CN114532587B - Modified Al with controllable slow release performance 2 O 3 Preparation method and application of perfume composite material - Google Patents
Modified Al with controllable slow release performance 2 O 3 Preparation method and application of perfume composite material Download PDFInfo
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- CN114532587B CN114532587B CN202210033438.4A CN202210033438A CN114532587B CN 114532587 B CN114532587 B CN 114532587B CN 202210033438 A CN202210033438 A CN 202210033438A CN 114532587 B CN114532587 B CN 114532587B
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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 a modified Al with adjustable slow release performance 2 O 3 Perfume composite material and application thereof in tobacco, al prepared by the invention 2 O 3 The modified material takes tobacco stems with lower utilization value in tobacco raw materials as a bottom plate, and the tobacco stems are mixed with Al 2 O 3 The preparation of the modified material is combined, so that the application of the tobacco stems is greatly widened. The invention firstly thinks that the release rate of the perfume in the adsorption material/perfume composite material is controlled by controlling the temperature, and further, the invention finds the adsorption material with excellent perfume storage capacity and controllable slow release performance. Modified Al prepared by the invention 2 O 3 The composite material of the perfume can be applied to cigarettes, so that the smoking quality of the cigarettes can be effectively improved, and the fragrance characteristic, the smoke characteristic and the taste characteristic of the cigarettes are obviously improved.
Description
Technical Field
The invention belongs to the field of tobacco industry application, and in particular relates to a modified Al with adjustable slow release performance 2 O 3 Preparation method of perfume composite material and its application in tobacco.
Background
The target is treated by a certain method or is released slowly and controllably by depending on certain special properties of matrix materials, so that the method is a slow and controlled release technology which is widely applied in the field of medicines at present, and the slow and controlled release technology is also applied in the field of essence and perfume along with the development of technology and the increase of requirements. In the field of cigarette manufacturing, the fragrance of cigarettes and the release of fragrance in the smoking process are important factors for evaluating the quality of cigarettes, in order to improve the smoking quality of cigarettes and highlight the style characteristics of cigarettes, the flavoring technology undoubtedly becomes a research hot spot, and the flavoring adsorbent is applied to the cigarette manufacturing process by adsorbing spice substances on specific adsorption materials so as to achieve the purposes of storing slow-release spice, ensuring the quality of the spice and fully utilizing the spice.
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 controllable release rate is not improved, but in the practical application process, the most hope is that the release rate is low in the storage and transportation process, the perfume is hardly released, and the release rate is improved to a certain extent in the normal suction process. The adsorption material with excellent fragrance storage capacity and controllable slow release performance is difficult to study, and on one hand, the adsorption effect on the fragrance is influenced by the characteristics of the 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, a preparation method of the adsorption material/spice composite material with controllable slow release performance is explored, so that the essence composite material prepared by the preparation method is applied to cigarette flavoring, and the improvement of the sensory quality of cigarettes is important.
The present invention has been made to solve the above problems.
Disclosure of Invention
The first aspect of the invention provides a modified Al with controllable slow release performance 2 O 3 A process for the preparation of a fragrance composite comprising the steps of:
(1) Soaking tobacco stems by adopting HCL, and carrying out gradient dehydration on the soaked tobacco stems by using absolute ethyl alcohol to obtain treated tobacco stems;
(2) Weighing aluminum nitrate hydrate, dissolving the aluminum nitrate hydrate in deionized water, heating and stirring the aluminum nitrate hydrate to a transparent state solution, then dropwise adding ammonia water, continuously stirring the aluminum nitrate solution, stopping titration when the pH value reaches 8.5, and continuously stirring the aluminum nitrate 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, drying the precipitate, and calcining to obtain Al 2 O 3 A modified material;
(4) Weighing perfume, adding Al obtained in the step (3) 2 O 3 Stirring the modified material, centrifuging to obtain a solid, and drying to obtain modified Al 2 O 3 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 percentage of the aluminum nitrate hydrate is 37.5%, the concentration of ammonia water is 2moL/L, and stirring is continued for 2-3h.
Preferably, in the step (3), soaking is carried out for 48-72 hours, and the drying process is as follows: and (3) naturally drying the precipitate at room temperature, and then placing the precipitate in a baking oven at 90-95 ℃ for further drying for 24-36h, wherein the calcining temperature is 500-650 ℃ and the calcining time is 2-3h.
Preferably, in step (4), 0.3-0.5% of perfume is weighed and 80-150g of Al is added 2 O 3 The modified material is stirred for 4-5h and centrifuged, and the drying process is as follows: naturally drying at room temperature.
In a second aspect the present invention provides a method of modulating the rate of release of a perfume, the perfume being formulated as a modified Al according to the method of preparation as claimed in any one of claims 1 to 5 2 O 3 Perfume composite material and then modified Al by controlling the temperature 2 O 3 Rate of perfume release in perfume composite.
Preferably, the control temperature is less than or equal to 15 ℃, the release rate of the perfume is low, the control temperature is more than 15 ℃, and the release rate of the perfume is high.
The third aspect of the invention provides a modified Al with adjustable slow release performance, which is prepared by the preparation method 2 O 3 Use of a flavor composite in tobacco, based on mass percent, of 0.5-0.8% modified Al 2 O 3 The flavor composite is added to a cigarette filter rod.
Preferably, the modified Al is controlled by controlling the temperature 2 O 3 Rate of release of fragrance in the fragrance composite; in particular, during storage and transportation, the temperature is ensured to be less than or equal to 15 ℃, the release rate of the spice is low, and during the sucking process, the temperature is more than 15 DEG CThe release rate of the perfume is high at the temperature.
The measurement method of the invention comprises the following steps:
1、Al 2 O 3 method for measuring perfume loading (adsorption rate) of modified material:
extracting modified Al with absolute ethanol 2 O 3 The composite material of the perfume is subjected to ultrasonic treatment for 30min, and is centrifuged for 5 times by using a 4000r/min centrifuge for 10min each time, an extracting solution is collected, the extracting solution is diluted to 25mL by using absolute ethyl alcohol, the peak area of the corresponding concentration of the perfume is detected by using a high performance liquid chromatography, the perfume concentration is calculated by using a standard curve, and the loading capacity (adsorption rate) is calculated.
2. Al at different temperatures and times 2 O 3 Method for measuring perfume loading (adsorption rate) of modified material:
5 parts of modified Al 2 O 3 The perfume composite material is placed in a thermostat at 15 deg.C, 30 deg.C, 50 deg.C, 70 deg.C and 90 deg.C respectively, and left open. Every 1 hour, the concentration of the perfume solution eluted from the composite material was detected by high performance liquid chromatography, and the load (adsorption rate) was calculated.
3. Sensory evaluation was performed using the following method:
the three aspects of aroma, smoke and taste characteristics are mainly inspected, and the three aspects comprise 10 indexes of aroma quality, aroma quantity, miscellaneous gas, concentration, strength, fineness, irritation, dryness, cleanliness and sweet returning; scoring values of the 10 quality detection indexes are respectively as follows: 0-10 parts of aroma quality, 0-10 parts of aroma quantity, 0-10 parts of miscellaneous gas, 0-10 parts of concentration, 0-10 parts of strength, 0-10 parts of fineness, 0-10 parts of irritation, 0-10 parts of dryness, 0-10 parts of cleanliness and 0-10 parts of sweet returning.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention firstly thinks that the release rate of the perfume in the adsorption material/perfume composite material is controlled by controlling the temperature, so that the lower temperature in the storage and transportation process and the slow release of the perfume are realized, and the perfume release is improved to a certain extent but still is the slow release degree when the perfume is truly sucked. Furthermore, the invention finds the adsorption material with excellent fragrance storage capacity and controllable slow release performance.
2. Al prepared by the invention 2 O 3 The method for modifying the material is simple and easy to popularize and apply, and simultaneously, the tobacco stems with lower utilization value in the tobacco raw materials are used as the bottom plate, and the tobacco stems are mixed with Al 2 O 3 The preparation of the modified material is combined, so that the application of the tobacco stems is greatly widened.
3. Modified Al prepared by the invention 2 O 3 The perfume composite material has high perfume loading capacity (adsorption rate) up to 98% or more and high perfume storing capacity.
4. Modified Al prepared by the invention 2 O 3 The composite material of the perfume can slowly release the perfume for 30% after being exposed to air for two days at the temperature of 15 ℃, and can show stronger perfume-retaining performance. The composite material has strong slow release performance at 30-90 ℃, and the loading capacity (adsorption rate) of the composite material can be reduced by about 89% at the highest after one week, so that an effective means is provided for regulating and controlling the slow release performance of the perfume, the regulation and control of the perfume release can be realized by regulating the temperature in practice, and the possibility is provided for regulating and controlling the slow release of the perfume.
5. Modified Al prepared by the invention 2 O 3 The composite material of the perfume can be applied to cigarettes, so that the smoking quality of the cigarettes can be effectively improved, and the fragrance characteristic, the smoke characteristic and the taste characteristic of the cigarettes are obviously improved.
Detailed Description
The present invention will be described in further detail with reference to the following examples in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
Experimental methods, in which specific conditions are not specified in examples, are generally available commercially according to conventional conditions as well as those described in handbooks, or according to general-purpose equipment, materials, reagents, etc. used under conditions suggested by manufacturers, unless otherwise specified. The raw materials required in the following examples and comparative examples are all commercially available.
Example 1
(1) Tobacco stems were soaked with 6% HCL.
(2) And (3) carrying out gradient dehydration on the product (1) by using absolute ethyl alcohol.
(3) 37.5% aluminum nitrate hydrate was weighed into deionized water and heated to stir to a clear state solution.
(4) Titration was performed on (3) with 2moL/L ammonia water, and stirring was continued until the pH reached 8.5, and the titration was stopped while stirring was continued for 2 hours.
(5) And (3) placing the step (2) in the step (4) for soaking for 50h.
(6) Filtering the solution (5), and naturally drying the precipitate at room temperature.
(7) And (5) placing the dried (6) in a 90 ℃ oven for further drying for 30 hours.
(8) And (3) placing the dried (7) in a muffle furnace for calcination, wherein the calcination temperature is 550 ℃.
(9) Calcining to obtain Al 2 O 3 And (3) modifying the material.
(10) 0.4% ethyl maltol was weighed and 100g Al was added 2 O 3 Placing the modified material on a magnetic stirrer, stirring for 4h, centrifuging to obtain solid, and naturally drying at room temperature to obtain modified Al 2 O 3 Ethyl maltol composite.
(11) 0.6% of (10) was added to a cigarette filter rod.
Determination of modified Al 2 O 3 The loading (adsorption rate) of ethyl maltol composite material to perfume is shown in Table 1, and Al is measured at different temperatures and times 2 O 3 The loading (adsorption rate) of the ethyl maltol composite material to the perfume was shown in Table 2, and the results were shown for the added Al 2 O 3 Cigarette smoking evaluation was performed on ethyl maltol composite material, and the results are shown in Table 3.
Example 2
Preparation of TiO by the method of example 1 2 The materials were modified and the rest was the same as in example 1.
Determination of modified TiO 2 The perfume loading of the ethyl maltol composite is shown in Table 1.
Example 3
Preparation of SiO by the method of example 1 2 The materials were modified and the rest was the same as in example 1.
Determination of modified SiO 2 The perfume loading of the ethyl maltol composite is shown in Table 1.
Example 4
The methods (11) and (12) in example 1 were employed, except that unmodified Al was directly used 2 O 3 Compounding with ethyl maltol.
Comparative example
Equal amounts of ethyl maltol were directly added to the cigarette filter rod and the samples were evaluated for smoking, the results are shown in table 3.
Table 1 comparison of the adsorption of para-ethyl maltol loading by different materials
| Sequence number | Material | Load (adsorption rate)/% |
| Example 1 | Modified Al 2 O 3 | 98.9％ |
| Example 2 | Modified TiO 2 | 50.8％ |
| Example 3 | Modified SiO 2 | 54.9％ |
| Example 4 | Unmodified Al 2 O 3 | 18.4％ |
TABLE 2 Al at different temperatures and times 2 O 3 Variation of fragrance loading (adsorption Rate) of ethyl maltol composite (%)
Table 3 sensory evaluation results of cigarettes
As can be seen from Table 1, the modified Al prepared by the present invention 2 O 3 The loading capacity (adsorption rate) of the ethyl maltol of the composite material of the ethyl maltol is up to more than 98%, which shows that the composite material prepared by the invention has stronger fragrance storage capacity. In addition, as can be seen from comparative examples 1 and 4, the modification was made to Al 2 O 3 The improvement of the loading capacity (adsorption rate) is important, and the loading capacity (adsorption rate) is directly improved to 98.9% after modification from unmodified 18.4%.
As can be seen from Table 2, the modified Al prepared by the present invention 2 O 3 The composite material of ethyl maltol can release perfume 30% after being exposed to air for two days at 15 ℃, and can show stronger fragrance-holding performance. The composite material has strong slow release performance at 30-90 ℃, and the loading capacity of the composite material can be reduced by about 89% at most after one week, thus providing an effective means for regulating and controlling the slow release performance of the perfume, and in practice, the perfume can be regulated by regulatingThe temperature is saved to realize the regulation and control of the perfume release.
As can be seen from Table 3, the modified Al prepared by the present invention 2 O 3 The 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 performance 2 O 3 A process for the preparation of a fragrance composite, characterized in that it comprises the following steps:
(1) Soaking tobacco stems by adopting HCL, and carrying out gradient dehydration on the soaked tobacco stems by using absolute ethyl alcohol to obtain treated tobacco stems;
(2) Weighing aluminum nitrate hydrate, dissolving the aluminum nitrate hydrate in deionized water, heating and stirring the aluminum nitrate hydrate to a transparent state solution, then dropwise adding ammonia water, continuously stirring the aluminum nitrate solution, stopping titration when the pH value reaches 8.5, and continuously stirring the aluminum nitrate 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, drying the precipitate, and calcining to obtain Al 2 O 3 A modified material;
(4) Weighing perfume, adding Al obtained in the step (3) 2 O 3 Stirring the modified material, centrifuging to obtain a solid, and drying to obtain modified Al 2 O 3 Perfume composite.
2. The method according to claim 1, wherein in the step (1), the mass fraction of HCL is 5 to 7%.
3. The method according to claim 1, wherein in the step (2), the aqueous aluminum nitrate hydrate is dissolved in deionized water at a mass percentage of 37.5%, the concentration of the aqueous ammonia is 2moL/L, and stirring is continued for 2 to 3 hours.
4. The method according to claim 1, wherein in the step (3), the soaking is performed for 48 to 72 hours, and the drying process is as follows: and (3) naturally drying the precipitate at room temperature, and then placing the precipitate in a baking oven at 90-95 ℃ for further drying for 24-36h, wherein the calcining temperature is 500-650 ℃ and the calcining time is 2-3h.
5. The process according to claim 1, wherein in step (4), 0.3 to 0.5% of the perfume is weighed and 80 to 150g of Al is added 2 O 3 The modified material is stirred for 4-5h and centrifuged, and the drying process is as follows: naturally drying at room temperature.
6. A method for regulating the release rate of a perfume, characterized in that the perfume is prepared into a modified Al according to the preparation method as claimed in any one of claims 1 to 5 2 O 3 Perfume composite material and then modified Al by controlling the temperature 2 O 3 Rate of perfume release in perfume composite.
7. The method of claim 6, wherein the temperature is controlled to 15 ℃ or less, the rate of release of the fragrance is low, the temperature is controlled to more than 15 ℃, and the rate of release of the fragrance is high.
8. Modified Al with adjustable slow release performance prepared by the preparation method of any one of claims 1-5 2 O 3 Use of a perfume composite material, characterized in that 0.5-0.8% of modified Al is added on a mass percentage basis 2 O 3 The flavor composite is added to a cigarette filter rod.
9. The use according to claim 8, wherein the modified Al is controlled by controlling the temperature 2 O 3 Rate of release of fragrance in the fragrance composite; in the process of storage and transportation, the temperature is guaranteed to be less than or equal to 15 ℃, the release rate of the perfume is low, and in the process of sucking, the temperature is higher than 15 ℃, and the release rate of the perfume 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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| 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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| RU2530655C2 (en) * | 2009-04-24 | 2014-10-10 | Омиа Интернэшнл Аг | Meterial in form of particles for controlled release of active ingredients |
| CN108523216B (en) * | 2018-04-19 | 2020-08-25 | 云南巴菰生物科技有限公司 | Preparation method of polylactic acid tow filter stick for reducing smoke temperature and reducing suction resistance |
| 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 |
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