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CN1166753C - Method for deep-processing tobacco extract to prepare tobacco cleaned oil and enriched solanesol - Google Patents

Method for deep-processing tobacco extract to prepare tobacco cleaned oil and enriched solanesol Download PDF

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Publication number
CN1166753C
CN1166753C CNB01108703XA CN01108703A CN1166753C CN 1166753 C CN1166753 C CN 1166753C CN B01108703X A CNB01108703X A CN B01108703XA CN 01108703 A CN01108703 A CN 01108703A CN 1166753 C CN1166753 C CN 1166753C
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China
Prior art keywords
tobacco
cleaned oil
solanesol
enriched
oil
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Expired - Fee Related
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CNB01108703XA
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CN1400300A (en
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孔宁川
唐自文
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Yunnan Ruisheng Science & Technology Co Ltd
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Yunnan Ruisheng Science & Technology Co Ltd
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Abstract

The present invention relates to a method for preparing tobacco cleaned oil and enriched solanesol by deeply processing tobacco extract, which comprises the steps: using tobacco extract as raw material; processing the tobacco extract in segments by a molecular distillation and short-path distillation technology through controlling the vacuum degree from 0.1 to 100Pa and the evaporating temperature from 80 to 220DEG C; obtaining the front segment of high-vacuum tobacco cleaned oil at the vacuum degree of 0.1 to 100Pa and the evaporating temperature of 80 to 180DEG C; processing the separated leftovers of the front segment of the cleaned oil at the vacuum degree of 0.1 to 10Pa and the evaporating temperature of 180 to 220 DEG C to obtain the back segment of the high-vacuum tobacco cleaned oil, wherein the molecular distillation residues are the segments of black enriched solanesol. In the method, the valuable ingredients in tobacco extract are comprehensively used, the contents of fragrance increasing ingredients of tobacco cleaned oil are enhanced, and the application range of tobacco cleaned oil is widened. Thus, the tobacco cleaned oil can be used for adding perfume to tobaccos and for adjusting daily and chemical essence.

Description

A kind of method to tobacco extract deep processing tobacco curing grass absolute oil and enriched solanesol
" technical field "
The present invention relates to the tobacco preparation field, particularly a kind of method that from tobacco extract, prepares tobacco cleaned oil and enriched solanesol.
" background technology "
Tobacco is a kind of important cash crop, gathers tobacco, produces a large amount of tobacco leaf small shreds, offal and offal in the production process of baking and cigarette.Sign and be worth for a short time in tobacco leaf small shreds, offal and offal for production of cigarettes, thereby go out of use mostly, these wastes not only cause the waste but also the contaminate environment of tobacco resource.Over nearly more than 20 years, the numerous scientific workers of China have carried out a large amount of research to the utilization of the various wastes of tobacco, have obtained the scientific and technological achievement of a lot of practicality, as using tobacco rod slurrying, system shaving board; With tobacco rod, discarded tobacco leaf, waste tobacco, offal the like waste extraction nicotine, plant pesticide, Nicotine, fructose, pectin, tobacco essential oil, eggplant Buddhist nun alcohol, make tobacco extract etc.But China at present the tobacco extract that extracts with tobacco waste is produced high-quality tobacco cleaned oil by the molecular distillation method and the applied research of enriched solanesol still had bibliographical information in the end.Tobacco cleaned oil is the natural perfume product, is mainly used in tobacco flavoring, and the raising physiological strength is arranged, and covers assorted gas, improves and inhales flavor, the fragrant effect of promoting or transferring cigarette.Domestic most employing traditional method prepares tobacco cleaned oil at present, promptly with organic solvent tobacco (comprising tobacco leaf, tobacco leaf fragment, offal, offal) is extracted, and reconcentration removes the preparation tobacco extract that desolvates.The tobacco extract dissolve with ethanol is removed the part resin through freezing treatment, concentrates to obtain tobacco cleaned oil.Adopt the tobacco cleaned oil composition complexity of this method preparation, the fragrant composition that causes that not only contains in the tobacco contains eggplant Buddhist nun alcohol, glyceryl ester and pigment etc. simultaneously.Cause in the product that fragrant component content is low, color and luster is dark, can only be used for the perfuming of cigarette products.
Development along with supercritical extraction method, there is report to adopt supercritical extraction method to prepare tobacco cleaned oil, disclose as Chinese patent CN1127778A and to have utilized supercritical extraction method to prepare tobacco cleaned oil, it is to adopt carbonic acid gas or ethene supercritical extraction under high pressure to prepare tobacco cleaned oil from tobacco.The preparation method comprises: the extraction of raw materials pretreatment, one-level, secondary extraction-absorption and step such as separate.The supercritical fluid extraction that this invention is adopted one step from tobacco directly obtains tobacco cleaned oil, is ultimate aim with the preparation tobacco cleaned oil, does not consider the comprehensive utilization of other valuable substance in the tobacco.
Eggplant Buddhist nun alcohol is used for the side chain of synthesis of medical Coenzyme Q10 99.0.The method of traditional preparation process eggplant Buddhist nun alcohol is: after saponification was handled, solvent extraction concentrated preparation eggplant Buddhist nun alcohol first product with tobacco extract, and eggplant Buddhist nun alcohol first product obtains high-load eggplant Buddhist nun alcohol through column chromatography.Chinese patent CN1026485C discloses a kind of method for preparing eggplant Buddhist nun alcohol from mould cigarette or tobacco waste, preparation process is: come for after raw material (not containing offal) the oven dry fragmentation with mould cigarette or cigarette, the industrial normal hexane that adds 60~80% content is an extraction solvent, extraction temperature is 55~60 degrees centigrade, through twice extracting, obtain pasty solanesol after concentrating.The separation method of above-mentioned eggplant Buddhist nun alcohol is a ultimate aim to obtain eggplant Buddhist nun alcohol, does not consider to cause in the tobacco utilization of fragrant composition, can't avoid more lower boiling tobacco to cause fragrant composition and resin to the isolating influence of eggplant Buddhist nun alcohol.
" summary of the invention "
The technical problem to be solved in the present invention provides a kind ofly carries out the novel method that deep processing prepares tobacco cleaned oil and enriched solanesol to tobacco extract.Can fully utilize valuable composition in the tobacco extract, promptly consider from tobacco extract, to obtain high-quality tobacco cleaned oil enriched solanesol simultaneously.
For reaching the purpose of technical solution problem, the present invention adopts molecular distillation and minor axis distillation technique, obtains high-quality tobacco cleaned oil and enriched solanesol from tobacco extract.Because tobacco causes fragrant composition (as nicotine in the tobacco extract, hot phytadiene, carboxylic acid, carboxylicesters, phytol, solanone, dihydroactinidiolide, trans-Damascenone, Megastigmatrienone etc.) molecular weight less (with respect to eggplant Buddhist nun alcohol, glyceryl ester, the molecular weight of pigment), boiling point is relatively low, and that the non-tobacco in the tobacco extract causes fragrant composition (as eggplant Buddhist nun alcohol, glyceryl ester and pigment) molecular weight is bigger, and boiling point is higher relatively, thereby can the different tobacco compositions that boiling point differs greatly be separated by the control of distillation vacuum tightness and vaporization temperature.For preventing to cause decomposition and the polymerization at high temperature of fragrant composition in the tobacco, simultaneously also in order to prevent that the decomposition at high temperature of eggplant Buddhist nun alcohol from destroying, thereby need to reduce distillation temperature and shorten and cause fragrant composition and eggplant Buddhist nun alcohol and high temperature duration of contact in the tobacco, the way that addresses this problem adopts molecular distillation and thin film distillation technology exactly, and molecular distillation is the best approach that satisfies this condition.Utilize molecular distillation to handle tobacco extract, (major ingredient is a nicotine, hot phytadiene, carboxylic acid can to obtain to keep the light high-quality tobacco cleaned oil of tobacco feature fragrance, carboxylicesters, phytol, solanone, dihydroactinidiolide, trans-Damascenone, Megastigmatrienone etc., annotate: different varieties tobacco cleaned oil composition is variant), while enriched solanesol (major ingredient is eggplant Buddhist nun alcohol, glyceryl ester and pigment) in the molecular distillation residue.The enrichment section of eggplant Buddhist nun alcohol can obtain eggplant Buddhist nun alcohol by eggplant Buddhist nun alcohol traditional separation method.It is low that the separation that molecular distillation is used for tobacco extract has temperature, and the efficient height does not destroy the heat-sensitive materials (high temperature decomposes down or the polymeric material easily) in the tobacco, advantages such as good separating effect.
Provided by the present inventionly tobacco extract is carried out the technical solution that deep processing prepares tobacco cleaned oil and enriched solanesol be, the employing tobacco extract is a raw material, it is characterized in that, adopt molecular distillation and minor axis distillation technique, basic technology is: tobacco extract is sent in the vaporizer of molecular distillation, in 0.1~100 handkerchief vacuum tightness; 80~220 degrees centigrade of vaporization temperatures, medicinal extract flow velocity, scraper plate rotating speed form uniform thin film with material and are advisable on the evaporation wall, by the control of vacuum tightness and vaporization temperature, tobacco extract is carried out staging treating.In 0.1~100 handkerchief vacuum tightness; Under the condition of 80~180 degrees centigrade of vaporization temperatures, obtain the tobacco cleaned oil first product leading portion of semicure, the optimum separation condition is vacuum tightness 0.1~40 handkerchief, and vaporization temperature is 120~160 degrees centigrade.To isolate the residue medicinal extract of burley absolute oil first product leading portion in 0.1~10 handkerchief vacuum tightness, (the optimum separation condition is vacuum tightness 0.1~1 handkerchief under the condition of 180~220 degrees centigrade of vaporization temperatures, vaporization temperature is 180~200 degrees centigrade), obtain high vacuum sorrel tobacco cleaned oil back segment (it is main that tobacco causes fragrant composition), the molecular distillation residue is the eggplant Buddhist nun alcohol enrichment section (with eggplant Buddhist nun alcohol, glyceryl ester and pigment are main) of black.The tobacco cleaned oil first product is carried out deresination handle, prepare high-quality high vacuum tobacco cleaned oil leading portion.The molecular distillation residue is that eggplant Buddhist nun alcohol enrichment section can obtain high-content eggplant Buddhist nun alcohol by the processing of eggplant Buddhist nun alcohol traditional separation method.
Technical scheme provided by the present invention also can be, the employing tobacco extract is a raw material, it is characterized in that, adopt molecular distillation and minor axis distillation technique, basic technology is: the deresination of tobacco extract raw material is handled, obtain black tobacco cleaned oil first product, black tobacco cleaned oil first product is sent in the vaporizer of molecular distillation, in 0.1~100 handkerchief vacuum tightness; 80~220 degrees centigrade of vaporization temperatures, medicinal extract flow velocity, scraper plate rotating speed form uniform thin film with material and are advisable on the evaporation wall, by the control of vacuum tightness and vaporization temperature, the tobacco cleaned oil first product is carried out staging treating.In 0.1~100 handkerchief vacuum tightness, obtain the leading portion of light high vacuum tobacco cleaned oil in 80~180 degrees centigrade of vaporization temperatures (the optimum separation condition is 0.1~40 handkerchief vacuum tightness, 120~160 degrees centigrade of vaporization temperatures).To isolate the residuum of absolute oil leading portion in 0.1~10 handkerchief vacuum tightness, (the optimum separation condition is 0.1~1 handkerchief vacuum tightness under vaporization temperature 180~220 degrees celsius, 180~200 degrees centigrade of vaporization temperatures), obtain high vacuum tobacco cleaned oil back segment russet, the molecular distillation residue is the eggplant Buddhist nun alcohol enrichment section of black, handles to obtain high-content eggplant Buddhist nun alcohol by eggplant Buddhist nun alcohol traditional separation method.
The present invention produces tobacco cleaned oil and enriched solanesol owing to adopted molecular distillation technique under high vacuum condition, as long as by the control to vacuum tightness and vaporization temperature, just can prepare high-quality tobacco cleaned oil and enriched solanesol from tobacco extract.It is dark that the tobacco cleaned oil of the present invention's preparation has been eliminated the tobacco cleaned oil product color of traditional method preparation, the shortcoming of appearance poor, improved the content that tobacco cleaned oil causes fragrant composition, remove eggplant Buddhist nun alcohol, glyceryl ester and pigment in the tobacco cleaned oil, widened the range of application of tobacco cleaned oil, the perfuming that makes it not only to can be used for tobacco also can be used for allocating daily chemical essence.In the sepn process of eggplant Buddhist nun alcohol, avoid tobacco to cause of the influence of fragrant composition, reduce isolating workload, improve separation efficiency mask work.Adopt the method that from the clean cream of tobacco, prepares tobacco cleaned oil and enriched solanesol provided by the present invention can obtain satisfied result.Experimental data is as shown in the table:
The preparation method Appearance luster Major ingredient and content
Traditional method tobacco curing grass absolute oil Brown black or black Tobacco causes (55~75%) such as fragrant composition (20~35%) eggplant Buddhist nun alcohol (5~10%) glyceryl ester and pigments
Tobacco curing grass absolute oil leading portion of the present invention Yellow or red Tobacco causes fragrant composition (greater than 98%)
Tobacco curing grass absolute oil back segment of the present invention Sorrel Cause fragrant composition (greater than 85%) in the tobacco
Eggplant Buddhist nun alcohol enrichment section of the present invention Black (80~90%) such as eggplant Buddhist nun alcohol (10~20%) glyceryl ester and pigments
" description of drawings "
Fig. 1 carries out the scheme that deep processing prepares tobacco cleaned oil and enriched solanesol for the present invention to tobacco extract.Fig. 2 carries out another program that deep processing prepares tobacco cleaned oil and enriched solanesol for the present invention to tobacco extract." embodiment "
Below, describe embodiments of the invention in conjunction with the accompanying drawings in detail.
Embodiment one: get 150 kilograms of Baoshan Turkish tobaccos fragment boiling ranges and be that 60~90 degrees centigrade of sherwood oils are cold carries twice, concentrate 4.5~5 kilograms of Turkish tobaccos medicinal extract.With 95% dissolve with ethanol of 4~6 times of volumes, the freezing treatment after-filtration is removed the resin of separating out, concentrate 3.5~4 kilograms of Turkish tobaccos absolute oil.The Turkish tobaccos absolute oil is handled with molecular distillation, control vacuum tightness is 0.1~0.2 handkerchief, vaporization temperature is 80 degrees centigrade, get high vacuum Turkish tobaccos absolute oil leading portion 450~550 grams, the residuum of isolating the absolute oil leading portion is distilled under 180~200 degrees centigrade of vaporization temperature conditions, get high vacuum spices absolute oil back segment 1000~1300 grams.With molecular distillation residue 1800~2300 gram with after the 5% sodium hydroxide solution saponification, petroleum ether extraction concentrate eggplant Buddhist nun alcohol first product, get eggplant Buddhist nun alcohol (greater than 90%) 150~200 through column chromatography and restrain.(see figure 2)
Embodiment two: getting Red River, 150 kilograms of Yunnan flue-cured tobacco fragment boiling range is that 60~90 degrees centigrade of sherwood oil heat are carried, concentrate 3.8~4.2 kilograms of flue-cured tobacco medicinal extract.Handle with molecular distillation, control vacuum tightness is 10 handkerchiefs, vaporization temperature is 120 degrees centigrade, get high vacuum tobacco cleaned oil first product leading portion 1300~1500 grams, the residuum of isolating the absolute oil leading portion is distilled under 180~200 degrees centigrade of vaporization temperature conditions, high vacuum tobacco cleaned oil back segment 150~250 gram, with high vacuum flue-cured tobacco absolute oil first product leading portion with 2~4 times of 95% dissolve with ethanol freezing treatment, after removing by filter the resin of separating out, concentrate to such an extent that high vacuum flue-cured tobacco absolute oil leading portion 350~450 restrains.Molecular distillation residue 2100~2500 gram, with 5% sodium hydroxide solution saponification after, petroleum ether extraction, concentrate eggplant Buddhist nun alcohol first product, get eggplant Buddhist nun alcohol (greater than 90%) 400~450 through column chromatography and restrain.(see figure 1)
Embodiment three: get double centner Zimbabwe tobacco fragment, carry twice with dehydrated alcohol heat, concentrate 18 kilograms of ethanol extracts, with boiling range is 60~90 degrees centigrade of petroleum ether extraction ethanol extracts three times, merge petroleum ether layer, concentrate 2.8 kilograms of Petroleum ether extraction cream, 4 times of 95% alcohol dilution, the freezing resin of removing, concentrate 2.0 kilograms of Zimbabwe's tobacco cleaned oils.Handle with molecular distillation, vacuum tightness is 100 handkerchiefs, vaporization temperature is 180 degrees centigrade, get Zimbabwe's molecular distillation tobacco cleaned oil leading portion 280 grams, under 180~200 degrees centigrade of vaporization temperature conditions, distill the residuum of isolating the absolute oil leading portion to such an extent that Zimbabwe's molecular distillation tobacco cleaned oil back segment 130 restrains, molecular distillation isolate residue eggplant Buddhist nun alcohol enrichment section behind the tobacco cleaned oil with 5% sodium hydroxide solution saponification after, petroleum ether extraction, concentrate eggplant Buddhist nun alcohol first product, get eggplant Buddhist nun alcohol (greater than 90%) 190 grams through column chromatography.(see figure 2)

Claims (3)

1, a kind of method to tobacco extract deep processing tobacco curing grass absolute oil and enriched solanesol, the employing tobacco extract is a raw material, it is characterized in that, adopts molecular distillation and minor axis distillation technique, basic technology is: tobacco extract is sent in the vaporizer of molecular distillation, in 0.1~100 handkerchief vacuum tightness; Under 80~220 degrees centigrade of vaporization temperatures, control by vacuum tightness and vaporization temperature, tobacco extract is carried out stepwise distillation, in 0.1~100 handkerchief vacuum tightness, 80~180 degrees centigrade of vaporization temperatures obtain the tobacco cleaned oil leading portion, will isolate the residuum of absolute oil leading portion at vacuum tightness 0.1~10 handkerchief, obtain high vacuum tobacco cleaned oil back segment under vaporization temperature 180~220 degrees celsius, the molecular distillation residue is the eggplant Buddhist nun alcohol enrichment section of black.
2, the method for preparing tobacco cleaned oil and enriched solanesol as claimed in claim 1 is characterized in that, earlier the deresination of tobacco extract raw material is handled, and sends into vaporizer again and carries out subsequent disposal.
3, the method for preparing tobacco cleaned oil and enriched solanesol as claimed in claim 2 is characterized in that, the processing condition of described preparation tobacco cleaned oil leading portion are that vacuum tightness is 0.1~40 handkerchief; Vaporization temperature is 120~160 degrees centigrade; The processing condition of described preparation tobacco cleaned oil back segment are 0.1~1 handkerchief vacuum tightness; Vaporization temperature is: 180~200 degrees centigrade.
CNB01108703XA 2001-08-01 2001-08-01 Method for deep-processing tobacco extract to prepare tobacco cleaned oil and enriched solanesol Expired - Fee Related CN1166753C (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
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US9022040B2 (en) 2010-03-09 2015-05-05 British American Tobacco (Investments) Limited Methods for extracting and isolating constituents of cellulosic material

Families Citing this family (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100398100C (en) * 2005-09-27 2008-07-02 四川大学 Liquid-liquid two-phase extraction method of high-content solanesol extract
CN101284765B (en) 2008-02-20 2011-03-30 西北师范大学 A method for microwave-assisted extraction of solanesol from potato stem and leaf waste
CN102041174B (en) * 2011-01-07 2012-05-30 江苏中烟工业有限责任公司 Preparation method of moss-flavored tobacco flavor and its application in cigarette flavoring
CN103484252A (en) * 2013-09-11 2014-01-01 上海聚华科技股份有限公司 Zimbabwe tobacco essential oil preparation method
CN104856216A (en) * 2015-05-31 2015-08-26 中国烟草总公司郑州烟草研究院 Treatment method for concrete and absolute type natural extractive suitable for electronic cigarette
CN107802027A (en) * 2017-09-29 2018-03-16 昆明坤九香精香料有限公司 A kind of method that pure tobacco oil is prepared using biology enzyme
CN108395932A (en) * 2018-03-29 2018-08-14 武汉黄鹤楼香精香料有限公司 A kind of preparation method of cigarette jasmine oil
CN108192726A (en) * 2018-03-29 2018-06-22 武汉黄鹤楼香精香料有限公司 A kind of preparation method of cigarette tree moss absolute
CN109700068B (en) * 2019-03-05 2021-11-26 云南中烟新材料科技有限公司 Method for preparing sun-cured tobacco absolute oil by oil bleaching method and application thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US9022040B2 (en) 2010-03-09 2015-05-05 British American Tobacco (Investments) Limited Methods for extracting and isolating constituents of cellulosic material
EP2544560B1 (en) 2010-03-09 2017-12-20 British American Tobacco (Investments) Limited Methods for extracting and isolating constituents of cellulosic material

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