Functional particles applied to multi-component system fragrances and preparation method

Abstract

The application provides a functional granule applied to a multi-element system flavor and a preparation method, and relates to the tobacco processing technical field. The granule has a three-dimensional net structure in which calcium alginate gel is mixed with content, compared with a traditional burst bead which wraps liquid substances in the inside, the weight of the granule is lighter, the single granule is lighter than the traditional granule, the use cost is low for filter rod production manufacturers or cigarette enterprises; the content is mostly a substance with a microporous structure, the substance has good adsorption force on the flavor, the total adsorption amount of the granule flavor is large, and the adsorbed flavor can be stably reserved; the flavor in the granule is released in turn, the release of the flavor forms a gradient, the flavor is light at first and then strong, and the flavor releasing time is prolonged; the granule does not need an adhesive, therefore, the use of ester-soluble flavor and alcohol-soluble flavor for flavoring will not affect the granulation and molding; and when water-soluble flavor is used, the volatilization loss of the flavor is not enough to affect the subsequent normal use.

Description

TECHNICAL FIELD

[0001] The application belongs to the technical field of tobacco processing, and particularly relates to a functional particle applied to a multi-component system flavor and a preparation method. BACKGROUND

[0002] There are various ways to add flavor to cigarettes, such as through the forms of flavor lines, flavor sheets, gels, burst beads, and flavor-loaded particles. In actual use, these flavor-loaded forms have their own characteristics.

[0003] Flavor lines and flavor sheets have the characteristics of strong aroma release capacity and simple manufacturing, but due to their structural characteristics, the retention time of flavor substances is short, and the speed of aroma release during cigarette smoking is too fast, and the continuous release capacity is relatively poor; gels have strong flavor loading capacity and strong slow-release capacity during use, and can release flavor substances uniformly from the beginning to the end of cigarette smoking, providing a good use experience; however, due to the amorphous nature of gels, it is difficult to prepare them in cooperation with cigarettes, and they have a great impact on and change to the cigarette paper and filter rod forming process; burst beads are the earliest flavor-loaded form for cigarettes, have strong flavor loading capacity, mature production process, and are easy to store, and the addition process in the filter rod is relatively simple, but they are expensive and have high use cost.

[0004] The most widely used functional flavor-loaded particles can also be subdivided into various types, such as hollow particles and solid particles, which are porous structure particles with adsorption and flavor modulation functions. For example, porous starch has high specific surface area, rich pore structure, low bulk density, and low particle density, and the prepared particles have high adsorption capacity and adsorption volume. For example, “Ophiopogon japonicus porous particle and its application in cigarettes CN201310645655.X”, the ophiopogon japonicus powder with a water content of 5-6% and a particle size of 100-140 mesh is used as the raw material, and a 10-50% honey water solution is added, and a 20-60 mesh ophiopogon japonicus porous particle is prepared by using a fluidized bed top spraying process, which can effectively reduce the irritation of cigarette smoke and has the function of increasing the sweet and smooth feeling of smoke”; “CN103689801A-A kind of puerariae radix porous particle and its application in cigarettes”, the puerariae radix powder with a water content of 5-6% and a particle size of 100-160 mesh is used as the raw material, and one or more of gelatin, polyvinylpyrrolidone, and carboxymethyl starch sodium is used as the binder, and a 20-60 mesh puerariae radix porous particle is prepared by using a fluidized bed top spraying process”; “CN201911165344.7 A kind of natural biological matrix filter rod particle and its preparation method and application, the porous structure formed by hydrolyzing puerariae radix starch has strong adsorption capacity, which is beneficial to the removal of harmful substances in smoke”.

[0005] The main problem is that the adsorption ability and adsorption capacity of this type of particles mainly depend on the characteristics of the granulation raw materials themselves. The biggest problem with the finished particles also comes from its most critical raw materials. As mentioned in the two references listed above, the two key raw materials are Pueraria powder and Ophiopogon japonicus. Although Pueraria powder has a porous structure with strong adsorption, it can also cause the taste of the smoke to be dry; Ophiopogon japonicus can effectively reduce the irritation of smoke and increase the sweetness, but its sugar content is high and it is easy to deteriorate and breed bacteria and microorganisms, resulting in the particles not meeting safety standards; in addition, some raw materials for preparing functional particles have special odors that are difficult to remove, etc. These are all adverse effects of raw materials with special functions on the final functional particles.

[0006] In addition, there are the following problems: the flavor substances commonly used in cigarette flavoring mainly include water-soluble flavors, alcohol-soluble flavors, and ester-soluble flavors. Different flavors are dissolved in their corresponding solvents and then applied in two ways: one is to mix with other auxiliary materials and prepare them into particles after adding adhesives; the other is to mix with the prepared particles and adhere to the surface of the particles or be adsorbed into the interior of the particles. For existing functional particles, no matter which application method is used, it is difficult to avoid

[0007] The following questions: Water-soluble flavors need to be dissolved in water and mixed with other raw materials before granulation.

[0008] The amount must be dried. Since it is a solid particle, the drying time and the drying temperature must be increased. As the water evaporates, the volatilization loss of the flavor is relatively large; alcohol-soluble flavors need to be dissolved in alcohol solvents and then mixed with other raw materials and auxiliary materials for granulation and molding, but alcohol solvents will dissolve and destroy the adhesives commonly used in granulation, reduce the overall viscosity, and affect granulation and molding; ester-soluble flavors, the addition of ester substances will cause the raw materials to remain soft and unable to be shaped, and cannot be dried in a short time.

[0009] Therefore, in the process of preparing flavoring functional particles, under the premise of meeting strong adsorption and large adsorption capacity, defects caused by the characteristics of the raw materials themselves should be avoided, especially to avoid negative impacts on their taste, storage and transportation, and cigarette or filter rod molding; at the same time, the obtained functional particles should be able to be applied to flavors and fragrances of various systems to expand their application range. These will be important research directions in this field. Summary of the Invention

[0010] In order to solve the problems in the prior art, the functional granule applied to multi-system essence and perfume and the preparation method are provided, the raw materials and the preparation process of the granule are changed, the functional granule with light weight, high specific surface area, rich pore structure, no influence on the structure strength after contacting with the liquid essence and perfume, no problems such as shedding of the outer surface and the content, etc.

[0011] In order to achieve the above object, the following technical scheme is adopted in the present application.

[0012] The functional granule applied to multi-system essence and perfume is characterized in that the functional granule is a composite structure, comprising a peripheral three-dimensional reticular wrapping layer, an internal three-dimensional grid main body, and pretreated contents uniformly distributed in the internal three-dimensional grid main body; the peripheral three-dimensional reticular wrapping layer is composed of calcium alginate gel particles connected with each other, and the internal three-dimensional grid main body is formed by calcium alginate gel connected with each other; the peripheral three-dimensional reticular wrapping layer comprises an incomplete cross-linking structure formed by one sodium alginate molecule combined with one calcium ion, and a complete cross-linking structure formed by two sodium alginate molecules combined with one calcium ion, and the wrapping layer composed of the incomplete cross-linking structure and the complete cross-linking structure has several holes with a certain diameter; the internal three-dimensional grid main body is composed of the complete cross-linking structure formed by two sodium alginate molecules combined with one calcium ion, and the cross-linking degree and the stretching degree of the internal three-dimensional grid main body are greater than those of the shell, and the pores between the internal three-dimensional grid main body and the shell are filled with the pretreated contents; the pretreated contents are substances with a particle size of 150-500 mesh and insoluble or hardly soluble in water.

[0013] Preferably, the particle size of the functional granule is 18-50 mesh.

[0014] The pretreated contents are inorganic non-metallic substance powders with large pore volume and without water-soluble calcium salt, including any one of microcrystalline cellulose, micro-powder silica gel, light calcium carbonate, diatomite, montmorillonite and activated carbon.

[0015] The process and principle of the peripheral three-dimensional reticular wrapping layer and the internal three-dimensional grid main body are as follows:

[0016] Sodium alginate coagulates when it encounters a water-soluble calcium salt. Sodium alginate dropped into a calcium chloride solution forms calcium alginate; facing the small amount of sodium alginate molecules dropped, not all of them can form a fully cross-linked gel structure with one calcium ion combining with two sodium alginate hydroxyl groups, but only some of them can form a one-to-one combination with some calcium ions, and others can form a one-to-two combination, forming an outer shell of incomplete cross-linking structure and fully cross-linked structure combined on the surface of the droplet. Because it is a combination of the two structures, the surface combination is not tight, resulting in holes on the outer shell, and calcium ions can penetrate the outer shell and gradually penetrate into the interior of the droplet. In the relatively isolated environment inside, the number of sodium alginate molecules is relatively sufficient, and the complete cross-linking combination of sodium alginate and calcium ions can be completed, and the pre-processed content can be fully wrapped by using the multi-cavity structure formed by cross-linking combination; eventually forming a particle composed of a peripheral three-dimensional network wrapping layer, an internal three-dimensional grid main body, and pre-processed content uniformly distributed in the internal three-dimensional grid main body, without forming a structure of a liquid bead or a similar liquid bead structure with a dense and hard outer shell on the outside and no complete gel structure inside.

[0017] The above functional particles are prepared by the following method, characterized by comprising the following steps:

[0018] ①Prepare a sodium alginate solution; use high-viscosity sodium alginate, with a viscosity of 100-670 mPas, a concentration of 0.5%-1.0%;

[0019] ②Prepare a water-soluble calcium salt solution; use a 5%-20% calcium chloride solution, with a viscosity of 4 mPas, a density of 100-120.81 g / 100 ml, and a surface tension of 45-60 mN / m; to facilitate the dehydration of the particle forming suspension in the curing liquid, and to reduce the forming error in the later process, a low concentration will prolong the soaking time;

[0020] ③After the pre-processed content is processed into a powder of 150-500 mesh, add the sodium alginate solution to the powder according to the weight ratio of powder:sodium alginate solution=1:2-1:5, mix uniformly to form an emulsion, with a viscosity of 170-930 mPas, a density of 110-125 g / 100 ml, and a surface tension of 55-60 mN / m;

[0021] ④The emulsion obtained in step ③ is delivered to the liquid substance granulation nozzle by a pneumatic diaphragm pump according to the specified volume and frequency, and the emulsion is sprayed from the liquid substance granulation nozzle into the molding liquid with a certain particle size and frequency by the pulse airflow generated by the pulse air pump, the distance between the outlet end of the liquid substance granulation nozzle and the liquid level of the molding liquid is greater than 0 cm and less than 2 cm, and the emulsion particles enter the water-soluble calcium salt solution to form particles with a particle size of 0.27 mm-0.88 mm;

[0022] ⑤The particles prepared in step ④ are filtered and cleaned, and then soaked in clean water for 10-20 min;

[0023] ⑥The filtered particles are dried and sieved;

[0024] ⑦The particles are perfumed to obtain functional particles.

[0025] Preferably, the perfuming process is to add liquid essence to the particles, mix uniformly according to a mass ratio of 1:1, and then dry at a low temperature of 40-50°C to obtain functional particles; the liquid essence includes water-soluble essence, alcohol-soluble essence, and ester-soluble essence; the added liquid essence is mainly stored in the particle, including the incomplete cross-linked structure and the complete cross-linked structure in the peripheral three-dimensional network wrapping layer, the remaining part of the pores in the complete cross-linked structure in the internal three-dimensional grid body after accommodating the pretreated content, and the pores in the content itself. This adsorption method can not only increase the total adsorption amount of the essence, but also ensure that the adsorbed essence can be relatively stable and retained, even if the essence retained in the pores of the particle structure itself is lost in the subsequent processing process, the essence retained in the pores of the pretreated content in the particle structure is almost unaffected and can be mostly retained, which ensures that during smoking, the high-temperature smoke makes the essence in the particles release in turn, the release of the essence forms a gradient, which is light at the beginning and strong at the end, prolonging the release time, i.e., the essence retained in the pores of the particle structure itself is released at the early stage, and due to the relatively small amount of essence, the aroma is light; at the later stage, as the burning segment is closer and closer to the particles, the smoke temperature gradually rises, and the essence retained in the pretreated content is released, and the amount of essence is large, so the aroma is strong and the duration is long, which has a good aroma retention and release effect.

[0026] In addition, since the above-mentioned particles are formed by the mutual fusion of the incomplete cross-linked structure and the complete cross-linked structure formed by sodium alginate and calcium ions, and the pores of these structures are used to wrap the content, and no adhesive is needed, the use of alcohol-soluble essence for perfuming will not affect the granulation and molding; at the same time, as described above, when water-soluble essence is used, the adsorption and retention sites of the essence are more, so the volatilization loss of the essence during the subsequent drying process is not enough to affect the subsequent normal use; of course, whether there is an adhesive, ester-soluble essence will not affect the molding of the particles.

[0027] Preferably, in order to prevent the problem of bacterial breeding of the particles after perfuming, the filtered and washed particles are mixed with a chitosan aqueous solution with a mass concentration of 1%-5% in step ⑤. The pores in the particles can better accommodate the chitosan solution, thereby achieving a better antibacterial effect. Since chitosan is a natural high-molecular polymer, it is relatively stable and will not volatilize even under heating, so it can still have a relatively high storage amount after granulation.

[0028] Preferably, the functional particles are applied in the preparation of a cigarette multi-element composite filter rod, and a plurality of functional particles are directly used as an independent structure in the filter rod to prepare a multi-element filter rod, or the plurality of functional particles are uniformly dispersed in the filter rod tow to be formed together with the filter rod.

[0029] The filter rod tow.

[0030] Beneficial effects:

[0031] The particles prepared by the application have the following advantages:

[0032] The particles described in the application have a three-dimensional network structure in which calcium alginate gel and contents are mixed. Compared with traditional blasting beads that wrap liquid substances inside, the particles are lighter in weight, the single particle is lighter than the traditional particle, and the number of particles per unit weight is more, which is low in use cost for filter rod manufacturers or cigarette enterprises. Since the contents are mostly substances with microporous structures, the particles have good adsorption force for fragrances, the total adsorption amount of the particles is large, and the adsorbed fragrances can be stably retained. The fragrances in the particles are released in turn, and the release of the fragrances forms a gradient, which is light at first and then strong, thereby prolonging the fragrance release time. The particles do not need adhesive, so the use of ester-soluble fragrances and alcohol-soluble fragrances for perfuming will not affect the granulation and molding. When water-soluble fragrances are used, the volatilization loss of the fragrances is not enough to affect the subsequent normal use. DETAILED DESCRIPTION

[0033] The application will be further described below through specific examples.

[0034] Example 1

[0035] The content of the particles described in this example uses light calcium carbonate with a particle size of 200 mesh, which is prepared according to the following steps.

[0036] ① 4g of sodium alginate is added to 796g of pure water, and stirred for 20 min to prepare a sodium alginate solution with a mass concentration of 0.5%;

[0037] viscosity: 170 mPas density: 121.4 g / 100 ml surface tension: 56.5 mN / m; viscosity: 4 mPas density: 105.88 g / 100 ml surface tension: 55 mN / m;

[0038] viscosity: 170 mPas density: 121.4 g / 100 ml surface tension: 56.5 mN / m; viscosity: 4 mPas density: 105.88 g / 100 ml surface tension: 55 mN / m;

[0039] viscosity: 170 mPas density: 121.4 g / 100 ml surface tension: 56.5 mN / m; viscosity: 4 mPas density: 105.88 g / 100 ml surface tension: 55 mN / m;

[0040] viscosity: 170 mPas density: 121.4 g / 100 ml surface tension: 56.5 mN / m; viscosity: 4 mPas density: 105.88 g / 100 ml surface tension: 55 mN / m;

[0041] viscosity: 170 mPas density: 121.4 g / 100 ml surface tension: 56.5 mN / m; viscosity: 4 mPas density: 105.88 g / 100 ml surface tension: 55 mN / m;

[0042] viscosity: 170 mPas density: 121.4 g / 100 ml surface tension: 56.5 mN / m; viscosity: 4 mPas density: 105.88 g / 100 ml surface tension: 55 mN / m;

[0043] viscosity: 170 mPas density: 121.4 g / 100 ml surface tension: 56.5 mN / m; viscosity: 4 mPas density: 105.88 g / 100 ml surface tension: 55 mN / m;

[0044] Example 2

[0045] The content of the granules described in this example uses activated carbon with a particle size of 300 mesh, which is prepared according to the following steps.

[0046] viscosity: 170 mPas density: 121.4 g / 100 ml surface tension: 56.5 mN / m; viscosity: 4 mPas density: 105.88 g / 100 ml surface tension: 55 mN / m;

[0047] viscosity: 170 mPas density: 121.4 g / 100 ml surface tension: 56.5 mN / m; viscosity: 4 mPas density: 105.88 g / 100 ml surface tension: 55 mN / m;

[0048] viscosity: 170 mPas density: 121.4 g / 100 ml surface tension: 56.5 mN / m; viscosity: 4 mPas density: 105.88 g / 100 ml surface tension: 55 mN / m;

[0049]

[0050] viscosity: 929 mPas density: 121.67 g / 100 ml surface tension: 58.3 mN / m;

[0051] viscosity: 929 mPas density: 121.67 g / 100 ml surface tension: 58.3 mN / m;

[0052] viscosity: 929 mPas density: 121.67 g / 100 ml surface tension: 58.3 mN / m;

[0053]

[0054]

[0055]

[0056] Example 3

[0057] The content of the granules described in this example uses microcrystalline cellulose with a particle size of 500 mesh, and is prepared according to the following steps.

[0058]

[0059] viscosity: 4 mPas density: 118.81 g / 100 ml surface tension: 58.3 mN / m;

[0060] viscosity: 170 mPas density: 121.4 g / 100 ml surface tension: 56.5 mN / m;

[0061] ​​​​​IV. The microcrystalline cellulose / sodium alginate emulsion is delivered to the liquid substance granulating nozzle at a specified volume and frequency by a pneumatic diaphragm pump, and the emulsion is sprayed from the liquid substance granulating nozzle into the molding liquid in a certain particle size by a 1HZ pulse airflow generated by a pulse air pump, the distance between the outlet end of the liquid substance granulating nozzle and the liquid level of the molding liquid is 1.0 cm, the emulsion particles enter the water-soluble calcium salt solution to form particles, and the average particle size of the particles is 0.83 mm;

[0062] V. The filtered and cleaned particles are soaked in clean water for 10 min;

[0063] VI. The filtered particles are dried, sieved, and then mixed with a chitosan aqueous solution with a mass concentration of 1%-5% and dried again;

[0064] VII. The particles are added with ester-soluble flavoring essence and mixed uniformly according to a mass ratio of 1:1 to obtain functional particles.

[0065] Obviously, the above-mentioned embodiments of the present application are only examples for clearly illustrating the present application, and are not intended to limit the embodiments of the present application. Based on the above description, other different forms of changes or variations can be made by those skilled in the art. Here, all the embodiments cannot be exhausted. Any obvious changes or variations derived from the technical solutions of the present application are still within the protection scope of the present application.

[0066] The corresponding pretreated contents in Examples 1-3 are granulated by fluidized bed granulation process, wet granulation process and dry granulation process respectively, and the retention amount of flavoring substances of the obtained particles after being added with flavoring essence in different systems is compared with that of traditional particles:

[0067]

[0068] Conclusion: The functional particles prepared by the present application have obvious improvement in the application scope of flavoring essence, retention of flavoring essence and prevention of volatile loss.

Claims

1. A functional particle for use in a multi-component flavor and fragrance system, characterized by: The functional particles are a composite structure, including an outer three-dimensional mesh wrapping layer, an inner three-dimensional grid body, and pre-treated contents uniformly distributed in the inner three-dimensional grid body; the outer three-dimensional mesh wrapping layer is composed of interconnected calcium alginate colloid particles, and the inner three-dimensional grid body is formed by interconnected calcium alginate gel; the outer three-dimensional mesh wrapping layer includes an incomplete cross-linking structure formed by the combination of a sodium alginate molecule and a calcium ion, and a complete cross-linking structure formed by the combination of two sodium alginate molecules and a calcium ion, and the wrapping layer composed of the incomplete cross-linking structure and the complete cross-linking structure has a plurality of holes with a certain diameter; the inner The three-dimensional grid body is composed of a completely cross-linked structure formed by two sodium alginate molecules and a calcium ion. The degree of cross-linking and stretching are greater than that of the outer shell, and the pores between them are filled with pretreated contents; the pretreated contents are substances with a particle size of 150-500 mesh and are insoluble or difficult to dissolve in water; the particle size of the final functional particles is 18-50 mesh; the main storage parts of the liquid flavor in the particles include the incompletely cross-linked structure and the completely cross-linked structure in the three-dimensional network wrapping layer outside the particles, the remaining part of the pores of the completely cross-linked structure in the internal three-dimensional grid body after accommodating the pretreated contents, and the pores of the contents themselves.

2. The functional particles for use in multi-component flavors and fragrances according to claim 1, characterized in that: The pretreatment content is an inorganic non-metallic powder with a large pore volume and no water-soluble calcium salt, including any one of microcrystalline cellulose, micropowder silica gel, light calcium carbonate, diatomaceous earth, montmorillonite, and activated carbon.

3. A method for preparing the functional particles for use in multi-component flavors and fragrances according to claim 1 or 2, characterized in that: The following steps are involved: ① Prepare sodium alginate solution; use high viscosity sodium alginate, the viscosity is controlled at 100mpas-670mpas, 0.5%<concentration<1.0%; ② Prepare a water-soluble calcium salt solution; use a 5%-20% calcium chloride solution with a viscosity of 4 mPas, a density of 100 g / 100 ml - 120.81 g / 100 ml, and a surface tension of 45-60 mN / m. ③ Process the pretreated contents into a 150-500 mesh powder and add it to the sodium alginate solution in a weight ratio of 1:2-1:

5. Mix well to form an emulsion with a viscosity of 170-930 mpas, a density of 110g / 100ml-125g / 100ml, and a surface tension of 55-60mN / m. ④ The emulsion obtained in step ③ is delivered to the liquid material granulation nozzle by a pneumatic diaphragm pump according to the specified capacity and frequency, and the pulse airflow generated by the pulse air pump is used to spray the emulsion from the liquid material granulation nozzle into the forming liquid at a certain particle size and frequency, wherein the distance between the outlet end of the liquid material granulation nozzle and the liquid surface of the forming liquid is greater than 0 cm and less than 2 cm, and the emulsion particles enter the water-soluble calcium salt solution to form particles; ⑤ Filter and clean the particles prepared in step ④ and soak them in clean water for 10-20 minutes; ⑥ The filtered particles are dried and sieved; ⑦ Add fragrance to the granules to obtain functional granules.

4. The method according to claim 3, characterized in that: In step 7, the flavoring is performed by adding liquid flavor to the particles, mixing them evenly in a mass ratio of 1:1, and then drying them at a low temperature of 40-50° C. to obtain functional particles; the liquid flavor includes water-soluble flavor, alcohol-soluble flavor and ester-soluble flavor.

5. The method according to claim 3 or 4, characterized in that: In step ⑤, the filtered and cleaned particles are mixed evenly with a chitosan aqueous solution having a mass concentration of 1%-5%.

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