CN1181169C - Method for preparing pure tobacco oil - Google Patents
Method for preparing pure tobacco oil Download PDFInfo
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- CN1181169C CN1181169C CNB021337586A CN02133758A CN1181169C CN 1181169 C CN1181169 C CN 1181169C CN B021337586 A CNB021337586 A CN B021337586A CN 02133758 A CN02133758 A CN 02133758A CN 1181169 C CN1181169 C CN 1181169C
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Abstract
The present invention discloses a method for preparing pure tobacco oil. The oil yield is improved markedly by making use of the method, perfume components are expanded effectively, and the perfuming effect of cigarettes is improved. The present invention has the method that tobacco extract and magnetic chemical filler are mixed evenly to be put in an extraction tank, and lipid matter in the tobacco extract extracted by supercritical fluid is led in the extraction tank; one kind of ethanol, acetone and water is selected as entrainer led to a mixing tank to be mixed evenly with extraction fluid, the mixture is preheated by a preheating tank to enter the extraction tank, the tobacco extract which is degreased is extracted circularly, and the obtain article is separated by a separator to obtain the pure tobacco oil.
Description
Technical field
The invention relates to the preparation method of tobacco cleaned oil, more particularly, the invention relates to the method for utilizing supercritical liquid extraction technique from tobacco extract, to extract tobacco cleaned oil.
Background technology
The reinforced Technology that must demonstrate its importance in the contemporary production of cigarettes indispensable and further that become of tobacco flavoring, in production of cigarettes, enrich perfume (or spice) material and sweetener in the goods by flavoring and casing, improving smoke perfume, improve the pipe tobacco physical form and to inhale flavor, thereby make the sucking quality of cigarette product more become perfect, perfect.Current, along with carrying out of anti-smoking campaign, the development low-coke tar cigarette has become the direction of tobacco industry survival and development.Inhale flavor in order to compensate flue gas, will extremely use up institute's energy of Technology with the formulating of recipe of leaf, also must remedy the loss of fragrance, recover and the aromatic degree of raising cigarette by means of the flavoring and casing means except pipe tobacco.Therefore, the modulation of essence spice for cigarette seems more important with selecting the status in current low-coke tar cigarette research, exploitation and manufacturing for use, and it is imperative to develop new high-quality essence spice for cigarette.
Tobacco extract is from the tobacco plant, for example: the class of extracting in flue-cured tobacco, burley tobaccos or the Turkish tobaccos with tobacco characteristic perfume causes aroma compounds, is considered to the optimal additive of tobacco product.At present, tobacco extract mostly adopts traditional steam distillation, have method such as agent solvent extraction to extract, but these methods are to the poor selectivity of material, impurity such as many resins, pigment and wax in the raw material can be extracted simultaneously, and might make the sex change of many thermo-sensitivity fragrance matters because of processing temperature is too high, thus influenced product quality, not only outward appearance and solubility property are not good, and odour characteristics is not outstanding, and the perfuming cigarette effect is undesirable.In addition, the quality of tobacco extract and raw materials used quality have much relations, for saving cost, often adopt junior tobacco leaf or offal the like waste, because of itself containing less fragrance matter and more impurity in these raw materials, so the quality of the tobacco extract that obtains is just poor.
In recent years, supercritical liquid extraction technique develops rapidly as a kind of new separation technology, and the extraction temperature of this technology is low, and is nontoxic, and solvent-free pollution is called as green isolation technique.Compare with traditional separation method, it can effectively overcome the problems such as thermolysis, dissolvent residual or part material volatilization destruction that adopt the traditional extraction method to occur in leaching process, thereby extract the crucial chemical ingredients in the natural matter selectively, avoid introducing or reducing impurity, improve the quality of products, improve product appearance, can obtain to keep high-quality, the high value-added product of natural color.Aspect tobacco extract, existing using super critical fluid technology extracts some relevant reports of tobacco effective constituent both at home and abroad, for example: domestic disclosed patent CN1127778A, CN1302568A and U.S. Pat 4,506,682 all is to adopt supercritical fluid extraction directly to extract tobacco cleaned oil from tobacco.
But up to now, prior art mainly is to adopt supercutical fluid directly tobacco material to be extracted, because the volume of tobacco is big, tap density is little, so the treatment capacity when extracting is very little at every turn, yield is corresponding lower, and facility investment is bigger.In addition, owing to adopt pure supercutical fluid, do not relate to and carry agent, make that the object range of supercritical fluid extraction is less, mainly be confined to high volatile volatile, low polar compound, but can not extract the aromatoising substance of many low volatilities that perfuming cigarette is played a crucial role of also containing in the tobacco.This is a technical barrier extremely to be solved.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art part, a kind of improved method for preparing tobacco cleaned oil is provided.Utilize present method can improve oil yield significantly, and effectively enlarge flavour ingredient, improve the perfuming cigarette effect.
The preparation method of technical scheme---tobacco cleaned oil provided by the invention comprises the step of following order:
(1) pre-treatment of raw material, at first to raw material dust removal, dryings such as inferior grade tobacco leaf, waste tobacco powder, offals, pulverized 5 mesh sieves, use 50%-95% ethanol then, heat lixiviate 2-4 time down at 50 ℃～100 ℃, each 3-6 hour, extracting solution merged sedimentation, extracted supernatant liquid, obtain the thick extracted extract of tobacco through concentrating under reduced pressure, the relative density of this medicinal extract in the time of 20 ℃ is 1.200～1.480.
The thick extracted extract of above-mentioned tobacco can prepare voluntarily, also can directly buy the commercially available prod.
(2) degreasing of tobacco extract mixes tobacco extract and magnetic chemical filler, and the weight ratio of tobacco extract and chemical filler is 1: 5～15, puts into extractor then, feeds the lipid material in the supercritical fluid extraction tobacco extract;
(3) select a kind of in ethanol, acetone and the water for use as entrainment agent, feed mixing tank and extract fluid and mix, entrainment agent is 2: 8～100 with extraction fluidic volume ratio, through the preheating can preheating, 45 ℃～50 ℃ of preheating temperatures enter extractor again, and the tobacco extract after the degreasing is carried out cycling extraction, extracting pressure is 15～50 MPas, and extraction temperature is 45 ℃～50 ℃; When selecting for use ethanol to be entrainment agent, the alcoholic acid mass percentage concentration is 50%～98%.
(4) gains that will go up step separate through separator, and the fluid that obtains is required tobacco cleaned oil.
Adopt second-stage separator to separate the tobacco cleaned oil of step (4) gained, at first enter first step separator and separate, the separating pressure 5-15 MPa of first step separator, 30 ℃～80 ℃ extraction components of temperature are separated from the separator bottom; The fluid that comes out from first separator enters second stage separator again, further to product separation; The separating pressure 2-10 MPa of second stage separator, 10 ℃～60 ℃ of temperature; Two absolute oil fragrance differences that separator obtains can be allocated or use separately, and last supercutical fluid is got back to basin through behind the purification utensil, reenters cycling extraction.
Described chemical filler is selected from a kind of in granulated glass sphere, Raschig ring or the rectangular saddle ring.
Described supercutical fluid is selected from a kind of in carbonic acid gas or the propane.
When supercutical fluid adopted the carbon dioxide degreasing, pressure was 6～15 MPas, 20 ℃～40 ℃ of temperature; When supercutical fluid adopted the propane gas degreasing, pressure was 3～10 MPas, and temperature is 30 ℃～150 ℃.
The tobacco cleaned oil of the present invention's extraction, outward appearance is brown fluid, limpid transparent, has pure tobacco characteristic perfume, this tobacco cleaned oil through 2～5 times of 50%-95% alcohol dilutions, evenly is sprayed in the pipe tobacco in 0.1～0.2 ratio that restrains absolute oil/50 kilogram pipe tobacco, rolls into cigarette, smoke panel test through the smoke panel test group of smokeing panel test of composition of personnel of specialty, smoking result sees Table 1.
Smoking result shows that tobacco cleaned oil provided by the invention can increase cigarette perfume (or spice) after adding cigarette, and the harmony flue gas makes the flue gas exquisiteness soft, increases sweet sense, and can reduce to stimulate, and covers assorted gas, is a kind of high-quality essence spice for cigarette.
The present invention compared with prior art has following beneficial effect:
1. before supercritical extraction, earlier tobacco is carried out pre-treatment and make tobacco extract; Be raw material with commercially available tobacco extract perhaps, the object of supercritical fluid extraction is a tobacco extract, has increased the tap density of material, has improved the filling capability and the absolute oil output capacity of extraction kettle.Reduced equipment scale, realized continuous cycling extraction, reduced cost effectively.
2. the present invention sloughs the materials such as wax lipid that are unfavorable for cigarette smoking in the tobacco extract with supercutical fluid earlier.In single scrubbed gas solvent, add a spot of ethanol, acetone or water then as entrainment agent, become overcritical mixed stream.The more single supercutical fluids of character such as the dissolving power of this mixed stream, selectivity all change, can extract the flavour ingredient of low volatility, thereby widened the aroma component scope in the tobacco of supercritical fluid extraction, comprised the flavor matter of contained low volatility in the tobacco in the tobacco cleaned oil, make fragrance matter comprehensive and abundant more in the tobacco cleaned oil, the perfuming cigarette effect also has obvious improvement.
3. the productive rate of the tobacco cleaned oil that existing extracting process extracts is about 1%, and the tobacco cleaned oil amount that the present invention extracts from tobacco extract is the 8-15% of medicinal extract amount, the 3-6% that is equivalent to amount of tobacco, thus a new way provided for effective utilization of tobacco waste.
Embodiment
By specific embodiment given below, can further be well understood to the present invention.But they are not limitation of the invention.
Embodiment 1
Get Turkish tobaccos medicinal extract and the glass sphere filler mixes, the weight ratio of tobacco extract and glass sphere is 1: 6, puts into extractor then, feeds carbon dioxide, high-pressure pump is pressurized to 10 MPas, 35 ℃ of temperature, separating pressure 4 MPas, 40 ℃ of separation temperatures extracted 30 minutes, carried out degreasing.Change the composition of supercutical fluid then, squeezing into volume ratio by the entrainment agent pump is that 2% ethanol is entrainment agent, necessary mixing tank and the carbon dioxide mix of adding earlier of entrainment agent ethanol is even, then through preheating can 50 ℃ of following preheatings, enter extractor and carry out cycling extraction, extracting pressure is 38 MPas, and temperature is 50 ℃.After 90 minutes, from separator, emit tobacco cleaned oil.This product appearance is limpid, has the Turkish tobaccos characteristic perfume, and the solvability in tobacco flavoring common solvent such as edible ethanol, propylene glycol is fine.Quality test the results are shown in Table 2.
Embodiment 2
Removing chemical filler is Raschig ring, and the weight ratio of tobacco extract and Raschig ring is outside 1: 9, and other process is with embodiment 1.
Embodiment 3
Removing chemical filler is rectangular saddle ring, and the weight ratio of tobacco extract and rectangular saddle ring is outside 1: 6, and other process is with embodiment 1.
Embodiment 4
Remove entrainment agent and adopt acetone, supercutical fluid adopts propane, and the volume ratio of acetone and propane is outside 6%, and other process is with embodiment 1.
Embodiment 5
Get Red River flue-cured tobacco medicinal extract and Raschig ring filler and mix, put into extractor, feed carbon dioxide, high-pressure pump is pressurized to 6 MPas, 35 ℃ of temperature, and separating pressure 4 MPas, 40 ℃ of separation temperatures extracted 50 minutes, carried out degreasing.Change the composition of supercutical fluid then, adding volume ratio by the entrainment agent pump is that 8% ethanol is entrainment agent, entrainment agent must add earlier mixing tank and carbon dioxide and mix, then through preheating can 45 ℃ of following preheatings, feed extractor again and carry out cycling extraction, extracting pressure is 40 MPas, temperature is 45 ℃, after 120 minutes, emits tobacco extracts from separator, contain part ethanol in the extract, obtain pure tobacco cleaned oil through vacuum concentration.This product appearance is limpid, has the tobacco characteristic perfume, and is fine to the solvability of edible ethanol, propylene glycol.Quality test the results are shown in Table 3.
Table 1.
Table 2.
| Sample number into spectrum | ET200206003 | |
| The sample title | Turkish tobaccos absolute oil Z3-1 | |
| Sample presentation unit | Tobacco cleaned oil development group | |
| Test item | Detected result | Detect foundation |
| Acid number | 48.0 | YC/T145.1 --1998 | YC/T145.9 --1998 |
| Relative density d 20 20 | 1.0037 | |
| Refractive index n D 20 | 1.4892 | |
| Molten mixed degree in the ethanol (25 ℃) | The 1g sample is dissolved in the ethanolic soln of 0.5-20 volume 95%. | |
| Outward appearance and clarity | Brown half-cream body clarification | |
| Volatile component total amount (m/m) % | 5 | |
| As. content (mg/kg) | ＜3 | GB8450-87 |
| Heavy metal (in Pb) content (mg/kg) | ＜40 | GB8451-87 |
Table 3.
| Sample number into spectrum | ET200206004 | |
| The sample title | Red River cigarette absolute oil H3-8 | |
| Sample presentation unit | Tobacco cleaned oil development group | |
| Test item | Detected result | Detect foundation |
| Acid number | 45.0 | YC/T145.1 --1998 | YC/T145.9 --1998 |
| Relative density d 20 20 | 0.9837 | |
| Refractive index n D 20 | 1.4592 | |
| Molten mixed degree in the ethanol (25 ℃) | The 1g sample is dissolved in the ethanolic soln of 0.5-20 volume 95%. | |
| Outward appearance and clarity | The clarification of light brown half-cream body | |
| Volatile component total amount (m/m) % | 10 | |
| As. content (mg/kg) | ＜3 | GB8450-87 |
| Heavy metal (in Pb) content (mg/kg) | ＜40 | GB8451-87 |
Claims (7)
1. the preparation method of a tobacco cleaned oil, this method comprises the step of following order:
(1) degreasing of tobacco extract mixes tobacco extract and magnetic chemical filler, and the weight ratio of tobacco extract and chemical filler is 1: 5～15, puts into extractor then, feeds the lipid material in the supercritical fluid extraction tobacco extract;
(2) select a kind of in ethanol, acetone and the water for use as entrainment agent, feed mixing tank and extract fluid and mix, entrainment agent is 2～8: 100 with extraction fluidic volume ratio, through the preheating can preheating, 45 ℃～50 ℃ of preheating temperatures enter extractor again, and the tobacco extract after the degreasing is carried out cycling extraction, extracting pressure is 15～50 MPas, and extraction temperature is 45 ℃～50 ℃;
(3) gains that will go up step separate through separator, and the fluid that obtains is required tobacco cleaned oil.
2. according to the preparation method of the tobacco cleaned oil of claim 1, when selecting for use ethanol to be entrainment agent, the alcoholic acid mass percentage concentration is 50%～98%.
3. according to the preparation method of the tobacco cleaned oil of claim 1, comprise that further the tobacco cleaned oil with step (3) gained separates with second-stage separator, at first entering first step separator separates, the separating pressure 5-15 MPa of first step separator, 30 ℃～80 ℃ extraction components of temperature are separated from the separator bottom; The fluid that comes out from first separator enters second stage separator again, further to product separation; The separating pressure 2-10 MPa of second stage separator, 10 ℃～60 ℃ of temperature; Two absolute oil fragrance differences that separator obtains can be allocated or use separately, and last supercutical fluid is got back to basin through behind the purification utensil, reenters cycling extraction.
4. according to the preparation method of the tobacco cleaned oil of claim 1, wherein said chemical filler is selected from a kind of in granulated glass sphere, Raschig ring or the rectangular saddle ring.
5. according to the preparation method of the tobacco cleaned oil of claim 1, wherein said supercutical fluid is selected from a kind of in carbonic acid gas or the propane.
6. according to the preparation method of the tobacco cleaned oil of claim 5, when supercutical fluid adopted carbon dioxide, pressure was 6～15 MPas, 20 ℃～40 ℃ of temperature.
7. according to the preparation method of the tobacco cleaned oil of claim 5, when supercutical fluid adopted the propane gas degreasing, pressure was 3～10 MPas, and temperature is 30 ℃～150 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021337586A CN1181169C (en) | 2002-09-13 | 2002-09-13 | Method for preparing pure tobacco oil |
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| CNB021337586A CN1181169C (en) | 2002-09-13 | 2002-09-13 | Method for preparing pure tobacco oil |
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| CN1181169C true CN1181169C (en) | 2004-12-22 |
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| US8887737B2 (en) * | 2005-07-29 | 2014-11-18 | Philip Morris Usa Inc. | Extraction and storage of tobacco constituents |
| CN1860947B (en) * | 2006-06-16 | 2010-05-12 | 中国烟草总公司郑州烟草研究院 | Supercritical carrot extractive juice, and its application in perfuming of cigarette |
| CN100415126C (en) * | 2006-07-24 | 2008-09-03 | 宋光泉 | Method for extracting tobacco essence perfume |
| CN102212423B (en) * | 2011-04-14 | 2013-03-06 | 新疆科宇科技有限公司 | Carbon dioxide supercritical extraction method for extracting Ziziphora bungeana Juz. oil by using alcohol as entrainer |
| CN103131536B (en) * | 2011-11-29 | 2015-03-04 | 福建中烟工业有限责任公司 | Preparation device and preparation method of essence and flavor powder |
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| CN103783660B (en) * | 2014-01-22 | 2015-11-18 | 江苏中烟工业有限责任公司 | The supercritical extraction method of flavor matter and application thereof in a kind of tobacco leaf fragment |
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