CN112931934A - Fragrance-holding and cooling additive and preparation method and application thereof - Google Patents
Fragrance-holding and cooling additive and preparation method and application thereof Download PDFInfo
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- CN112931934A CN112931934A CN202110314315.3A CN202110314315A CN112931934A CN 112931934 A CN112931934 A CN 112931934A CN 202110314315 A CN202110314315 A CN 202110314315A CN 112931934 A CN112931934 A CN 112931934A
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Images
Classifications
-
- 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
Abstract
The invention provides a fragrance-holding and cooling additive and a preparation method and application thereof. The preparation method of the aroma-holding and cooling additive adopts natural L-lysine to catalyze and synthesize the silicon dioxide nano microspheres, and the silica nano microspheres are chemically modified into a supermolecular structure by g 3-aminopropyltrimethoxysilane, so that the adsorbability of an aroma carrier is improved. And then, adding sucrose fatty acid ester to physically coat the silica nanospheres with the supramolecular structure, and chemically modifying the silica nanospheres by utilizing strawberry aldehyde, so that the adsorbability of the modified silica nanospheres with the supramolecular structure on perfume components is further improved, the dispersion uniformity of the modified silica nanospheres with the supramolecular structure in an impregnation liquid containing the perfume components is enhanced, and the modified silica nanospheres can adsorb more cumin essential oil and loquat leaf extract composite perfume components more stably. In addition, the sucrose fatty acid ester has the functions of absorbing heat and reducing temperature, so that the smoke temperature is reduced, the burning sensation of the throat is reduced, and the sensory quality of suction is improved.
Description
Technical Field
The invention belongs to the technical field of tobacco additives, and particularly relates to a fragrance-holding and cooling additive as well as a preparation method and application thereof.
Background
The highest temperature of a traditional cigarette after being ignited is nearly thousand ℃, the temperature of the smoke of the cigarette is reduced after being filtered by the cigarette and the filter stick before being inhaled into the oral cavity of a consumer, but the temperature of the main stream smoke reaching the oral cavity can still reach 35-90 ℃; in order to meet the requirements of smokers in recent years, a new product, namely a short cigarette, enters the market, the cigarette is generally short in length, low in smoke resistance and short in smoke channel, the smoke temperature at the filter tip can reach 65-80 ℃ at most when the cigarette is smoked for 2-3 mouths near the end of smoking, so that consumers feel scorched smoke, and the sensory quality is affected. The low-temperature cigarette is a novel tobacco which is not combusted, and flavor substances of tobacco products are released by electric heating, carbon heating or other heating modes, the heating temperature is usually below 500 ℃, but the taste of the cigarette is influenced due to the fact that a low-temperature cigarette filter stick is short, a smoke channel is short, and the temperature is too high. Generally, under the same reference state, the solid, liquid and gaseous heat break amount of the same substance is sequentially increased, namely the heat energy content is sequentially increased, namely the solid, liquid and gas with the same temperature are ingested, the sensory temperature of a human body is sequentially increased, so that a consumer can feel a certain burning sensation when smoking a short cigarette, certain damage is caused to the oral viscosity, tracheal mucosa and the like of the consumer, and the burning sensation is more severe due to the further shortening of the smoke heat exchange time at the later stage of cigarette smoking, thereby influencing the cigarette smoking quality. Therefore, the existing short cigarettes, the novel low-temperature electric heating tobacco and the like have the design requirement of smoke cooling. The measures in the aspect of cooling at home and abroad mainly focus on the aspects of adding polylactic acid phase-change cooling materials (Feimo corporation), polyethylene glycols, hydrated salts and the like, designing cavities, lengthening smoke channels, improving cooling structures and the like.
Meanwhile, the traditional and novel tobaccos have the requirements of fragrance compensation, aroma enhancement, rich fragrance and fragrance retention. The flavoring substance is used as tobacco additive, and has effects of flavoring, increasing sweetness, improving taste, relieving irritation, and improving tobacco quality. At present, most of cigarette flavor substances have the characteristics of low boiling point and volatility, the flavor of the cigarette flavor substances is gradually lightened under the influence of external factors or combustion heating, the quality of the cigarette flavor substances is reduced, the application range of the cigarette flavor substances is limited to a certain extent, and the release rate of the tobacco flavor substances can be effectively stabilized and delayed by a stable slow release technology, so that the flavor is lasting and stable. At present, the stable slow release technology of the inclusion compound is more applied to slow release of the tobacco flavor. Common inclusion compounds are inclusion complexes and microcapsules, which maintain the stability of the inclusion subject and slowly release the inclusion subject upon heating. Common inclusion compound main molecules are cyclodextrin, cucurbituril, liposome and the like; the microcapsule has a core-shell structure, wherein the shell is a polymer, and the core is an inclusion object. The capsule core is protected by the capsule shell, has stable property at normal temperature and normal pressure, and the substances in the capsule core penetrate through the capsule shell to be slowly released under certain pressure, temperature or enzymolysis conditions. Wuyan, etc. uses mango as raw material to extract fragrant substance, uses sodium alginate as wrapping material, and adopts phase separation-coacervation method-spray drying to prepare mango fragrance microcapsule, the grain size distribution range is 36-1100 μm, the capsule shell surface is porous structure, and when it is added into tobacco, it has long-lasting and full fragrance and less impurity gas. The balm and the like respectively adopt a phase separation-coacervation method and a solvent dehydration method to prepare the peppermint oil microcapsules, and the content of the peppermint oil in the microcapsules prepared by the two methods is respectively 11.96 percent and 16.30 percent. The peppermint oil is stable in the capsule under normal temperature and pressure. And then adding the peppermint oil microcapsules (the adding amount is 10-15 mg/cigarette) into the cloud tobacco (panda), the cloud tobacco (soft delicacies) and the cloud tobacco (red impression) filter tips. The red date essential oil microcapsule is prepared by adopting an agglomeration method, namely spray drying, and the like, so that the stability of the red date essential oil is effectively maintained. The stability and the slow release performance of the mint oil microcapsules on tobacco shreds are inspected by using the Xulan orchid and the like, and the transfer rate can reach 30-45%, and the release of the menthol is stable when the transfer rate is higher than that of mint type cigarettes with the same tar amount. In the existing slow release materials for adsorbing the spices, such as porous material activated carbon, the capacities of adsorbing and retaining the essences are very strong, but when smoke passes through, only a small amount of the essences enter main stream smoke, so that the slow release capacity of the activated carbon slow release spices is weak when the cigarettes are burnt and smoked and heated, and the characteristic aroma is difficult to release; mesoporous molecular sieves are expensive and difficult to manufacture and synthesize, are commercially rare at present, and are reported to be used for smoke adsorption in cigarettes; the adsorbability of other adsorbing materials to volatile spices is low, such as forest, and the like, and the loading capacity of aluminum silicate and modified aluminum silicate to menthol is 8-14% which is obtained by researching the adsorption/tolyful performance research of the aluminum silicate modified by different metal ions to the menthol (thesis, modern food technology); the microcapsule perfuming technology has large influence of temperature and pressure on microcapsules and uneven fragrance release; the ion exchange resin perfuming technology has stable property, good fragrance retention property and good slow release performance, but has narrow range of applicable perfume and high cost; zhang Xin et al propose a method for preparing light-controlled slow-release rod-shaped silica nano perfume (invention patent, acceptance number 201810358478. X), which adopts nano mesoporous silica to carry perfume and prepare photoresponse slow-release nano perfume for enhancing fragrance of wallpaper, and the carrier: the ratio of the spices is 1-5: 1, the loading capacity of the spices is less than 16.67%, the spices have a normal-temperature fragrance-holding slow-release effect, and thermogravimetric experiments show that the release rate of the spices is 50% at about 200 ℃, and the heat release performance is not strong. The prior clathrate compound slow-release material has the defects and problems of complex material components and process, higher cost of raw materials and processing, unobvious characteristic of heat-releasing fragrance effect, insufficient stability and durability, and the like.
Therefore, it is necessary to research short cigarettes, novel low-temperature electrically heated tobacco and the like on the aspects of enhancing aroma characteristics and enhancing controllable heat release performance, so that the cigarette can lower smoke temperature, reduce irritation and throat burning sensation and comprehensively improve the sensory quality of the cigarettes while enhancing aroma, enriching aroma and keeping the aroma.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a fragrance-holding and temperature-reducing additive and a preparation method and application thereof.
In order to solve the technical problems, the invention adopts the following technical scheme:
a preparation method of a fragrance-holding and temperature-reducing additive comprises the following steps:
(1) dispersing silicon dioxide nano microsphere powder into absolute ethyl alcohol, carrying out ultrasonic treatment, then adding 3-aminopropyltrimethoxysilane into the dispersion liquid for modification treatment, and washing and drying a reaction product to obtain the silicon dioxide nano microsphere powder with a supermolecular structure;
(2) heating a mixed system containing the supermolecular structure silicon dioxide nano microsphere powder, sucrose fatty acid ester, strawberry aldehyde and distilled water at 70-90 ℃, condensing and refluxing for reaction for 12-24 hours, and washing and drying a reaction product to obtain modified supermolecular structure silicon dioxide nano microsphere powder;
(3) and (3) placing the modified silica nanoparticle powder with the supramolecular structure into an ethanol solution containing cumin essential oil and loquat leaf extract for dipping treatment, and then preparing the flavoring and cooling additive powder by adopting spray drying.
Preferably, the silicon dioxide nano microsphere powder is prepared by the following method: adding tetraethyl orthosilicate into an aqueous solution of L-lysine, placing a reaction system at 20-35 ℃ for stirring reaction, and drying and roasting a reaction product to obtain the L-lysine.
Preferably, the mass ratio of the L-lysine to the tetraethyl orthosilicate in the reaction system is (0.11-0.2): (0.5 to 10).
Preferably, the roasting treatment temperature is 500-600 ℃, and the roasting time is 6-10 h.
Preferably, the mass ratio of the silicon dioxide nano microsphere powder to the g 3-aminopropyltrimethoxysilane is (0.5-10): (0.1 to 1).
Preferably, the mass ratio of the supermolecular structure silicon dioxide nano microsphere powder, the sucrose fatty acid ester and the strawberry aldehyde in the mixed system is (1-10): (0.1-8): (0.1-2.5).
Preferably, the mass ratio of the cumin essential oil to the loquat leaf extract in the ethanol solution is (0.1-0.5): 1, and the mass of the modified silica nanoparticle powder with the supramolecular structure is 3-20 times of the sum of the mass of the cumin essential oil and the loquat leaf extract.
The invention also provides a fragrance-holding and cooling additive which is prepared by the preparation method of the fragrance-holding and cooling additive.
The invention also provides an application of the aroma-holding and cooling additive in cigarette aroma-holding and cooling: and uniformly adding the aroma-holding and temperature-reducing additive into a filter fiber tow of the cigarette filter stick.
Preferably, the addition amount of the aroma-holding and temperature-reducing additive in the cigarette filter stick is 0.2-0.8 g per filter stick.
Compared with the prior art, the invention has the beneficial effects that:
when the aroma-holding cooling additive is prepared, the silica nano-microspheres are subjected to supermolecular structure modification by adding the g 3-aminopropyltrimethoxysilane, and amino functional groups are introduced to the surfaces of the silica nano-microspheres, so that supermolecular action is constructed between the silica nano-microspheres and aroma components loaded by the silica nano-microspheres, the loading capacity and the normal-temperature loading stability of the aroma components are improved, and the slow-release aroma-holding effect is enhanced. On the other hand, the invention further adopts sucrose fatty acid ester to physically coat the silica nano microspheres with the supermolecular structure and utilizes strawberry aldehyde to chemically modify the silica nano microspheres, thereby further improving the adsorbability of the modified silica nano microspheres with the supermolecular structure to perfume components and enhancing the dispersion uniformity of the modified silica nano microspheres with the supermolecular structure in the impregnation liquid containing the perfume components, so that the modified silica nano microspheres can adsorb more and more stable cumin essential oil and loquat leaf extract composite perfume components. In addition, the sucrose fatty acid ester has the functions of absorbing heat and reducing temperature, so that the smoke temperature is reduced, the burning sensation of the throat is reduced, and the sensory quality of suction is improved.
The prepared fragrant cooling additive has controllable heat release property of slow-release cumin essential oil and loquat leaf extract, and can reduce the smoke temperature. The aroma-holding and cooling additive prepared by the invention has the advantages of enhancing the stability of normal-temperature storage and heat release stability of characteristic aroma while holding aroma and enriching aroma, reducing smoke burning sensation and irritation, and improving smoking taste and aroma quality.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention. The objectives and other advantages of the invention may be realized and attained by the structure particularly pointed out in the written description and claims hereof as well as the appended drawings.
It will be appreciated by those skilled in the art that the objects and advantages that can be achieved with the present invention are not limited to the specific details set forth above, and that these and other objects that can be achieved with the present invention will be more clearly understood from the detailed description that follows.
Drawings
FIG. 1 is a comparison graph of the results of the investigation of the stability at room temperature of additives of different forms provided in application example 1 of the present invention after being left for 15 days at 40 ℃;
FIG. 2 is a comparative graph showing the results of the investigation of the loading of various additives of the present invention in application example 2;
FIG. 3 is a comparison chart of actual content investigation results of different forms of additives in cigarettes provided by application example 3 of the present invention;
FIG. 4 is a comparison chart of the heat release behavior examination results of different forms of additives provided in application example 4 of the present invention when heated at 80 ℃ for 10min in an electrically heated low temperature cigarette.
Detailed Description
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention.
It is to be understood that the processing equipment or apparatus not specifically identified in the following examples is conventional in the art.
Furthermore, it is to be understood that one or more method steps mentioned in the present invention does not exclude that other method steps may also be present before or after the combined steps or that other method steps may also be inserted between these explicitly mentioned steps, unless otherwise indicated; moreover, unless otherwise indicated, the numbering of the various method steps is merely a convenient tool for identifying the various method steps, and is not intended to limit the order in which the method steps are arranged or the scope of the invention in which the invention may be practiced, and changes or modifications in the relative relationship may be made without substantially changing the technical content.
The embodiment of the invention provides a preparation method of a fragrance-holding and cooling additive, which comprises the following steps:
(1) dispersing silicon dioxide nano microsphere powder into absolute ethyl alcohol, carrying out ultrasonic treatment, then adding 3-aminopropyltrimethoxysilane into the dispersion liquid for modification treatment, and washing and drying a reaction product to obtain the silicon dioxide nano microsphere powder with a supermolecular structure;
(2) heating a mixed system containing the silica nano microsphere powder with the supermolecular structure, sucrose fatty acid ester, strawberry aldehyde and distilled water at 70-90 ℃, condensing and refluxing for 12-24 hours, and washing and drying a reaction product to obtain modified silica nano microsphere powder with the supermolecular structure;
(3) and (3) placing the modified silica nanoparticle powder with the supramolecular structure into an ethanol solution containing cumin essential oil and loquat leaf extract for soaking treatment, and then preparing the flavoring and cooling additive powder by adopting spray drying.
When the aroma-holding cooling additive is prepared, the silica nano-microspheres are subjected to supermolecular structure modification by adding the g 3-aminopropyltrimethoxysilane, and amino functional groups are introduced to the surfaces of the silica nano-microspheres, so that supermolecular action is constructed between the silica nano-microspheres and aroma components loaded by the silica nano-microspheres, the loading capacity and the normal-temperature loading stability of the aroma components are improved, and the slow-release aroma-holding effect is enhanced. On the other hand, the invention further adopts sucrose fatty acid ester to physically coat the silica nano microspheres with the supermolecular structure and utilizes strawberry aldehyde to chemically modify the silica nano microspheres, thereby further improving the adsorbability of the modified silica nano microspheres with the supermolecular structure to perfume components and enhancing the dispersion uniformity of the modified silica nano microspheres with the supermolecular structure in the impregnation liquid containing the perfume components, so that the modified silica nano microspheres can adsorb more and more stable cumin essential oil and loquat leaf extract composite perfume components. In addition, the sucrose fatty acid ester has the functions of absorbing heat and reducing temperature, so that the smoke temperature is reduced, the burning sensation of the throat is reduced, and the sensory quality of suction is improved.
Preferably, the silicon dioxide nano microsphere powder in the step (1) is prepared by the following method: adding tetraethyl orthosilicate into an aqueous solution of L-lysine, placing a reaction system at 20-35 ℃ for stirring reaction, and drying and roasting a reaction product to obtain the L-lysine. More preferably, the mass ratio of L-lysine to tetraethyl orthosilicate in the reaction system is (0.11-0.2): (0.5 to 10). Preferably, the roasting treatment temperature is 500-600 ℃, and the roasting time is 6-10 h. In the step (1), L-lysine is used as a catalyst in the preparation process of the silicon dioxide nano microsphere powder, and the L-lysine is natural alkalescent amino acid, so that compared with conventional acid and alkali catalysts, the speed of catalytic synthesis is low, the preparation of the silicon dioxide nano microspheres with uniform size is facilitated, the batch stability of the prepared silicon dioxide nano microspheres is improved, and the product quality is more stable; meanwhile, acid and alkali pollution and residues are avoided in the preparation process, and the L-lysine can be used as a natural additive for cigarettes, so that the residual L-lysine in the reaction product is not required to be recovered or removed, the preparation process is simpler, and the preparation process is more environment-friendly.
Preferably, the mass ratio of the silicon dioxide nano microsphere powder to the g 3-aminopropyltrimethoxysilane in the step (1) is (0.5-10): (0.1 to 1). The ultrasonic treatment frequency is 25 KHZ-50 KHZ, and the ultrasonic treatment time is 10-30 min. And promoting the silicon dioxide nano microsphere powder to be uniformly dispersed in the absolute ethyl alcohol solution through ultrasonic treatment.
Preferably, the mass ratio of the supermolecular structure silicon dioxide nano microsphere powder, the sucrose fatty acid ester and the strawberry aldehyde in the mixed system in the step (2) is (1-10): (0.1-8): (0.1-2.5). The silica nanospheres with the supermolecular structure are chemically modified by strawberry aldehyde, so that the adsorption performance of the silica nanospheres with the supermolecular structure on perfume substances is improved. The sucrose fatty acid ester can be uniformly coated on the surface of the silica nano microsphere with the supermolecular structure, the surface property of the silica nano microsphere can be changed, the agglomeration among powder particles is reduced, the monodispersion stability of the silica nano microsphere with the supermolecular structure is improved, the adsorbability of the silica nano microsphere to perfume substances is improved, and the loading capacity and the normal temperature stability of the silica nano microsphere with the supermolecular structure for adsorbing perfume are improved. In addition, the sucrose fatty acid ester can absorb heat and melt under the heating working condition, the controllable heat release property of the adsorbed perfume is increased, the modified silica nano microsphere with the supermolecular structure can keep balanced and lasting characteristic fragrance heat release, and the modified silica nano microsphere has the effects of absorbing heat and reducing temperature.
Preferably, the mass ratio of the cumin essential oil to the loquat leaf extract in the ethanol solution in the step (3) is (0.1-0.5): 1, and the mass of the modified silica nanoparticle powder with the supramolecular structure is 3-20 times of the sum of the mass of the cumin essential oil and the mass of the loquat leaf extract. Preferably, in the dipping treatment process, in order to promote the modified silica nanospheres with the supramolecular structure to adsorb the cumin essential oil and the loquat leaf extract composite perfume components more quickly, the dipping system can be placed in a constant-temperature oscillator, the oscillation frequency is 400-500 rpm, and the oscillation time is 0.1-0.5 h. The cumin essential oil used in the invention has aromatic and strong flavor, strong style and characteristics, strong bactericidal action, natural and strong inoxidizability, and has health care effects of regulating qi, stimulating appetite, dispelling cold, removing dampness, resisting allergy, resisting platelet aggregation, reducing blood sugar and the like; the loquat leaf extract is rich in ursolic acid, is a triterpenoid, has various biological effects of calming, resisting inflammation, resisting bacteria, resisting diabetes, resisting ulcer, reducing blood sugar and the like, also has the effects of resisting cancer, promoting cancer, inducing F9 teratoma cell differentiation and resisting angiogenesis, and has obvious antioxidant function. The natural substances with the biological activities of characteristic aroma, strong oxidation resistance, cough relieving, phlegm eliminating and the like are adsorbed into the modified silica nano microsphere powder with the supermolecular structure, so that the stability is obviously enhanced when the natural substances are stored at normal temperature, the heat release behavior is good, stable and uniform when the natural substances are electrically heated and sucked, and the style and the characteristics of the product can be kept stable. The cumin aroma style is stable, uniform and strong, the aroma and the taste can be enriched, the loquat leaf extract has the moistening effect of relieving cough and reducing sputum, and the irritation of smoke to the throat is reduced.
The invention also provides a fragrance-holding and cooling additive which is prepared by the preparation method of the fragrance-holding and cooling additive. The prepared fragrant cooling additive has controllable heat release property of slow-release cumin essential oil and loquat leaf extract, and can reduce the smoke temperature. The aroma-holding and cooling additive prepared by the invention has the advantages of enhancing the stability of normal-temperature storage and heat release stability of characteristic aroma while holding aroma and enriching aroma, reducing smoke burning sensation and irritation, and improving smoking taste and aroma quality.
The invention also provides an application of the aroma-holding and cooling additive in cigarette aroma-holding and cooling: the aroma-holding and temperature-reducing additive is uniformly added into the filter fiber tow of the cigarette filter stick. Specifically, the prepared fragrance-holding and temperature-reducing additive powder containing the supermolecular structure is directly and uniformly added into a filter fiber tow of a cigarette filter stick in the process of forming the electrically-heated low-temperature cigarette filter stick, and the filter fiber tow is generally an acetate fiber tow. Preferably, the addition amount of the aroma-holding and temperature-reducing additive in the cigarette filter stick is 0.2-0.8 g per filter stick. Then, the mixture is cut and compounded into the electric heating low-temperature cigarette composite filter stick, and the electric heating low-temperature cigarette is rolled and connected by the conventional process.
The following is a further description with reference to specific examples.
Example 1
The embodiment 1 of the invention provides a fragrance-holding and cooling additive and a preparation method and application thereof. The aroma-holding and cooling additive is prepared by the following steps:
(1) preparing silicon dioxide nano microsphere powder: 0.11 part of L-lysine and 10 parts of distilled water were weighed and mixed in a container, magnetons were added, and stirred at 25 ℃ for 10min to form a colorless solution. Adding 0.5 part of tetraethyl orthosilicate, sealing the container, stirring for 10min at 25 ℃, and rotating at 300 rpm to obtain the silicon dioxide nano microsphere dispersion liquid. And (3) after the dispersion liquid is subjected to solid-liquid separation, placing the solid product in a 60 ℃ oven for heat preservation for 6 h for drying, placing the dried solid in a muffle furnace, roasting for 6 h at 500 ℃, and heating at the rate of 1 ℃/min to obtain silicon dioxide nano microsphere powder.
(2) Preparing supermolecular structure silicon dioxide nano microsphere powder: and (2) dispersing 0.5 part of the silicon dioxide nano microsphere powder in the step (1) in 10 parts of absolute ethyl alcohol, performing ultrasonic treatment for 10min at the frequency of 25 KHZ, adding 0.1 part of 3-aminopropyltrimethoxysilane, stirring at room temperature (100 rpm for 12 h), filtering, washing with absolute ethyl alcohol, and performing vacuum drying at 60 ℃ to obtain the silicon dioxide nano microsphere powder with the supermolecular structure.
(3) Preparing modified supermolecular structure silicon dioxide nano microsphere powder: preparing 1 part of the silica nano microsphere powder with the supermolecular structure in the step (2), 0.1 part of sucrose fatty acid ester, 0.1 part of strawberry aldehyde and 10 parts of distilled water into a mixed system, heating the mixed system at 70 ℃, condensing and refluxing, stirring at the rotating speed of 350 rpm for 12 hours, washing a reaction product with absolute ethyl alcohol, then placing the washed reaction product in a 60 ℃ oven, preserving heat for 12 hours, and drying to obtain the modified silicon dioxide nano microsphere powder with the supermolecular structure.
(4) Preparing aroma-holding and cooling additive powder: sequentially adding cumin essential oil and loquat leaf extract in a mass ratio of 0.1:1 and supermolecular structure silicon dioxide nanometer microsphere powder (the mass ratio is 3 times of the mass of the mixture of the cumin essential oil and the loquat leaf extract) in the step (3) into a 60% ethanol solution for impregnation treatment, and placing an impregnation system in a constant temperature oscillator, wherein the oscillation frequency is 400rpm, and the oscillation time is 0.1 h. After the impregnation is finished, the solvent of the impregnation system is volatilized by adopting spray drying, and the fragrance-holding and temperature-reducing additive powder containing the supermolecular structure is obtained.
(5) The application of the flavor-holding and temperature-reducing additive containing a supermolecular structure in electrically heating low-temperature cigarettes comprises the following steps: applying the aroma-holding and temperature-reducing additive powder prepared in the step (4) to the forming process of the electric heating low-temperature cigarette filter stick: directly and uniformly adding the mixture into an acetate fiber tow, wherein the adding amount is 0.2 g per filter stick, then slitting and compounding the mixture into an electric heating low-temperature cigarette composite filter stick, and rolling and connecting the electric heating low-temperature cigarette composite filter stick into an electric heating low-temperature cigarette by a conventional process.
Example 2
The embodiment 2 of the invention provides a fragrance-holding and cooling additive and a preparation method and application thereof. The aroma-holding and cooling additive is prepared by the following steps:
(1) preparing silicon dioxide nano microsphere powder: 0.15 part of L-lysine and 50 parts of distilled water were weighed and mixed in a container, magnetons were put in, and stirred at 35 ℃ for 15min to form a colorless solution. Adding 5 parts of tetraethyl orthosilicate, sealing the container, stirring for 20min at 35 ℃, and rotating at 650 rpm to obtain the silicon dioxide nano microsphere dispersion liquid. And (3) after solid-liquid separation is carried out on the dispersion, the solid product is placed in a 70 ℃ oven for heat preservation for 9 h for drying, the dried solid is placed in a muffle furnace for roasting at 550 ℃ for 8 h, and the heating rate is 3 ℃/min, so that silicon dioxide nano microsphere powder is obtained.
(2) Preparing supermolecular structure silicon dioxide nano microsphere powder: and (2) dispersing 5.5 parts of the silicon dioxide nano microsphere powder in the step (1) in 55 parts of absolute ethyl alcohol, performing ultrasonic treatment for 20min at the frequency of 35 KHZ, adding 0.5 part of 3-aminopropyltrimethoxysilane, stirring at room temperature (200 rpm for 18 h), filtering, washing with absolute ethyl alcohol, and performing vacuum drying at 70 ℃ to obtain the silicon dioxide nano microsphere powder with the supermolecular structure.
(3) Preparing modified supermolecular structure silicon dioxide nano microsphere powder: preparing 5.5 parts of the silica nano microsphere powder with the supermolecular structure in the step (2), 4 parts of sucrose fatty acid ester, 1.2 parts of strawberry aldehyde and 55 parts of distilled water into a mixed system, heating the mixed system at 85 ℃, condensing and refluxing, stirring at the rotation speed of 550 rpm for 12 hours, washing a reaction product with absolute ethyl alcohol, placing the washed reaction product in a 70 ℃ oven, preserving heat for 12 hours, and drying to obtain the modified silicon dioxide nano microsphere powder with the supermolecular structure.
(4) Preparing aroma-holding and cooling additive powder: sequentially adding 0.25:1 mass ratio of cumin essential oil, loquat leaf extract and supermolecular structure silicon dioxide nanometer microsphere powder (12 times of the mass of the mixture of cumin essential oil and loquat leaf extract) in (3) into 70% ethanol solution for impregnation treatment, and placing an impregnation system in a constant temperature oscillator, wherein the oscillation frequency is 450rpm, and the oscillation time is 0.25 h. After the impregnation is finished, the solvent of the impregnation system is volatilized by adopting spray drying, and the fragrance-holding and temperature-reducing additive powder containing the supermolecular structure is obtained.
(5) The application of the flavor-holding and temperature-reducing additive containing a supermolecular structure in electrically heating low-temperature cigarettes comprises the following steps: applying the aroma-holding and temperature-reducing additive powder prepared in the step (4) to the forming process of the electric heating low-temperature cigarette filter stick: directly and uniformly adding the mixture into an acetate fiber tow, wherein the adding amount is 0.4 g per filter stick, then slitting and compounding the mixture into an electric heating low-temperature cigarette composite filter stick, and rolling and connecting the electric heating low-temperature cigarette composite filter stick into an electric heating low-temperature cigarette by a conventional process.
Example 3
The embodiment 3 of the invention provides a fragrance-holding and cooling additive and a preparation method and application thereof. The aroma-holding and cooling additive is prepared by the following steps:
(1) preparing silicon dioxide nano microsphere powder: 0.2 part of L-lysine and 100 parts of distilled water were weighed and mixed in a container, magnetons were added, and stirred at 20 ℃ for 20min to form a colorless solution. Adding 10 parts of tetraethyl orthosilicate, sealing the container, stirring for 30 min at 20 ℃, and rotating at 1000 rpm to obtain the silicon dioxide nano microsphere dispersion liquid. And (3) after the dispersion liquid is subjected to solid-liquid separation, placing the solid product in an oven at 80 ℃ for heat preservation for 12h for drying, placing the dried solid in a muffle furnace, roasting at 600 ℃ for 10h, and heating at the rate of 5 ℃/min to obtain silicon dioxide nano microsphere powder.
(2) Preparing supermolecular structure silicon dioxide nano microsphere powder: and (2) dispersing 10 parts of the silicon dioxide nano microsphere powder in the step (1) in 100 parts of absolute ethyl alcohol, performing ultrasonic treatment for 30 min at the frequency of 50 KHZ, adding 1 part of 3-aminopropyltrimethoxysilane, stirring slightly at room temperature (stirring at 300 rpm for 24 h), filtering, washing with absolute ethyl alcohol, and performing vacuum drying at 80 ℃ to obtain the silicon dioxide nano microsphere powder with the supermolecular structure.
(3) Preparing modified supermolecular structure silicon dioxide nano microsphere powder: preparing 10 parts of the silica nano microsphere powder with the supermolecular structure in the step (2), 8 parts of sucrose fatty acid ester, 2.5 parts of strawberry aldehyde and 100 parts of distilled water into a mixed system, heating the mixed system at 95 ℃, condensing and refluxing, stirring at the rotating speed of 900 rpm for 24 hours, washing a reaction product with absolute ethyl alcohol, placing the washed reaction product in an oven at 80 ℃ for heat preservation for 12 hours, and drying to obtain the modified silica nano microsphere powder with the supermolecular structure.
(4) Preparing aroma-holding and cooling additive powder: sequentially adding cumin essential oil and loquat leaf extract in a mass ratio of 0.5:1 and supermolecular structure silicon dioxide nanometer microsphere powder (the mass ratio is 20 times of the mass of the mixture of the cumin essential oil and the loquat leaf extract) in the step (3) into 75% ethanol solution for impregnation treatment, and placing an impregnation system in a constant temperature oscillator, wherein the oscillation frequency is 500rpm, and the oscillation time is 0.5 h. After the impregnation is finished, the solvent of the impregnation system is volatilized by adopting spray drying, and the fragrance-holding and temperature-reducing additive powder containing the supermolecular structure is obtained.
(5) The application of the flavor-holding and temperature-reducing additive containing a supermolecular structure in electrically heating low-temperature cigarettes comprises the following steps: applying the aroma-holding and temperature-reducing additive powder prepared in the step (4) to the forming process of the electric heating low-temperature cigarette filter stick: directly and uniformly adding the mixture into an acetate fiber tow, wherein the adding amount is 0.8g per filter stick, then slitting and compounding the mixture into an electric heating low-temperature cigarette composite filter stick, and rolling and connecting the electric heating low-temperature cigarette composite filter stick into an electric heating low-temperature cigarette by a conventional process.
Application example 1 different forms of additives were examined for stability at ambient temperature after 15 days at 40 deg.C
The storage conditions of the perfume were simulated, the perfume was placed in a forced air oven at a constant temperature of 40 ℃ for 15 days in an open air environment, and the room temperature stability of the pure additive (composite perfume of cumin essential oil and loquat leaf extract), the nanoparticle loaded additive (the nanoparticle is the silica nanoparticle powder prepared in step (1) of example 1), and the fragrance-holding and cooling additive containing a supramolecular structure (prepared in example 1) was compared by a weighing method, and the results are shown in fig. 1. As seen from fig. 1, the retention rate of the nano microsphere loaded additive is increased from 10.5% to 67.3%, the normal temperature stability of the additive is improved, and the retention rate of the fragrance-holding and temperature-reducing additive introduced with the supermolecular structure is further increased to 93.2%, compared with the nano microsphere loaded additive, the retention rate of the nano microsphere loaded additive to the perfume is increased by 39.10%; compared with pure additive, the retention rate of the perfume is improved by 8.88 times. Namely, the aroma-holding and cooling additive prepared in the embodiment 1 of the invention has obviously enhanced normal temperature stability, and greatly maintains the natural biological activity of the aroma substances and the lasting stability of the characteristic aroma.
Application example 2 load investigation of different forms of additives
The nano microspheres (the nano microspheres are the silica nano microsphere powder prepared in the step (1) of example 1) and the microspheres with the modified supramolecular structure (the modified supramolecular structure silica nano microsphere powder prepared in the step (3) of example 1) are respectively impregnated with an excessive amount of additive (the composite spice of cumin essential oil and loquat leaf extract), and after elution and drying by a 70% ethanol solution, the additive loading amount is weighed, and the result is shown in fig. 2. As seen from FIG. 2, the modified microspheres containing supramolecular structures have obviously enhanced affinity to additives, and the loading capacity is increased from 18.3% to 26.8%, which is increased by 36.61%.
Application example 3 actual content investigation of different forms of additives in cigarettes
The actual contents of the additives carried by the different forms of carriers (referring to the actual contents of the composite spices of cumin essential oil and loquat leaf extract in the cigarettes) are shown in fig. 3. As seen from figure 3, the highest loading capacity of the fragrance-holding and cooling additive containing a supramolecular structure, prepared in example 1 of the invention, on the composite spice is 13.4 mg/cigarette, which is 10 mg/cigarette higher than the addition of a pure additive in a cigarette, and the addition is increased by 25%.
Application example 4 investigation of heat release behavior of additives with different forms in electrically heated low-temperature cigarette heated at 80 ℃ for 10min
Comparing different forms of additives, namely pure additives (composite spice of cumin essential oil and loquat leaf extract), nano microsphere loaded additives (nano microspheres are silicon dioxide nano microsphere powder prepared in the step (1) of the example 1) and fragrance-holding and temperature-reducing additives containing a supramolecular structure (prepared in the example 1), respectively and uniformly adding the additives into acetate fiber tows in the filter rod forming process to prepare a composite filter rod, then rolling and connecting the composite filter rod into cigarettes, standing for 15 days, and heating at 80 ℃ for 10min, wherein the quality of the additives actually released by heat of each cigarette is shown in fig. 4. As can be seen from FIG. 4, the release of the different forms of the additive to the compounded perfume was 1.01 mg/ramus, 4.879 mg/ramus, and 11.49 mg/ramus, respectively. The aroma-holding and temperature-reducing additive prepared in the embodiment 1 of the invention can obviously improve the heat release amount of the aroma of the cigarette under the heated condition.
Application example 5 sensory evaluation
After the three cigarettes rolled in application example 4 and the conventional blank cigarette (i.e., the cigarette without the compound flavor) were left under the same conditions for 15 days, sensory evaluation was performed using main indexes such as flavor characteristics, durability, heat release characteristic strength, uniformity, and the like, and the evaluation results are shown in table 1.
The same manner is adopted for the aroma-holding and temperature-reducing additives prepared in the embodiment 2 and the embodiment 3 of the invention to sequentially conduct the performance or index investigation of the application examples 1-5, and the investigation result is similar to the conclusion that the aroma-holding and temperature-reducing additives prepared in the embodiment 1 have controllable heat release performance of the slow-release cumin essential oil and the loquat leaf extract, and the aroma-holding and temperature-reducing additives prepared in the embodiment of the invention can hold aroma and enrich aroma, enhance the storage stability and heat release stability of characteristic aroma at normal temperature, and improve the smoking taste and the aroma quality.
The protective scope of the present invention is not limited to the above-described embodiments, and it is apparent that various modifications and variations can be made to the present invention by those skilled in the art without departing from the scope and spirit of the present invention. It is intended that the present invention cover the modifications and variations of this invention provided they come within the scope of the appended claims and their equivalents.
Claims (10)
1. A preparation method of a fragrance-holding and temperature-reducing additive is characterized by comprising the following steps:
(1) dispersing silicon dioxide nano microsphere powder into absolute ethyl alcohol, carrying out ultrasonic treatment, then adding 3-aminopropyltrimethoxysilane into the dispersion liquid for modification treatment, and washing and drying a reaction product to obtain the silicon dioxide nano microsphere powder with a supermolecular structure;
(2) heating a mixed system containing the supermolecular structure silicon dioxide nano microsphere powder, sucrose fatty acid ester, strawberry aldehyde and distilled water at 70-90 ℃, condensing and refluxing for reaction for 12-24 hours, and washing and drying a reaction product to obtain modified supermolecular structure silicon dioxide nano microsphere powder;
(3) and (3) placing the modified silica nanoparticle powder with the supramolecular structure into an ethanol solution containing cumin essential oil and loquat leaf extract for dipping treatment, and then preparing the flavoring and cooling additive powder by adopting spray drying.
2. The method for preparing the aroma-holding and temperature-reducing additive according to claim 1, wherein the silicon dioxide nano microsphere powder is prepared by the following method: adding tetraethyl orthosilicate into an aqueous solution of L-lysine, placing a reaction system at 20-35 ℃ for stirring reaction, and drying and roasting a reaction product to obtain the L-lysine.
3. The preparation method of the aroma-maintaining and temperature-reducing additive according to claim 2, wherein the mass ratio of the L-lysine to the tetraethyl orthosilicate in the reaction system is (0.11-0.2): (0.5 to 10).
4. The preparation method of the aroma-maintaining and temperature-reducing additive according to claim 3, wherein the roasting treatment temperature is 500-600 ℃, and the roasting time is 6-10 h.
5. The preparation method of the aroma-maintaining and temperature-reducing additive according to claim 2, wherein the mass ratio of the silica nano microsphere powder to the g 3-aminopropyltrimethoxysilane is (0.5-10): (0.1 to 1).
6. The preparation method of the aroma-maintaining and temperature-reducing additive according to claim 2, wherein the mass ratio of the supermolecular structure silica nanosphere powder, the sucrose fatty acid ester and the strawberry aldehyde in the mixed system is (1-10): (0.1-8): (0.1-2.5).
7. The preparation method of the fragrant cooling additive as claimed in claim 2, wherein the mass ratio of the cumin essential oil to the loquat leaf extract in the ethanol solution is (0.1-0.5): 1, and the mass of the modified silica nanosphere powder with the supramolecular structure is 3-20 times of the sum of the mass of the cumin essential oil and the mass of the loquat leaf extract.
8. An aroma-holding and temperature-reducing additive, which is characterized by being prepared by the preparation method of the aroma-holding and temperature-reducing additive according to any one of claims 1 to 7.
9. The use of the flavor-holding and temperature-reducing additive for holding flavor and reducing temperature of cigarettes according to claim 8, wherein the flavor-holding and temperature-reducing additive is uniformly added into filter fiber tows of cigarette filter sticks.
10. The application of the aroma-holding and cooling additive to cigarette aroma-holding and cooling according to claim 9, wherein the addition amount of the aroma-holding and cooling additive in a cigarette filter stick is 0.2-0.8 g per filter stick.
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