CN113974213B - Composite additive for reducing release amount of phenol in flue gas, and preparation method and application thereof - Google Patents

Composite additive for reducing release amount of phenol in flue gas, and preparation method and application thereof Download PDF

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Publication number
CN113974213B
CN113974213B CN202111476641.0A CN202111476641A CN113974213B CN 113974213 B CN113974213 B CN 113974213B CN 202111476641 A CN202111476641 A CN 202111476641A CN 113974213 B CN113974213 B CN 113974213B
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extract
phenol
composite additive
parts
release amount
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CN113974213A (en
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杨叶昆
李雪梅
李晶
谢姣
詹建波
余振华
耿永勤
孔维松
刘欣
黄海涛
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China Tobacco Yunnan Industrial Co Ltd
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China Tobacco Yunnan Industrial Co Ltd
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    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24DCIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
    • A24D3/00Tobacco smoke filters, e.g. filter-tips, filtering inserts; Filters specially adapted for simulated smoking devices; Mouthpieces for cigars or cigarettes
    • A24D3/06Use of materials for tobacco smoke filters
    • A24D3/061Use of materials for tobacco smoke filters containing additives entrapped within capsules, sponge-like material or the like, for further release upon smoking
    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24DCIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
    • A24D3/00Tobacco smoke filters, e.g. filter-tips, filtering inserts; Filters specially adapted for simulated smoking devices; Mouthpieces for cigars or cigarettes
    • A24D3/02Manufacture of tobacco smoke filters
    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24DCIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
    • A24D3/00Tobacco smoke filters, e.g. filter-tips, filtering inserts; Filters specially adapted for simulated smoking devices; Mouthpieces for cigars or cigarettes
    • A24D3/06Use of materials for tobacco smoke filters
    • A24D3/067Use of materials for tobacco smoke filters characterised by functional properties

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Manufacture Of Tobacco Products (AREA)

Abstract

The invention relates to a composite additive for reducing phenol release amount in flue gas, and a preparation method and application thereof, wherein the composite additive comprises the following raw materials in parts by weight: 1-20 parts of dark plum extract, 0-10 parts of wild jujube seed extract and 100 parts of propylene glycol. The composite additive is uniformly sprayed into tobacco shreds, so that the release amount of phenol in smoke can be obviously reduced, the taste of cigarettes is improved, the irritation is reduced, and the sensory quality of the cigarettes is improved.

Description

Composite additive for reducing release amount of phenol in flue gas, and preparation method and application thereof
Technical Field
The invention belongs to the technical field of tar and harm reduction of cigarettes, and particularly relates to a composite additive for reducing the release amount of phenol in smoke, a preparation method and application thereof.
Background
Smoking and health problems continue to be highly appreciated by the government, tobacco industry, and medical community. Tobacco contains a number of phenolic compounds, and currently identified phenolic compounds have been up to 280 or more [Baker RR,Massey ED,Smith G.An overview of the effects of tobacco ingredients on smoke chemistry andtoxicity[J].Food and Chemical Toxicology,2004,42:53-83], and are structurally classified into simple phenols and polyphenols. The simple phenol has strong volatility, enters a human body along with main stream smoke, and is a kind of harmful components needing to be focused in the main stream smoke of cigarettes. Wherein phenol has been listed by the Canadian government under 46 harmful components list and the WHO "tobacco products control research group" recommended control components list [Hoffmann D,Hoffmann I.The less harmfull cigarette:A controversial issue.A tribute to Ernst L.Wynder[J].Chemical Research in Toxicology,2001,14(7):761-791].
At present, the tobacco industry in China is actively advancing the harm-reducing and tar-reducing engineering, and phenol is also listed as a main harm-reducing object. A great deal of literature reports on a technical means for reducing phenol, mainly researches and develops a functional material of a filter tip, and selectively reduces harmful components in cigarette smoke. For example Xu Jianrong et al disclose the addition of glycin glycerides in cigarette filters to reduce the amount of phenol released in cigarette smoke [ use of amino acid glycerides to reduce the amount of phenol released in cigarette smoke, CN201610541856.9,20160712]. Xie Lanying et al discloses a forming paper composed of cellulose forming paper and a perfume-carrying substance doped polyvinylpyrrolidone micro-nano superfine fiber film layer on the surface of the cellulose forming paper, wherein the forming paper can selectively reduce the content of smoke phenol [ the superfine fiber functionalized cellulose forming paper with perfume-carrying and smoke phenol content selective reduction functions, and preparation and application thereof, CN201811324094.2,2018.11.08]. Wang Jin et al disclose a built-up additive (polyvinylpyrrolidone and vinylpyrrolidone-maleic acid copolymer) which can reduce the amount of released phenol in the smoke by adding to the filter tow [ a built-up additive and application for reducing the amount of released phenol in the smoke, CN201810237096.1,2018.03.21].
In the cigarette burning and smoking process, the time of smoke passing through the filter tip is very short, and meanwhile, the smoke of the cigarette is complex aerosol composed of thousands of components, and when the smoke passes through the filter tip, the adsorption effect of the disclosed functional material is influenced, so that the effect of reducing the release amount of phenol in the smoke is influenced.
The present invention has been made to solve the above problems.
Disclosure of Invention
The invention aims to provide a composite additive for reducing the release amount of phenol in flue gas, and a preparation method and application thereof, and the aim of the invention is realized by the following technical scheme:
The invention discloses a composite additive for reducing the release amount of phenol in flue gas, which comprises the following raw materials in parts by weight: 1-20 parts of dark plum extract, 0-10 parts of wild jujube seed extract and 100 parts of propylene glycol.
Preferably, the dark plum extract is prepared by the following method: removing impurities from dried mume fructus, pulverizing, adding 80-95v/v% ethanol, reflux extracting for 3 times, and concentrating under reduced pressure to obtain mume fructus ethanol extract; dispersing the obtained ethanol extract with water, adding petroleum ether solvent with volume 3 times of that of the sample, extracting for three times, and degreasing; concentrating the petroleum ether extract to obtain petroleum ether extract; extracting the water phase part with ethyl acetate for three times, and concentrating the ethyl acetate extract to obtain ethyl acetate extract; extracting the rest water phase part with n-butanol for three times, mixing the extractive solutions, and concentrating to obtain mume fructus extract.
Preferably, the spine date seed extract is prepared according to the following method: removing impurities from dried semen Ziziphi Spinosae, pulverizing, adding 95v/v% ethanol, reflux extracting for 3 times, and concentrating under reduced pressure to obtain semen Ziziphi Spinosae extract.
Preferably, the preparation method of the composite additive comprises the following steps: mixing mume fructus extract 1-20 parts, semen Ziziphi Spinosae extract 0-10 parts, propylene glycol 100 parts, and stirring for 5-10min to obtain the final product.
The invention discloses an application of the composite additive for reducing the release amount of phenol in smoke, which is characterized in that the composite additive is uniformly sprayed into tobacco shreds according to the mass of 0.05-0.5% of the tobacco shreds, and the tobacco shreds are baked, water is balanced and rolled into cigarette cigarettes.
The beneficial effects of the invention are as follows:
1. The compound additive mainly comprises dark plum extract, wild jujube seed extract and propylene glycol, and the wild jujube seed extract can be free. The composite additive is uniformly sprayed into tobacco shreds, can quickly and selectively reduce the release amount of phenol in the smoke, and has remarkable effect; meanwhile, the method has no obvious influence on the taste of cigarettes. It also has effects of softening smoke, reducing irritation, improving taste, and improving sensory quality of cigarette.
2. The dark plum extract is used for reducing the release amount of phenol in smoke for the first time. The dark plum extract is an extract obtained by extracting the rest water phase part of dark plum ethanol extract extracted by petroleum ether solvent and ethyl acetate with n-butanol and concentrating. The effect of reducing the release amount of phenol in the flue gas is obvious.
3. The composite additive has the advantages of simple preparation method, low cost and obvious harm reduction effect.
Detailed Description
The following description will be made clearly and fully with reference to the technical solutions in the embodiments, and it is apparent that the described embodiments are only examples of some of the present invention, not all of them. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without any inventive effort, are intended to be within the scope of the invention.
Example 1:
The composite additive of the embodiment comprises the following raw materials in parts by weight: 10 parts of dark plum extract and 90 parts of propylene glycol.
The preparation method of the dark plum refined extract comprises the following steps: removing impurities from dry mume fructus, pulverizing, adding 95v/v% ethanol, reflux extracting for 3 times, and concentrating under reduced pressure to obtain mume fructus ethanol extract. Dispersing the ethanol extract with water, adding petroleum ether solvent with volume 3 times of that of the sample, extracting for three times, and degreasing. Concentrating the petroleum ether extract to obtain petroleum ether extract. The aqueous phase part is extracted with ethyl acetate for three times, and the ethyl acetate extract is concentrated to obtain ethyl acetate extract. Extracting the rest water phase with n-butanol for three times, mixing the extractive solutions, and concentrating to obtain mume fructus extract.
In order to study the influence of different dark plum extracts on the release amount and the smoking quality of the phenol in the smoke, four dark plum extracts, namely dark plum ethanol extract, petroleum ether extract, ethyl acetate extract and dark plum refined extract, are respectively and uniformly sprayed into tobacco shreds according to 0.05 percent of the mass of the tobacco shreds, are baked, balance moisture and are coiled into cigarette cigarettes. The control sample was treated in the same manner as the experimental sample with ethanol added at 0.05% of the tobacco mass.
And analyzing the phenol release amount of the prepared cigarette according to a method specified in a high performance liquid chromatography for measuring main phenolic compounds in main stream smoke of the YC/T255-2008 cigarette. And carrying out sensory evaluation and smoking comparison on cigarette samples according to GB5606.4-2005 sensory technical requirements of cigarettes. The results are shown in Table 1.
TABLE 1 Effect of different dark plum extracts on the phenol Release amount and the suction quality of Smoke
From the results in table 1, it can be seen that: different dark plum extracts are used as additives and are uniformly added into tobacco shreds, so that the phenol release amount in the main stream smoke of cigarettes can be reduced, the tar of the cigarettes is not greatly influenced, the smoking quality of the cigarettes is not adversely influenced, and the reduction of phenol is 6.6% -24.1%. Especially dark plum extract, the reduction rate of phenol reaches 24.1 percent. Therefore, the dark plum extract is selected as the main component of the composite additive for reducing the release amount of phenol in cigarette smoke.
Example 2:
The composite additive for reducing the release amount of phenol in the flue gas comprises the following raw materials in parts by weight: 10 parts of dark plum extract, 10 parts of wild jujube seed and 80 parts of propylene glycol.
The dark plum extract was prepared as in example 1.
The preparation method of the semen zizyphi spinosae extract comprises the following steps: removing impurities from dried semen Ziziphi Spinosae, pulverizing, adding 95v/v% ethanol, reflux extracting for 3 times, and vacuum concentrating to obtain semen Ziziphi Spinosae extract.
Preparation of a composite additive for reducing the release amount of phenol in flue gas:
adding 10g of dark plum extract and 10g of wild jujube seed extract into 80g of propylene glycol, and stirring for 5-10min to obtain the required compound additive.
Uniformly spraying the composite additive into tobacco shreds according to the mass of 0.05% of the tobacco shreds, drying the tobacco shreds, balancing water content, and rolling into cigarette. The control sample was treated in the same manner as the experimental sample with ethanol added at 0.05% of the tobacco mass.
And analyzing the phenol release amount of the prepared cigarette sample according to a method prescribed by a high performance liquid chromatography for measuring main phenolic compounds in mainstream smoke of YC/T255-2008 cigarettes. And carrying out sensory evaluation and smoking comparison on the cigarette samples according to GB5606.4-2005 cigarette sensory technical requirements. The results are shown in tables 2 and 3. As can be seen from table 2, after the composite additive of this example is added, the phenol content of the cigarette smoke is reduced by 15.1%; and the smoke can be softened, the irritation is reduced, and the sensory quality of the cigarettes is improved.
Example 3
The preparation of the dark plum extract and the wild jujube seed extract is the same as that of the example 2.
Preparation of a composite additive for reducing the release amount of phenol in flue gas:
adding 20g of dark plum extract and 10g of wild jujube seed extract into 70g of propylene glycol, and stirring for 5-10min to obtain the required compound additive.
Uniformly spraying the composite additive into tobacco shreds according to the mass of 0.05% of the tobacco shreds, drying the tobacco shreds, balancing water content, and rolling into cigarette. The control sample was treated in the same manner as the experimental sample with ethanol added at 0.05% of the tobacco mass.
And analyzing the phenol release amount of the prepared cigarette sample according to a method prescribed by a high performance liquid chromatography for measuring main phenolic compounds in mainstream smoke of YC/T255-2008 cigarettes. And carrying out sensory evaluation and smoking comparison on the cigarette samples according to GB5606.4-2005 cigarette sensory technical requirements. The results are shown in tables 2 and 3. As can be seen from table 2, after the composite additive of this example is added, the phenol content of the cigarette smoke is reduced by 19.2%; and the smoke can be softened, the irritation is reduced, and the sensory quality of the cigarettes is improved.
Example 4:
the composite additive was the same as in example 4.
Uniformly spraying the composite additive into tobacco shreds according to the mass of 0.1% of the tobacco shreds, drying the tobacco shreds, balancing water content, and rolling into cigarette. The control sample is ethanol with the mass of 0.1% of the tobacco shred, and is treated in the same way as the experimental sample.
And analyzing the phenol release amount of the prepared cigarette sample according to a method prescribed by a high performance liquid chromatography for measuring main phenolic compounds in mainstream smoke of YC/T255-2008 cigarettes. And carrying out sensory evaluation and smoking comparison on the cigarette samples according to GB5606.4-2005 cigarette sensory technical requirements. The results are shown in tables 2 and 3. The results show that: after the composite additive of the embodiment is added, the phenol content of cigarette smoke is reduced by 21.6%; and has no obvious influence on the taste of cigarettes.
Example 5:
the preparation of the dark plum extract and the wild jujube seed extract is the same as that of the example 2.
Preparation of a composite additive for reducing the release amount of phenol in flue gas: adding 10g of dark plum extract and 5g of wild jujube seed extract into 85g of propylene glycol, and stirring for 5-10min to obtain the required compound additive.
Uniformly spraying the composite additive into tobacco shreds according to the mass of 0.05% of the tobacco shreds, drying the tobacco shreds, balancing water content, and rolling into cigarette. The control sample is ethanol with the mass of 0.05% of the tobacco shred, and is treated in the same way as the experimental sample.
And analyzing the phenol release amount of the prepared cigarette sample according to a method prescribed by a high performance liquid chromatography for measuring main phenolic compounds in mainstream smoke of YC/T255-2008 cigarettes. And carrying out sensory evaluation and smoking comparison on the cigarette samples according to GB5606.4-2005 cigarette sensory technical requirements. The results are shown in tables 2 and 3. The results show that: after the composite additive of the embodiment is added, the phenol content of cigarette smoke is reduced by 15.7%; and the smoke can be softened, the irritation is reduced, and the sensory quality of the cigarettes is improved.
TABLE 2 Effect of composite additives on the Release of phenol from flue gas
Sequence number Sample of Tar level (mg/cig) Phenol (ug/cig) Phenol reduction Rate (%)
1 Control cigarette 10.89 11.90 --
2 Example 1 10.90 9.03 24.1
3 Example 2 11.00 10.10 15.1
4 Example 3 10.89 9.61 19.2
5 Example 4 11.25 9.33 21.6
6 Example 5 10.93 10.03 15.7
TABLE 3 Effect of composite additives on smoking quality of cigarettes
From the above examples and the data in the table, it is clear that the dark plum extract in the composite additive can obviously reduce the phenol content of the cigarette smoke, but the addition amount is not as high as possible. The semen Ziziphi Spinosae extract is added to soften smoke, reduce irritation, and improve sensory quality of cigarette. The spine date seed extract can not reduce the phenol content of cigarette smoke.
The foregoing has shown and described the basic principles, principal features and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that the above embodiments and descriptions are merely illustrative of the principles of the present invention, and various changes and modifications may be made without departing from the spirit and scope of the invention, which is defined in the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.

Claims (1)

1. The application of the composite additive for reducing the release amount of phenol in the flue gas is characterized in that the composite additive comprises the following raw materials in parts by weight: 10 parts of dark plum extract, and supplementing 100 parts of the dark plum extract with propylene glycol; the composite additive is uniformly sprayed into tobacco shreds according to the mass of 0.05 of the tobacco shreds to prepare cigarettes; the dark plum refined extract is prepared by the following steps: removing impurities from dried mume fructus, pulverizing, adding 80-95v/v% ethanol, reflux extracting for 3 times, and concentrating under reduced pressure to obtain mume fructus ethanol extract; dispersing the obtained ethanol extract with water, adding petroleum ether solvent with volume 3 times of that of the sample, extracting for three times, and degreasing; concentrating the petroleum ether extract to obtain petroleum ether extract; extracting the water phase part with ethyl acetate for three times, and concentrating the ethyl acetate extract to obtain ethyl acetate extract; extracting the rest water phase part with n-butanol for three times, mixing the extractive solutions, and concentrating to obtain mume fructus extract.
CN202111476641.0A 2021-12-06 2021-12-06 Composite additive for reducing release amount of phenol in flue gas, and preparation method and application thereof Active CN113974213B (en)

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Citations (2)

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CN102499460A (en) * 2011-11-02 2012-06-20 深圳市大百汇技术有限公司 Extracting method for radix ophiopogonis extract and dark plum extract as well as cigarette containing radix ophiopogonis extract and dark plum extract
CN104489903A (en) * 2014-12-17 2015-04-08 贵州中烟工业有限责任公司 E-cigarette nicotine liquid with function of tranquilizing by nourishing the heart

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Publication number Priority date Publication date Assignee Title
US7581543B2 (en) * 2004-04-14 2009-09-01 Philip Morris Usa Inc. Reduction of phenolic compound precursors in tobacco
CN105038984A (en) * 2015-07-10 2015-11-11 湖北中烟工业有限责任公司 Acid-flavor essence for softening and smoothing smoke and reducing stimulation and application thereof
CN106551422A (en) * 2016-11-30 2017-04-05 湖北中烟工业有限责任公司 Preparation method and application of the cigarette with Semen Ziziphi Spinosae extractum

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102499460A (en) * 2011-11-02 2012-06-20 深圳市大百汇技术有限公司 Extracting method for radix ophiopogonis extract and dark plum extract as well as cigarette containing radix ophiopogonis extract and dark plum extract
CN104489903A (en) * 2014-12-17 2015-04-08 贵州中烟工业有限责任公司 E-cigarette nicotine liquid with function of tranquilizing by nourishing the heart

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乌梅浸膏成分分析及在卷烟中的应用;徐石磊;《广西烟草学会2014年学术年会论文集—技术创新篇》;第62页右栏最后一段和第63页左栏第1段以及第64页右栏最后一段 *

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