20-40min, and flow out, flow to second Room of mentioning in the above-mentioned batch process that comprises the container cascade thus by another end outlet of reactor.In leaching process, can supply in batches and remove carbon dioxide, the state that extracts solvent in the container remains on supercriticality continuously, and the steady flow of carbon dioxide perhaps can be provided.
In another continuous leaching process, wood tar and diatomaceous mixture dilute in order to the ethanol of wood tar stereometer 4%, and this mixture joined in the cylindrical reactor by high-pressure pump, reverse flow or cross-current with the Continuous Flow of carbon dioxide flow through reactor, after supercritical carbon dioxide stream contacts about 90min, the remainder of mixture is removed from cylindrical reactor.The wood of being extracted reclaims as mentioned above.
Claims (30)
1. method for preparing the tobacco extract that is used for foodstuff flavouring comprises the leaching process that relates to following steps:
Be basically supercriticality extraction solvent extraction wood tar one or more fractions and
In one or more fractions of the wood tar that recovery is extracted at least some obtain tobacco extract thus.
2. according to the process of claim 1 wherein that extracting solvent is selected from carbon dioxide, methane, ethane, propane, ethene, propylene, ammonia, methyl alcohol, water and these solvents one or more mixture.
3. according to the method for claim 1 or 2, the timber that wherein obtains tar is selected from Oak Tree, dragon spruce, pine tree, beech tree, cherry tree, mahogany, ash, maple, alder, elm, birch, hickory and white poplar.
4. according to each method of claim 1-3, wherein the leaching process circulation comprises step
A) the part wood tar is fed in the reaction vessel,
B) with the extracting section solvent supply in reaction vessel,
C) make extraction solvent under the supercriticality acting on wood tar given time of contact, extracting one or more fractions of wood tar,
D) will extract solvent and the wood tar component extracted and from reaction vessel, guide in second Room, and the not extraction unit branch of wood tar is retained in the reaction vessel and
E) reduce at least a of tar fraction that the pressure in second Room extracted to condense from extract solvent, reclaim the component that forms described tobacco extract thus.
5. according to the method for claim 4, wherein extract with batch process and carry out, and extract solvent in reaction vessel, to keep postcritical basically state given time of contact, to extract one or more fractions of wood tar.
6. according to the method for claim 5, wherein extract step b) in the circulation to e) repeat at least once to extract the multiple fraction of wood tar.
7. according to the method for claim 6, wherein each extraction solvent that extracts after circulating reuses in leaching process.
8. according to each method of claim 4-7, wherein be fed to part wood tar in the reaction vessel occupy the reaction vessel interior volume preferred 40% or still less, more preferably 30% or still less, most preferably 20% or still less.
9. according to each method of claim 1-4, wherein extract with continuous process and carry out.
10. according to the method for claim 9, wherein continuous leaching process circulation comprises step
A) the part wood tar is fed in the reaction vessel,
B) Continuous Flow that the extraction solvent under the supercriticality basically is provided is by reaction vessel, promoting to extract the contact between solvent and the wood tar, thereby extracts one or more fractions of wood tar,
C) the extraction solvent streams that will comprise the wood of being extracted is guided in second Room from reaction vessel continuously, and the not extraction unit branch of wood tar is retained in the reaction vessel,
D) reduce at least a of tar fraction that the pressure in second Room extracted to condense from extract solvent, reclaim thus the component that forms described tobacco extract and
E) make and extract solvent streams by reaction vessel and keep time enough, to extract the fraction surveyed of wood tar.
11. according to each method of claim 4-10, wherein the wood of being extracted reclaims by the pressure that progressively reduces in described second Room, wherein at each step that pressure reduces wood tar that part extracts that condenses.
12. according to each method of claim 4-11, wherein with extract before solvent contacts, make wood tar reach the approaching temperature of temperature with used extraction solvent, preferably in 30 ℃ of described temperature, most preferably in 20 ℃ of described temperature.
13., wherein wood tar is being diluted in solvent or suspending agent or is suspending according to each method of aforementioned claim.
14., wood tar and carrier are mixed according to each method of aforementioned claim.
15. according to the method for claim 14, wherein carrier is insoluble to the extraction solvent under the supercriticality basically.
16. according to the method for claim 14 or 15, wherein carrier is selected from diatomite, C salt, bentonite, perlite or its mixture.
17. according to each method of claim 14-16, wherein the volume ratio scope of wood tar and carrier is 1: 0.1-1: 10, preferred 1: 0.5-1: 2.
18., wherein extract solvent and comprise at least 85wt%, preferred 90wt% at least, the more preferably carbon dioxide of 95wt% at least according to each method of aforementioned claim.
19. according to each method of aforementioned claim, wherein in leaching process, the temperature maintenance of extracting solvent 20-100 ℃, preferred 30-70 ℃, more preferably in 40-60 ℃ the scope.
20. according to each method of claim 4-19, wherein the pressure in the reaction vessel maintain 75-500 crust, preferred 100-250 crust, more preferably in the scope of 120-180 crust.
21. according to each method of aforementioned claim, wherein the tobacco extract when leaching process finishes comprises to join the wood tar weight 1-60wt% in the reaction vessel, preferred 5-40wt%, the more preferably fraction of the wood tar that extracted of 5-20wt%.
22. according to each method of aforementioned claim, wherein wood tar and time of contact of extracting solvent are 5-120min, preferred 15-90min, most preferably 20-60min.
23. according to each method of aforementioned claim, wherein said wood tar prepares by the separation process that undressed wood tar product is carried out.
24. according to the method for claim 23, wherein the separation process that undressed wood tar product being used to of carrying out prepared wood tar comprises
Utilize liquid flux extract undressed wood tar one or more fractions and
Reclaim the extraction fraction of undressed wood tar, obtain being used for the wood tar of further leaching process thus.
25. according to the method for claim 24, wherein liquid flux is nonpolar basically solvent.
26. according to the method for claim 23, wherein liquid flux is selected from ether, ethanol, propyl alcohol, butanols, diethyl ether, hexane, methyl acetate and any mixture thereof.
27. according to each method of claim 23-26, wherein the separation process that undressed wood tar product being used to of carrying out prepared wood tar comprises
One or more fractions of separating undressed wood tar by machinery are to obtain being used for the wood tar of further leaching process.
28. according to each method of claim 23-27, wherein the separation process that undressed wood tar product being used to of carrying out prepared wood tar comprises
Distill undressed wood tar from distillate, to obtain being used for the wood tar of further leaching process.
29. method according to claim 28, wherein distillation is included in a plurality of congealing steps under different adiabatic condensation temperatures and/or the pressure, wherein collect the distillate fraction at each congealing step, the wood tar that is used for further leaching process comprises one or more of described fraction.
30. according to each method of claim 23-29, wherein the separation process that undressed wood tar product being used to of carrying out prepared wood tar comprises
One or more fractions of separating undressed wood tar by electrophoresis are to obtain being used for the wood tar of further leaching process.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DKPA200400877 | 2004-06-04 | ||
| DKPA200400875 | 2004-06-04 | ||
| DKPA200400875 | 2004-06-04 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1964637A true CN1964637A (en) | 2007-05-16 |
Family
ID=38083430
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2005800181966A Pending CN1964637A (en) | 2004-06-04 | 2005-06-01 | Preparation of tobacco extract |
Country Status (2)
| Country | Link |
|---|---|
| CN (1) | CN1964637A (en) |
| ES (1) | ES2352844T3 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104059778A (en) * | 2014-06-10 | 2014-09-24 | 苏州泽达兴邦医药科技有限公司 | Method for extracting endogenous aromatic substances with water under subcritical conditions |
-
2005
- 2005-06-01 ES ES05746272T patent/ES2352844T3/en active Active
- 2005-06-01 CN CNA2005800181966A patent/CN1964637A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104059778A (en) * | 2014-06-10 | 2014-09-24 | 苏州泽达兴邦医药科技有限公司 | Method for extracting endogenous aromatic substances with water under subcritical conditions |
| CN104059778B (en) * | 2014-06-10 | 2016-07-20 | 苏州泽达兴邦医药科技有限公司 | A kind of method of Subcritical water chromotagraphy endogenous flavor matter |
Also Published As
| Publication number | Publication date |
|---|---|
| ES2352844T3 (en) | 2011-02-23 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| EP1753308B1 (en) | Preparation of smoke extract | |
| CN101999618B (en) | Method for preparing liquid smoking spice for meat from pecan shells | |
| DE60122524T2 (en) | METHOD FOR THE PRODUCTION OF LIQUID SMOKE | |
| AU2001273892A1 (en) | A method of preparing liquid smoke | |
| CN1964637A (en) | Preparation of tobacco extract | |
| Varlet et al. | Smoke flavoring technology in seafood | |
| CN104872605B (en) | The method and liquid fumet of preparation solution fumet | |
| US20080138496A1 (en) | Preparation of Smoke Extract | |
| EP0859556A1 (en) | Smoke coloring and flavoring compositions derived from wood pyrolysis tar | |
| US4666498A (en) | Process and apparatus for obtaining raw materials from autumn foliage | |
| CN107129822A (en) | A kind of preparation method of refined bamboo vinegar | |
| CA3182534A1 (en) | Method of extraction | |
| Jones et al. | Adding value by culinary smoking | |
| RU2223654C1 (en) | Method of preparing smoking fluid | |
| EP0227263B1 (en) | Process for the recovery of volatile coffee constituents | |
| RU2090072C1 (en) | Method of smoking liquid producing | |
| EP0227262A1 (en) | Coffee production | |
| CN106165907A (en) | A kind of cigarette filter rod containing Thuja extract | |
| US1144171A (en) | Method of treating resinous woods to remove the soluble constituents therefrom. | |
| RU2250219C2 (en) | Method for production of pectin material | |
| RU2248372C2 (en) | Pectin preparation production method | |
| Saporito | Extraction of Coffee Aroma | |
| CN114989888A (en) | Ginger oil flavor improving method | |
| SU1337394A1 (en) | Method of processing pyroligneous distillate | |
| CA1226819A (en) | Process and apparatus for obtaining raw materials from autumn foliage |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Open date: 20070516 |