CN114532587A - Modified Al with controllable slow release performance2O3Preparation method and application of perfume composite material - Google Patents
Modified Al with controllable slow release performance2O3Preparation method and application of perfume composite material Download PDFInfo
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- CN114532587A CN114532587A CN202210033438.4A CN202210033438A CN114532587A CN 114532587 A CN114532587 A CN 114532587A CN 202210033438 A CN202210033438 A CN 202210033438A CN 114532587 A CN114532587 A CN 114532587A
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- composite material
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24D—CIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
- A24D3/00—Tobacco smoke filters, e.g. filter-tips, filtering inserts; Filters specially adapted for simulated smoking devices; Mouthpieces for cigars or cigarettes
- A24D3/02—Manufacture of tobacco smoke filters
- A24D3/0204—Preliminary operations before the filter rod forming process, e.g. crimping, blooming
- A24D3/0212—Applying additives to filter materials
- A24D3/0225—Applying additives to filter materials with solid additives, e.g. incorporation of a granular product
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24D—CIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
- A24D3/00—Tobacco smoke filters, e.g. filter-tips, filtering inserts; Filters specially adapted for simulated smoking devices; Mouthpieces for cigars or cigarettes
- A24D3/04—Tobacco smoke filters characterised by their shape or structure
- A24D3/048—Tobacco smoke filters characterised by their shape or structure containing additives
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- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24D—CIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
- A24D3/00—Tobacco smoke filters, e.g. filter-tips, filtering inserts; Filters specially adapted for simulated smoking devices; Mouthpieces for cigars or cigarettes
- A24D3/06—Use of materials for tobacco smoke filters
- A24D3/061—Use of materials for tobacco smoke filters containing additives entrapped within capsules, sponge-like material or the like, for further release upon smoking
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Fats And Perfumes (AREA)
- Cigarettes, Filters, And Manufacturing Of Filters (AREA)
Abstract
The invention discloses modified Al with adjustable and controllable slow release performance2O3Flavor composite material, application of flavor composite material in tobacco and Al prepared by flavor composite material2O3The modified material takes tobacco stems with low utilization value in tobacco raw materials as a bottom plate, and the modified material is mixed with Al2O3The preparation of the modified material is combined, and the application of the tobacco stems is greatly widened. The invention firstly thinks of controlling the release rate of the spice in the adsorption material/spice composite material by controlling the temperature, and furthermore, the invention finds the adsorption material which has the advantages of excellent spice storage capacity and controllable slow release performance. Modified Al prepared by the invention2O3Perfume composite material applied to cigarettes and capable of effectively improving smoking of cigarettesThe quality, the aroma characteristic, the smoke characteristic and the taste characteristic of the cigarette are obviously improved.
Description
Technical Field
The invention belongs to the field of application of tobacco industry, and particularly relates to modified Al with adjustable and controllable slow release performance2O3Preparation method of/spice composite material and application in tobacco.
Background
The target is slowly and controllably released by adopting a certain method to treat the target or depending on certain special properties of a matrix material, so that the sustained-release technology is a sustained-release technology which is applied more in the field of medicines at present, and the sustained-release technology is also applied in the field of essence and flavor along with the development and the increase of the demand of the technology. In the field of cigarette manufacturing, the aroma of cigarettes and the release of aroma in the smoking process are important factors for evaluating the quality of the cigarettes, in order to improve the smoking quality of the cigarettes and highlight the style characteristics of the cigarettes, the perfuming technology is undoubtedly a hot point of research, and a perfume substance is adsorbed on certain specific adsorbing materials and applied to the cigarette manufacturing process so as to fulfill the aims of storing and slowly releasing the perfume, ensuring the quality of the perfume and fully utilizing the perfume, wherein the conventional perfuming adsorbents comprise zeolite molecular sieves, activated carbon, aluminosilicate and the like.
At present, researchers pay attention to the slow release effect, the slower the release rate is, the better the release rate is, the adsorption material with the controllable release rate is not improved, but in the practical application process, the most hopeful is that in the storage and transportation process, the release rate is low, the perfume is hardly released, but in the normal suction process, the release rate is improved to a certain extent. The research on the adsorption material which has excellent fragrance storage capacity and controllable slow release performance is very difficult, and on one hand, the adsorption effect on the fragrance is influenced by the properties of fragrance molecules, and factors such as the diameter of the fragrance molecules, the average pore diameter of the adsorption material, the total content of acid groups on the surface of the adsorption material and the like.
Therefore, the method for preparing the adsorption material/spice composite material with adjustable and controllable slow release performance is explored, so that the essence composite material prepared by the method is applied to cigarette perfuming, and the improvement of the sensory quality of the cigarette is very important.
The present invention has been made to solve the above problems.
Disclosure of Invention
The invention provides modified Al with controllable slow release performance2O3A method for preparing a perfume composite, comprising the steps of:
(1) adopting HCL to soak tobacco stems, and after soaking, carrying out gradient dehydration by using absolute ethyl alcohol to obtain the treated tobacco stems;
(2) weighing aluminum nitrate hydrate, dissolving the aluminum nitrate hydrate in deionized water, heating and stirring the mixture until the solution is in a transparent state, then dropwise adding ammonia water, continuously stirring the mixture, stopping titration when the pH value reaches 8.5, and simultaneously continuing stirring the mixture to obtain a first mixture;
(3) soaking the treated tobacco stems obtained in the step (1) in the first mixture obtained in the step (2), filtering, taking out precipitates, drying and calcining to obtain Al2O3A modifying material;
(4) weighing spices, and adding the Al obtained in the step (3)2O3The modified material is stirred and centrifuged to obtain solid, and the solid is dried to obtain modified Al2O3A perfume composite.
Preferably, in step (1), the mass fraction of HCL is 5-7%.
Preferably, in the step (2), the aluminum nitrate hydrate is dissolved in deionized water, the mass percent of the aluminum nitrate hydrate is 37.5%, the concentration of ammonia water is 2moL/L, and the stirring is continued for 2-3 h.
Preferably, in the step (3), the soaking is carried out for 48-72h, and the drying process is as follows: naturally drying the precipitate at room temperature, and further drying in an oven at 90-95 ℃ for 24-36h at 500-650 ℃ for 2-3 h.
Preferably, in step (4), 0.3-0.5% of the perfume is weighed, and 80-150g of Al is added2O3And (3) modifying the material, stirring for 4-5h, and centrifuging, wherein the drying process comprises the following steps: and naturally drying at room temperature.
In a second aspect the present invention provides a method of manufacturing a semiconductor deviceMethod for modulating flavor release rate, according to the method of any one of claims 1 to 5, by modifying flavor to Al2O3Perfume composite material, then by controlling temperature, control modified Al2O3The release rate of the perfume in the perfume composite.
Preferably, the temperature is controlled to be less than or equal to 15 ℃, the release rate of the perfume is low, the temperature is controlled to be more than 15 ℃, and the release rate of the perfume is high.
The third aspect of the invention provides modified Al with adjustable and controllable slow release performance, which is prepared by the preparation method2O3The application of the/spice composite material in tobacco is characterized in that 0.5-0.8 percent of modified Al is added according to mass percentage2O3The perfume composite material is added into the cigarette filter stick.
Preferably, the modified Al is controlled by controlling the temperature2O3The release rate of the perfume in the perfume composite; specifically, in the process of storage and transportation, the temperature is ensured to be less than or equal to 15 ℃, the release rate of the perfume is low, and in the process of pumping, the temperature is greater than 15 ℃, and the release rate of the perfume is high.
The measurement method related to the present invention is as follows:
1、Al2O3method for measuring perfume loading (adsorption rate) of modified material:
extracting modified Al with anhydrous ethanol2O3Performing ultrasonic treatment for 30min, centrifuging for 5 times at 4000r/min for 10min each time, collecting extractive solution, diluting with anhydrous ethanol to 25mL, detecting peak area of perfume corresponding to concentration by high performance liquid chromatography, calculating perfume concentration by standard curve, and calculating loading capacity (adsorption rate).
2. Al at different temperatures and times2O3Method for measuring perfume loading (adsorption rate) of modified material:
5 parts of modified Al2O3The composite material of perfume is placed in thermostats of 15 deg.C, 30 deg.C, 50 deg.C, 70 deg.C and 90 deg.C respectively, and left open. Washing the composite material every 1h by high performance liquid chromatographyThe concentration of the stripped perfume solution and the loading (adsorption rate) were calculated.
3. Sensory evaluation was carried out by the following method:
mainly considers three aspects of aroma, smoke and taste characteristics, including 10 indexes of aroma quality, aroma quantity, miscellaneous gas, concentration, strength, fineness, irritation, dry feeling, cleanness degree and sweet return; the scoring values of the 10 quality detection indexes are respectively as follows: 0-10 minutes of fragrance quality, 0-10 minutes of fragrance amount, 0-10 minutes of miscellaneous gas, 0-10 minutes of concentration, 0-10 minutes of strength, 0-10 minutes of fineness, 0-10 minutes of irritation, 0-10 minutes of dry feeling, 0-10 minutes of cleanness degree and 0-10 minutes of rewweet.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention firstly thinks that the release rate of the spice in the adsorption material/spice composite material is controlled by controlling the temperature, thereby realizing that the temperature is lower and the spice is slowly released in the process of storage and transportation, and the spice is released to a certain extent but still is slowly released when really sucking. Furthermore, the invention finds the adsorbing material which has the advantages of excellent fragrance storage capacity, and controllable slow release performance.
2. Al prepared by the invention2O3The method for modifying the material is simple and easy to popularize and apply, and simultaneously, the tobacco stalks with lower utilization value in the tobacco raw materials are used as the bottom plate and are mixed with Al2O3The preparation of the modified material is combined, and the application of the tobacco stems is greatly widened.
3. Modified Al prepared by the invention2O3The loading capacity (adsorption rate) of the perfume composite material to the perfume is more than 98 percent, and the perfume composite material has strong perfume storage capacity.
4. Modified Al prepared by the invention2O3The composite material of the perfume can slowly release 30% of the perfume after being exposed in the air for two days at the temperature of 15 ℃, and then can show stronger fragrance-holding performance. When the temperature is between 30 ℃ and 90 ℃, the composite material shows strong slow release performance, the loading capacity (adsorption rate) of the composite material can be reduced by about 89% at most after one week, and the method is provided for regulating and controlling the slow release performance of the spiceProvides an effective means, can realize the regulation and control of the release of the perfume by regulating the temperature in practice, and provides possibility for the regulation and control of the slow release of the perfume.
5. Modified Al prepared by the invention2O3The composite material of the spice can be applied to cigarettes, the smoking quality of the cigarettes can be effectively improved, and the aroma characteristic, the smoke characteristic and the taste characteristic of the cigarettes are obviously improved.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The experimental methods not specified in the examples are generally commercially available according to the conventional conditions and the conditions described in the manual, or according to the general-purpose equipment, materials, reagents and the like used under the conditions recommended by the manufacturer, unless otherwise specified. The starting materials required in the following examples and comparative examples are all commercially available.
Example 1
(1) The tobacco stems were soaked with 6% HCL.
(2) And (3) carrying out gradient dehydration on the (1) by using absolute ethyl alcohol.
(3) 37.5% of aluminum nitrate hydrate was weighed and dissolved in deionized water, and the solution was heated and stirred until it became transparent.
(4) Titrating the solution (3) by using 2moL/L ammonia water, continuously stirring, stopping titrating when the pH value reaches 8.5, and simultaneously continuing stirring for 2 hours.
(5) And (3) soaking the (2) in the (4) for 50 h.
(6) And (5) filtering, and taking the precipitate to be naturally dried at room temperature.
(7) And (3) further drying the dried (6) in an oven at 90 ℃ for 30 h.
(8) And (7) placing the dried (7) in a muffle furnace for calcining at the temperature of 550 ℃.
(9) Calcining to obtain Al2O3And (3) modifying the material.
(10) 0 is weighed out.4% ethyl maltol, 100gAl2O3The modified material is placed on a magnetic stirrer to be stirred for 4 hours, and then is centrifuged to obtain a solid, and the solid is naturally dried at room temperature to obtain modified Al2O3Ethyl maltol composite material.
(11) 0.6% of (10) was added to the cigarette filter.
Determination of modified Al2O3The results of the loading (adsorption rate) of the flavor by the ethyl maltol composite material are shown in Table 1, and Al is measured at different temperatures and times2O3The results of the loading (adsorption rate) of the flavor by the ethyl maltol composite material are shown in Table 2 for Al addition2O3The results of the smoking evaluation of the cigarettes made of the ethyl maltol composite material are shown in Table 3.
Example 2
Preparation of TiO by the method of example 12The material was modified, and the remaining steps were the same as in example 1.
Determination of modified TiO2The results for the ethyl maltol composite versus perfume loading are shown in table 1.
Example 3
Preparation of SiO by the method of example 12The material was modified, and the remaining steps were the same as in example 1.
Determination of modified SiO2The/ethyl maltol composite had a loading of perfume as shown in table 1.
Example 4
The methods of (11) and (12) in example 1 were employed, except that unmodified Al was directly used2O3Compounding with ethyl maltol.
Comparative example
Equal amount of ethyl maltol was directly added to the cigarette filter and the sample was evaluated for smoking, the results are shown in table 3.
TABLE 1 comparison of adsorption para-ethyl maltol loadings for different materials
| Serial number | Material | Loading (adsorption)/% |
| Example 1 | Modified Al2O3 | 98.9％ |
| Example 2 | Modified TiO2 | 50.8％ |
| Example 3 | Modified SiO2 | 54.9％ |
| Example 4 | Unmodified Al2O3 | 18.4％ |
TABLE 2 Al at different temperatures and times2O3Change in flavor loading (%)/Ethyl maltol composite Material
TABLE 3 sensory evaluation results of cigarettes
As can be seen from Table 1, the modified Al prepared by the present invention2O3The loading capacity (adsorption rate) of the ethyl maltol of the composite material/ethyl maltol is more than 98 percent, which shows that the composite material prepared by the invention has stronger fragrance storage capacity. In addition, it can be seen by comparing example 1 and example 4 that the modification is for Al2O3The increase of the loading capacity (adsorption rate) is important, and the loading capacity (adsorption rate) is directly increased from 18.4 percent of unmodified to 98.9 percent of modified loading capacity.
As can be seen from Table 2, the modified Al prepared by the present invention2O3The composite material of ethyl maltol can slowly release 30% of perfume after being exposed in the air for two days at the temperature of 15 ℃, and then can show stronger fragrance-holding performance. When the temperature is between 30 ℃ and 90 ℃, the composite material shows strong slow release performance, the loading capacity can be reduced by about 89% at most after one week, an effective means is provided for the regulation and control of the slow release performance of the perfume, and the regulation and control of the perfume release can be realized by regulating the temperature in practice.
As can be seen from Table 3, the modified Al prepared by the present invention2O3The ethyl maltol composite material is applied to cigarettes, so that the smoking quality of the cigarettes is effectively improved, and the aroma characteristic, the smoke characteristic and the taste characteristic of the cigarettes are obviously improved.
Claims (9)
1. Modified Al with controllable slow release performance2O3A preparation method of the perfume composite material is characterized by comprising the following steps:
(1) soaking tobacco stems by using HCL, and performing gradient dehydration by using absolute ethyl alcohol after soaking to obtain the treated tobacco stems;
(2) weighing aluminum nitrate hydrate, dissolving the aluminum nitrate hydrate in deionized water, heating and stirring the solution until the solution is in a transparent state, then dropwise adding ammonia water, continuously stirring the solution, stopping titration when the pH value reaches 8.5, and meanwhile continuously stirring the solution to obtain a first mixture;
(3) soaking the treated tobacco stems obtained in the step (1) in the first mixture obtained in the step (2), filtering, taking out precipitates, drying and calcining to obtain Al2O3A modifying material;
(4) weighing spices, and adding the Al obtained in the step (3)2O3The modified material is stirred and centrifuged to obtain solid, and the solid is dried to obtain modified Al2O3A perfume composite.
2. The production method according to claim 1, wherein in the step (1), the mass fraction of HCL is 5 to 7%.
3. The preparation method of claim 1, wherein in the step (2), the aluminum nitrate hydrate is dissolved in deionized water, the mass percent of the aluminum nitrate hydrate is 37.5%, the concentration of ammonia water is 2moL/L, and the stirring is continued for 2-3 h.
4. The preparation method according to claim 1, wherein in the step (3), the soaking is carried out for 48-72h, and the drying process comprises the following steps: naturally drying the precipitate at room temperature, and further drying in an oven at 90-95 ℃ for 24-36h at the calcination temperature of 500-650 ℃ for 2-3 h.
5. The method according to claim 1, wherein in the step (4), 0.3-0.5% of the flavor is weighed and 80-150g of Al is added2O3And (3) modifying the material, stirring for 4-5h, and centrifuging, wherein the drying process comprises the following steps: naturally drying at room temperature.
6. A method for adjusting the release rate of a flavor, wherein the flavor is made into modified Al according to the method of any one of claims 1 to 52O3Perfume composite material, then by controlling temperature, control modified Al2O3The release rate of the perfume in the perfume composite.
7. The method of claim 6, wherein the temperature is controlled to 15 ℃ or less and the release rate of the flavorant is low, and wherein the temperature is controlled to greater than 15 ℃ and the release rate of the flavorant is high.
8. Modified Al with controllable slow-release performance prepared by the preparation method of any one of claims 1-52O3The application of the/perfume composite material is characterized in that 0.5-0.8 percent of modified Al is added according to the mass percentage2O3The perfume composite material is added into the cigarette filter stick.
9. Use according to claim 8, wherein the modified Al is controlled by controlling the temperature2O3The release rate of the perfume in the perfume composite; specifically, the temperature is ensured to be less than or equal to 15 ℃ in the storage and transportation process, the release rate of the spice is low, and the temperature is ensured to be greater than 15 ℃ in the pumping process, and the release rate of the spice is high.
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| CN202210033438.4A CN114532587B (en) | 2022-01-12 | 2022-01-12 | Modified Al with controllable slow release performance 2 O 3 Preparation method and application of perfume composite material |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20120039981A1 (en) * | 2009-04-24 | 2012-02-16 | Pedersen Kurt Moeller | Chewing Gum And Particulate Material For Controlled Release Of Active Ingredients |
| WO2019201290A1 (en) * | 2018-04-19 | 2019-10-24 | 云南巴菰生物科技有限公司 | Method for preparing low-suction-resistance polylactic acid tow filter rod used for reducing temperature of cigarette vapor |
| CN112790425A (en) * | 2019-11-13 | 2021-05-14 | 湖南中烟工业有限责任公司 | Aroma slow-release layered material, preparation thereof and application thereof in heating non-combustible tobacco products |
-
2022
- 2022-01-12 CN CN202210033438.4A patent/CN114532587B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20120039981A1 (en) * | 2009-04-24 | 2012-02-16 | Pedersen Kurt Moeller | Chewing Gum And Particulate Material For Controlled Release Of Active Ingredients |
| WO2019201290A1 (en) * | 2018-04-19 | 2019-10-24 | 云南巴菰生物科技有限公司 | Method for preparing low-suction-resistance polylactic acid tow filter rod used for reducing temperature of cigarette vapor |
| CN112790425A (en) * | 2019-11-13 | 2021-05-14 | 湖南中烟工业有限责任公司 | Aroma slow-release layered material, preparation thereof and application thereof in heating non-combustible tobacco products |
Non-Patent Citations (1)
| Title |
|---|
| 王猛;杨乾栩;杨莹;陈微;朱保昆;: "复合香料植物颗粒的制备及在卷烟中的应用", 精细化工, vol. 33, no. 03, pages 326 - 332 * |
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