CN111035056B - Preparation method of cigarette end tar extract and application of cigarette end tar extract in cigarettes - Google Patents
Preparation method of cigarette end tar extract and application of cigarette end tar extract in cigarettes Download PDFInfo
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- CN111035056B CN111035056B CN201911179702.XA CN201911179702A CN111035056B CN 111035056 B CN111035056 B CN 111035056B CN 201911179702 A CN201911179702 A CN 201911179702A CN 111035056 B CN111035056 B CN 111035056B
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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
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Abstract
The invention provides a preparation method of a cigarette end tar extract and application thereof in cigarettes, wherein the method comprises the step of performing supercritical carbon dioxide extraction on waste cigarette ends to obtain the tar extract; wherein the extraction pressure is 20-50 MPa, and the extraction temperature is 20-80 ℃. The invention takes the waste cigarette butts as raw materials, utilizes supercritical carbon dioxide extraction to prepare the tar extract, is applied to the heating non-combustion cigarettes, improves the characteristics of the aroma, the smoke and the taste of the heating non-combustion cigarettes, and effectively solves the problems of light cigarette aroma and the like of the heating non-combustion cigarettes. According to the invention, the tar extract with higher extraction rate is obtained from the waste cigarette butts by optimizing the conditions of supercritical carbon dioxide extraction. 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 utilize the byproduct tar after the cigarette is burnt and smoked.
Description
Technical Field
The invention relates to a preparation method of a cigarette butt tar extract with aroma characteristics and application of the cigarette butt tar extract in cigarettes, belonging to the technical field of tobacco processes.
Background
The cigarette end is the residual part of the cigarette after burning and smoking, mainly composed of tipping paper, fiber tows wrapped by forming paper, residual cigarette paper and cut tobacco, and the cigarette end mainly retains tar and other harmful particles in the particulate matters of the main stream smoke. A large amount of cigarettes are consumed in China every year, and accordingly a large amount of waste cigarette butts are produced, so that the environment is greatly polluted. The large amount of cigarette tar substances trapped in the waste cigarette butts not only contain aroma components which have positive effects on sensory quality, such as alcohols, ketones, furans, pyrazines, esters and the like, but also contain nicotine which can improve the physiological satisfaction of consumers, and also contain harmful substances which have obvious negative effects on sensory effects, 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 tobacco powder → organic solvent extraction → crude extract of essential oil → introduction of water vapor → 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 cigarette end tar extract and application thereof in cigarettes. The invention takes the waste cigarette butts as raw materials, adopts a supercritical carbon dioxide extraction method to obtain the tar extract with the components with the aroma characteristics, and applies the tar extract containing the aroma characteristics to the heating non-combustion cigarettes, thereby improving the cigarette aroma plumpness of the heating non-combustion cigarettes.
The waste cigarette butts as raw materials adopted by the invention are cigarette butts which are discarded in an ashtray or 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 invention provides a preparation method of a cigarette butt tar extract, which comprises the step of performing supercritical carbon dioxide extraction on waste cigarette butts to obtain the tar extract, wherein the extraction pressure is 20-50 MPa, and the extraction temperature is 20-80 ℃.
Preferably, the waste cigarette butts are added with an entrainer for supercritical carbon dioxide extraction, and the proportion of the entrainer to the waste cigarette butts is 1-20 ml: 1g of the total weight of the composition.
Preferably, the entrainer is selected from one or more of methanol, ethanol, petroleum ether, n-hexane, dichloromethane and ethyl acetate.
Preferably, the supercritical carbon dioxide extraction time is 1-15 min, and the flow rate of the carbon dioxide is 10-50 kg/h.
Preferably, the extraction is carried out using a supercritical fluid extraction apparatus: the pressure of the extraction kettle is 20-50 MPa, and the temperature is 20-80 ℃; the first pressure of the separation kettle is 5-10 MPa, and the temperature is 35-45 ℃; the pressure of the second separation kettle is 3-8 Mpa, and the temperature is 20-30 ℃.
Preferably, the method further comprises the step of pre-treating the waste cigarette butts;
preferably, the pretreatment specifically comprises the following steps: 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 cigarette auxiliary materials or cigarette secondary cut tobacco, and the addition amount of the tar extract is 2-5% of the weight of the cigarette.
Preferably, the cigarette is a cigarette which is not combusted by heating.
The invention has the beneficial effects that:
(1) the invention utilizes supercritical carbon dioxide extraction to prepare the tar extract with the characteristic component of aroma, and the tar extract is applied to the heating non-combustion cigarettes, so that the aroma, smoke and taste characteristics of the heating non-combustion cigarettes are improved, and the problems of light cigarette taste and insufficient cigarette aroma of the heating non-combustion cigarettes are effectively solved.
(2) According to the invention, the tar extract with higher extraction rate is obtained from the waste cigarette butts by optimizing the conditions of supercritical carbon dioxide extraction. 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 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 cigarette end tar extract
A preparation method of a cigarette end tar extract comprises the following steps:
(1) pretreatment of waste cigarette butts: tearing off tipping paper of the waste cigarette stub, removing cigarette paper and tobacco shred parts, collecting a tow part, and cutting the fiber tow part into small sections with the length of less than 1 cm;
(2) stirring and uniformly mixing 20g of treated waste cigarette butts and 200mL of 70% ethanol, and putting the mixture into an extraction kettle of a supercritical extraction device, wherein the pressure of the extraction kettle is 30MPa, and the temperature is 50 ℃; the pressure of the first separation kettle is 6MPa, the temperature is 42 ℃, the pressure of the second separation kettle is 5MPa, the temperature is 25 ℃, and CO is added2The flow rate is 20 kg/h; extracting for 3min after the pressure is stable, and collecting the obtained extract to obtain the 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, methylcyclopentenolone, nicotine, 2-acetylfuran, 2(5H) -furanone, phenol, 5-methylfuran aldehyde, 3-methyl-2-cyclopentene-1-one, 3, 4-dimethyl-2-cyclopentanone, methylcyclopentenolone, benzyl alcohol, 2, 3-dimethyl-2-cyclopentenone, 2, 6-dimethylphenol, ethylcyclopentenolone, 2,4, 6-trimethylphenol, ethyl maltol, 4-ethylguaiacol, ethanol, methanol, ethanol, methanol, cinnamaldehyde, 5-hydroxymethylfurfural, 2, 6-dimethoxyphenol, anisic aldehyde, 2-methylnaphthalene, vanillin, megastigmatrienone A, farnesol, 1-butyl-2-isobutyl phthalate, scopoletin, tributylprop-1-ene-1, 2, 3-tricarboxylate, oleamide and natural vitamin E.
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 butt tar extracts
The tar extract obtained in example 1 was added to a filter auxiliary material of a cigarette that was not burned under heating at an addition ratio of 3% by weight of the cigarette, to prepare a cigarette sample a that was not burned under heating (HnB sample a).
The tar extract obtained in example 1 was added to reconstituted tobacco shreds of a non-burning, heated cigarette at an addition ratio of 1% by weight of the non-burning, heated cigarette, to prepare a non-burning, heated cigarette sample B (HnB sample B).
The tar extract obtained in example 1 was added to reconstituted tobacco shreds of a non-burning, heated cigarette at an addition ratio of 3% by weight of the non-burning, heated cigarette, to prepare a non-burning, heated cigarette sample C (HnB sample C).
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 HnB cigarette samples by referring to a tobacco product sensory evaluation method (YC/T415-.
TABLE 1 sensory evaluation results
As shown in Table 1, compared with a control group, the cigarette fragrance plumpness of the cigarette which is not combusted by heating is obviously improved, and the fragrance amount and the fragrance quality are improved; the concentration and the strength are increased, and the fineness of the smoke is improved; reduced irritation, reduced dry feeling, enhanced moistening feeling, and good sweet feeling. After the tar extract prepared by the invention is added, the characteristics of smoke, aroma and taste of the cigarette which is not burnt after being heated can be effectively improved.
Example 3Selection of preparation Process conditions
1. Selection of supercritical extraction temperature
20g of the treated waste cigarette butts and 200mL of 70% (v/v) ethanol aqueous solution are mixed and put into a supercritical extraction kettle, the waste cigarette butts are extracted at 30 ℃, 40 ℃, 50 ℃ and 60 ℃ respectively for 3min, the influence of different extraction temperatures 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 tar extract having a component with a perfuming property at 50 ℃ in a 70% (v/v) ethanol aqueous solution was the most effective.
TABLE 2 extraction Effect (mg/g) at different extraction temperatures
2. Selection of supercritical extraction time
20g of the treated waste cigarette butts and 100mL of 70% (v/v) ethanol aqueous solution are mixed in a supercritical extraction kettle, the waste cigarette butts are respectively extracted for 1min, 3min, 5min and 7min at 50 ℃, the influence of different extraction time 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 supercritical extraction for 3min gave the best extraction results.
TABLE 3 extraction Effect (mg/g) for different extraction 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 method of preparing a cigarette butt tar extract, the method comprising:
(1) pretreatment of waste cigarette butts: tearing off tipping paper of the waste cigarette stub, removing cigarette paper and tobacco shred parts, collecting a tow part, and cutting the fiber tow part into small sections with the length of less than 1 cm;
(2) uniformly stirring 20g of pretreated waste cigarette butts and 200mL of 70% ethanol, putting into an extraction kettle of a supercritical extraction device, performing supercritical carbon dioxide extraction, and collecting the obtained extract, namely the tar extract; wherein the extraction pressure is 30MPa, the temperature is 50 ℃, the supercritical carbon dioxide extraction time is 3min, and the flow rate of the carbon dioxide is 20 kg/h; the pressure of the first separation kettle is 6MPa, the temperature is 42 ℃, the pressure of the second separation kettle is 5MPa, and the temperature is 25 ℃;
the tar extract is used for being added into cigarette auxiliary materials or cigarette reconstituted tobacco shreds, and the cigarette is a cigarette which is not burnt by heating.
2. A tar extract made by the method of claim 1.
3. Use of the tar extract of claim 2 for the preparation of cigarettes.
4. The application of claim 3, wherein the tar extract is added into cigarette auxiliary materials or cigarette re-making cut tobacco, and the addition amount of the tar extract is 2-5% of the weight of the cigarette.
5. The use according to claim 4, wherein the cigarette is a heat non-combustible cigarette.
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| CN113498874A (en) * | 2021-08-11 | 2021-10-15 | 河南金瑞香精香料有限公司 | Preparation method of heated cigarette with uniform alcohol release mouth by mouth |
| CN113754617B (en) * | 2021-09-09 | 2023-05-30 | 广州雅弥生物科技有限公司 | Refining method of furanone |
| CN114532581B (en) * | 2022-03-10 | 2022-12-23 | 浙江中烟工业有限责任公司 | Preparation method and application of acidic flavor components with characteristics of Canadian tobacco smoke |
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| US5328934A (en) * | 1992-10-27 | 1994-07-12 | Hoechst Celanese Corporation | Recycling cellulose esters from the waste from cigarette manufacture |
| US5504120A (en) * | 1994-03-18 | 1996-04-02 | Hoechst Celanese Corporation | Recycling cellulose esters from the waste from cigarette manufacture |
| US8887737B2 (en) * | 2005-07-29 | 2014-11-18 | Philip Morris Usa Inc. | Extraction and storage of tobacco constituents |
| RU2390285C1 (en) * | 2006-04-25 | 2010-05-27 | Джапан Тобакко Инк. | Cut tobacco and method for tobacco treatment |
| CN102199490B (en) * | 2010-03-24 | 2012-11-21 | 郑州轻工业学院 | Method for extracting neutral aroma compositions in tobacco |
| CN103675153B (en) * | 2013-12-26 | 2014-12-10 | 国家烟草质量监督检验中心 | Method for measuring main carbonyl compounds in cigarette filter through ultra-performance convergence chromatography |
| CN104450186B (en) * | 2014-10-29 | 2017-04-19 | 山东中烟工业有限责任公司 | Method for preparing tobacco herbal fragrant substance for cigarette solution of electronic cigarette |
| CN105861154A (en) * | 2016-03-30 | 2016-08-17 | 浙江中烟工业有限责任公司 | A method of directionally separating aroma substances from tobacco by utilizing supercritical extraction and molecule distillation and applications of the aroma substances |
| CN108998057B (en) * | 2018-07-18 | 2020-10-27 | 陕西科技大学 | Method for co-producing ester-rich pyrolysis oil and activated carbon by microwave depolymerization of waste filter tip |
| CN109181881A (en) * | 2018-10-18 | 2019-01-11 | 吕小萍 | A kind of nicotine tar extraction technology of preparing |
| CN110339628B (en) * | 2019-07-26 | 2020-07-07 | 河南农业大学 | Filter material prepared from cigarette butts, defective cigarette filters or waste acetate fibers, and preparation method and application thereof |
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