CN111035058B - Preparation method of tar extract in waste cigarette butts and application of tar extract in cigarettes - Google Patents
Preparation method of tar extract in waste cigarette butts and application of tar extract in cigarettes Download PDFInfo
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- CN111035058B CN111035058B CN201911179718.0A CN201911179718A CN111035058B CN 111035058 B CN111035058 B CN 111035058B CN 201911179718 A CN201911179718 A CN 201911179718A CN 111035058 B CN111035058 B CN 111035058B
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B15/00—Chemical features or treatment of tobacco; Tobacco substitutes, e.g. in liquid form
- A24B15/18—Treatment of tobacco products or tobacco substitutes
- A24B15/24—Treatment of tobacco products or tobacco substitutes by extraction; Tobacco extracts
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24B—MANUFACTURE OR PREPARATION OF TOBACCO FOR SMOKING OR CHEWING; TOBACCO; SNUFF
- A24B3/00—Preparing tobacco in the factory
- A24B3/12—Steaming, curing, or flavouring tobacco
Abstract
The invention provides a preparation method of a tar extract in waste cigarette butts and application of the tar extract in cigarettes, wherein the method comprises the following steps: (1) adding the waste cigarette butts into an organic solvent for ultrahigh pressure extraction, and performing vacuum filtration after extraction to obtain an extracting solution; (2) and filtering the extracting solution by using an ultrafiltration membrane with the KD of 10-50 KD to obtain a dialysate, namely the tar extract. The method takes the waste cigarette butts as raw materials, utilizes organic solvent ultrahigh pressure extraction and filtration membrane separation, removes tar macromolecule harmful ingredients in the waste cigarette butts, retains micromolecule components with aroma characteristics, can be used as aroma ingredients to be applied to spices or cigarettes, improves aroma, smoke and taste characteristics of the cigarettes, and provides an effective way for application of low-grade tobacco leaves in middle and low-end cigarettes.
Description
Technical Field
The invention relates to a preparation method of a tar extract in waste cigarette butts and application of the tar extract in cigarettes, belonging to the technical field of tobacco processes.
Background
The cigarette butt refers to the residual part of the cigarette after burning and smoking, and mainly comprises tipping paper at the outer layer, fiber tows wrapped by forming paper at the inner layer and main stream smoke particulate matters intercepted in the burning and smoking process. China is a large country for cigarette production and consumption, and a large amount of waste cigarette butts are correspondingly produced along with the consumption of a large amount of cigarettes every year, so that the environment is polluted. The discarded cigarette butts not only contain loose paper and tows, but also contain a large amount of tar substances, and the cigarette tar not only contains aroma components which have positive effects on sensory quality, such as alcohols, ketones, furans, pyrazines, esters and the like, but also contains nicotine which can improve the physiological satisfaction of consumers, and also contains harmful substances which have obvious negative effects on sensory, such as amines, aldehydes and the like. Therefore, the waste cigarette butts are used as raw materials, tar substances with aroma characteristics are extracted, the pollution of the waste cigarette butts to the environment can be avoided, the effective components of the waste cigarette butts can be recycled, and the method has important significance for circular economy and sustainable development.
CN109959649A discloses a cigarette tar extract with chemiluminescence property, and the preparation method of the cigarette tar extract comprises the following steps: adding reagent into cigarette tar for extraction to obtain cigarette tar extract. The cigarette tar can be prepared by the following steps: smoking the cigarette, filtering the generated smoke, and collecting the smoke particle phase substances to obtain the cigarette tar. In the patent, the cigarette tar extract is prepared by ultrasonic extraction in an open system under natural light conditions, so that the contained luminescent substance has stable property and is insensitive to factors such as illumination, oxygen, temperature and the like; the extract has wide luminescence response range to medium pH value, and can generate chemiluminescence reaction under acidic, neutral or alkaline conditions. In the patent, the cigarette tar is the tar in the smoke particulate matter, and the prepared tar extract has a luminous property, and does not relate to the extraction of the tar in the waste cigarette butts to obtain the extract with a fragrance characteristic.
CN102559388A discloses a tobacco essential oil, a preparation method thereof and an application thereof in cigarettes, wherein the tobacco essential oil is prepared by the following steps: waste and inferior tobacco powder → organic solvent extraction → essential oil crude extract → water vapor introduction → condensation → oil-water separation → tobacco essential oil. The tobacco essential oil of the invention is added into the cut tobacco of the cigarette as a flavoring agent, which can increase the herbal fragrance of the cigarette, improve the quality of the fragrance of the cigarette, reduce the stimulation and the miscellaneous gas of the tobacco and soften the smoke. The patent takes waste and inferior tobacco powder generated in the cigarette production process as a raw material, the waste and inferior tobacco powder does not contain tar components, and the patent does not relate to a preparation method of tar extract.
Disclosure of Invention
The invention aims to provide a preparation method of a tar extract in waste cigarette butts and application of the tar extract in cigarettes. The invention takes the waste cigarette butts as raw materials, adopts an organic solvent ultrahigh pressure extraction and filtration membrane separation method to obtain the tar extract, and applies the tar extract to cigarettes, thereby improving the fragrance of the cigarettes.
The waste cigarette butts which are used as raw materials are cigarette butts which are discarded in an ashtray or on a roadside and the like after the cigarette is consumed by people, and the cigarette butts are wide in raw material source and low in cost; the invention selects the cigarette end with yellow color, and the tar content is higher.
In a first aspect, the present invention provides a method for preparing a tar extract from waste cigarette butts, comprising the steps of:
(1) adding the waste cigarette butts into an organic solvent for ultrahigh pressure extraction, and performing vacuum filtration after extraction to obtain an extracting solution;
(2) and filtering the extracting solution by using an ultrafiltration membrane with the KD of 10-50 KD to obtain a dialysate, namely the tar extract.
Further, in the step (1), the ratio of the waste cigarette butts to the organic solvent is 1g: 5-35 mL; the organic solvent is at least one of methanol, ethanol, petroleum ether, n-hexane, dichloromethane and ethyl acetate.
Further, in the step (1), the pressure of the ultrahigh-pressure extraction is 100-700 MPa, the pressure maintaining time is 3-30 min, and the pressure relief time is 5-20 s.
Further, in the step (2), the pressure of the ultrafiltration membrane is 0.1-3.5 MPa, and the membrane flux is 10-50L/m2·h-1The temperature is 20-50 ℃.
Further, the method also comprises the step of carrying out reduced pressure distillation concentration on the dialysate.
Preferably, the temperature of the reduced pressure distillation is 30-50 ℃, and the pressure is 0.1-5 mmH.
Further, the method also comprises the step of pretreating the waste cigarette butts;
preferably, the pretreatment comprises the following specific operations: and tearing off the wrapping paper of the waste cigarette butts, and cutting the tows into small sections with the length less than 1 cm.
In a second aspect, the invention also provides a tar extract prepared by the method.
In a third aspect, the invention also provides the application of the tar extract in preparing a perfume, wherein the tar extract is used as a perfuming component in the perfume.
In a fourth aspect, the invention also provides application of the tar extract in preparing cigarettes.
Preferably, the tar extract is added into the cigarette auxiliary material or the cigarette re-making cut tobacco, and the addition amount of the tar extract is 2-5% of the weight of the cigarette.
The invention has the beneficial effects that:
(1) according to the invention, organic solvent ultrahigh-pressure extraction and filtration membrane separation are utilized, so that tar macromolecule harmful components in the waste cigarette butts are removed, micromolecule components with aroma characteristics are reserved, the tar macromolecule harmful components can be used as aroma components to be applied to spices or cigarettes, the aroma, smoke and taste characteristics of the cigarettes are improved, and an effective way is provided for the application of low-grade tobacco leaves in middle and low-end cigarettes.
(2) According to the invention, the tar extract with higher extraction rate is obtained from the waste cigarette butts by controlling the conditions of ultrahigh-pressure extraction of the organic solvent and separation by the filter membrane. The invention takes the waste cigarette butts as raw materials, which not only can avoid the pollution of the cigarette butts to the environment, but also can collect and utilize the byproduct tar after the cigarette is burnt and smoked.
Detailed Description
The present invention is described in detail with reference to specific examples, which are provided to facilitate the understanding of the technical solutions of the present invention by those skilled in the art, and the implementation or use of the present invention is not limited by the description of the present invention.
In the present invention, the raw materials and equipment used are commercially available or commonly used in the art, if not specified.
The methods in the examples are conventional in the art unless otherwise specified.
Example 1Preparation of tar extract from waste cigarette butts
A preparation method of a tar extract in waste cigarette butts comprises the following steps:
(1) pretreatment of waste cigarette butts: tearing off tipping paper of the waste cigarette butts, and cutting the fiber tow part into small sections with the length of less than 1 cm;
(2) adding 100g of waste cigarette butts into 1L of 75% (v/v) ethanol solution, then placing the mixture into an ultrahigh pressure PE bag for mixing, placing the PE bag into a high-pressure kettle, pressurizing to 300MPa, keeping for 10min, releasing the pressure for 10s, carrying out vacuum filtration on the extract at 0.02MPa, and taking the filtrate to obtain cigarette butts extract;
(3) subjecting the tobacco stalk extractive solution to dialysis separation with 30KD ultrafiltration membrane under 1.0MPa and with membrane flux of 30L/m2·h-1Collecting the dialysate at 30 deg.C;
concentrating the dialysate by reduced pressure distillation at 35 deg.C under 2mmH until no fraction is distilled out to obtain tar extract.
Performing GC/MS detection on tar extract to obtain tar extract containing furfural, furfuryl alcohol, ethylene glycol diacetate, 1- (1, 3-dioxolan-2-yl) acetone, 4-cyclopentene-1, 3-dione, methyl cyclopentenolone, nicotine, 2-acetylfuran, 2(5H) -furanone, 5-methylfuran aldehyde, 3-methyl-2-cyclopentene-1-one, methyl cyclopentenolone, benzyl alcohol, 2, 3-dimethyl-2-cyclopentenone, ethyl cyclopentenolone, 5-hydroxymethylfurfural, vanillin, megastigmatrienone A, 2,4, 4-trimethylpentane-1, 3-diylbis (2-methylpropionate), farnesol, 1-butyl-2-isobutyl phthalate, scopoletin, tributylprop-1-ene-1, 2, 3-tricarboxylate.
Wherein, the GC/MS conditions are as follows: HP6890-5973 gas chromatography-mass spectrometer
(1) GC conditions were as follows:
a chromatographic column: ULTRA2(50m 0.2mm i.d. 0.33 μm d.f.)
A detector: MS (Mass Spectrometry)
Carrier gas, flow rate: he, 0.6ml/min
Sample inlet temperature: 290 deg.C
Temperature rising procedure: 80 deg.C (1min)2 deg.C/min → 280 deg.C (10min)
Split ratio, sample injection amount: 1:10, 2. mu.l
(2) GC/MS conditions:
GC conditions were as follows: same as above
Transmission line temperature: 230 deg.C
Ion source temperature: 230 deg.C
Ionization energy: 70eV
Mass number range: 30 to 350u
Carrier gas: he (He)
MS spectrogram: NIsT library
Example 2Aroma-producing properties of cigarette tar extracts
The tar extract prepared in example 1 was added to a filter tip additive of a cigarette at an addition ratio of 2% by weight of the cigarette to prepare cigarette sample 1.
The tar extract obtained in example 1 was added to tobacco shreds of cigarettes at an addition ratio of 3% by weight of the cigarettes, to prepare cigarette sample 2.
The tar extract prepared in example 1 was added to tobacco shreds of cigarettes in an amount of 1% by weight of the cigarettes to prepare cigarette sample 3.
After the cigarette samples prepared by the scheme and the cigarettes without the tar extracts are balanced for 24 hours in a constant-temperature and constant-humidity environment with the temperature of (20 +/-1) DEG and the relative humidity of (60 +/-3)%, sensory evaluation is carried out on the cigarette samples by 10 or more smokers with reference to a tobacco product sensory evaluation method (YC/T415-.
TABLE 1 sensory evaluation results of cigarettes with different amounts of tar extract added
As shown in Table 1, compared with a control group, after the tar extract prepared by the invention is added, the aroma quality of the cigarette is obviously improved, the aroma quantity is improved, the miscellaneous gas is reduced, and the penetrability is improved; the concentration and the strength are increased, and the smoke becomes more exquisite; reduced irritation, increased moistening feeling, reduced dryness, and improved sweet feeling. After the tar extract prepared by the invention is added, the smoke characteristic, the aroma characteristic and the taste characteristic of the cigarette can be effectively improved.
Example 3Selection of preparation Process conditions
1. Selection of ultrahigh pressure extraction pressure
20g of waste cigarette butts and 200mL of 75% (v/v) ethanol aqueous solution are mixed and added into a high-pressure PE bag, the waste cigarette butts are extracted at 200MPa, 300MPa, 400MPa and 500MPa respectively, the extraction time is 10min, the pressure relief time is 10s, the influence of different pressures on the extraction effect (the content of components extracted from each g of cigarette butts) is analyzed in a comparative way, and the detection result of the extracting solution is shown in Table 2. As is clear from Table 2, the 75% (v/v) ethanol aqueous solution had the best extraction effect of the tar extract having the aroma characteristics at 300 MPa.
TABLE 2 extraction Effect (mg/g) under different pressures
2. Selection of dwell time
20g of waste cigarette butts and 200mL of 75% (v/v) ethanol aqueous solution are mixed and added into a high-pressure PE bag, the waste cigarette butts are respectively extracted for 6min, 8min, 10min and 12min under the pressure of 300MPa, the pressure relief time is 10s, the influence of different extraction times on the extraction effect is analyzed in a comparative way, and the detection result of the extracting solution is shown in Table 3. As can be seen from Table 3, the extraction efficiency was the best when the pressure was maintained for 10 min.
TABLE 3 extraction Effect (mg/g) at different dwell times
The above description is only an example of the present application, and the protection scope of the present application is not limited by these specific examples, but is defined by the claims of the present application. Various modifications and changes may occur to those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the technical idea and principle of the present application should be included in the protection scope of the present application.
Claims (5)
1. A preparation method of a tar extract in waste cigarette butts is characterized by comprising the following steps:
(1) pretreating waste cigarette butts, tearing off tipping paper of the waste cigarette butts, cutting fiber tow parts into small segments with the length of less than 1cm, adding 100g of the waste cigarette butts into 1L of 75% (v/v) ethanol solution, then putting the waste cigarette butts into an ultrahigh pressure PE bag for mixing, putting the PE bag into a high-pressure kettle, pressurizing to 300MPa, keeping for 10min, releasing the pressure for 10s, carrying out vacuum filtration on extract liquor under 0.02MPa, and taking filtrate to obtain cigarette butts extract;
(2) filtering the extractive solution with 30KD ultrafiltration membrane under 1.0MPa with membrane flux of 30L/m to obtain dialysate2·h-1Concentrating the dialyzate by reduced pressure distillation at 30 deg.C, controlling the temperature at 35 deg.C and pressure at 2mmH, and distilling until no fraction is distilled out to obtain tar extract.
2. A tar extract made by the method of claim 1.
3. Use of a tar extract according to claim 2 for the preparation of a fragrance, wherein the tar extract is used as a perfuming ingredient in a fragrance.
4. Use of the tar extract of claim 2 for the preparation of cigarettes.
5. The application of claim 4, wherein the tar extract is added into cigarette auxiliary materials or cigarette re-making tobacco shreds, and the addition amount of the tar extract is 2-5% of the weight of the cigarette.
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| CN113383986B (en) * | 2021-07-13 | 2022-08-02 | 云南中烟工业有限责任公司 | Preparation of low-temperature fraction capable of improving strength applied to heated cigarettes and application of low-temperature fraction in heated cigarettes |
| CN113749281B (en) * | 2021-09-20 | 2022-12-27 | 河南中烟工业有限责任公司 | Method for preparing tobacco flavor by using waste tobacco leaves and application of tobacco flavor |
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| FR2499369A1 (en) * | 1981-02-12 | 1982-08-13 | Bonneau Marc | Removing harmful components from vegetable extracts - by filtration on semipermeable membranes |
| US4941484A (en) * | 1989-05-30 | 1990-07-17 | R. J. Reynolds Tobacco Company | Tobacco processing |
| CN100415126C (en) * | 2006-07-24 | 2008-09-03 | 宋光泉 | Method for extracting tobacco essence perfume |
| CN101810367A (en) * | 2009-02-19 | 2010-08-25 | 广西中烟工业有限责任公司 | Tobacco additive for increasing smoke concentration and preparation method and application thereof |
| US9220295B2 (en) * | 2010-12-01 | 2015-12-29 | R.J. Reynolds Tobacco Company | Tobacco separation process for extracting tobacco-derived materials, and associated extraction systems |
| GB201213870D0 (en) * | 2012-08-03 | 2012-09-19 | British American Tobacco Co | Tobacco extract, preparation thereof |
| CN103222679B (en) * | 2012-10-25 | 2015-03-11 | 湖北中烟工业有限责任公司 | Method for preparing tobacco fragment extractives by high-pressure-puffing-flocculation and application of extractives |
| CN102952639B (en) * | 2012-11-13 | 2014-09-10 | 广东中烟工业有限责任公司 | Preparation method of tobacco endogenous perfume and application thereof |
| CN106307604B (en) * | 2016-11-22 | 2018-01-02 | 中国烟草总公司郑州烟草研究院 | tobacco extract, extracting method and application |
| CN109007958B (en) * | 2018-09-13 | 2021-05-25 | 云南中烟工业有限责任公司 | Tobacco baking fragrant substance and preparation method and application thereof |
| CN109749850A (en) * | 2019-03-28 | 2019-05-14 | 江西中烟工业有限责任公司 | A kind of preparation method of Turkish tobaccos ultra high pressure extraction liquid Maillard reaction flavor and the application in cigarette |
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