A preparation method of colored sustained-release scented beads and its products and applications

Abstract

The present invention provides a preparation method of colored slow-release scent beads, and its products and applications. The preparation method comprises the following steps: mixing an inorganic material, an ionic surfactant and water, stirring, filtering and drying to obtain a first material; mixing the first material, a thickener, a pigment, an auxiliary agent and water to obtain a suspension; dropping the suspension into a calcium salt solution, placing it, and obtaining a second material; washing and calcining the second material in sequence to obtain visualized particles; mixing the visualized particles with essence and / or spices to obtain the colored slow-release scent beads. The colored slow-release scent beads provided by the present invention have good appearance, high particle size and uniformity, low breakage rate, high product quality, high biological safety, and good fragrance effect.

Description

Technical Field

[0001] The invention belongs to the field of cigarette manufacturing, and specifically relates to a preparation method of colored slow-release scent beads and a product and application thereof. Background Art

[0002] With the advancement of tar reduction and harm reduction work, the tar content of cigarette smoke has been continuously reduced, and the requirements for cigarette flavoring and flavoring technology have become increasingly higher, which has led to the rapid development of the research and development of filter flavoring and flavoring methods, including the development and application of flavoring technologies such as tow flavoring, scented wire, popping beads, dripping pills, microcapsules, and nanoparticles. However, these technologies have certain drawbacks, such as the poor long-term storage aroma stability of tow and scented wire flavoring, the high cost of popping beads and dripping pills and the introduction of other unpleasant odors, and the safety risks of microcapsules and nanoparticles being inhaled into the lungs.

[0003] For this purpose, the industry has recently developed new technologies for flavor sustained-release particles, such as flavor sustained-release particles for cigarette filters (201510300776.X, 201610488221.7), porous solid flavor beads for cigarettes (201910888311.9), large-particle solid flavor beads cigarette filter rods (201810886849.1, 2018000887493.3, 201810887483.X, 2019000314422.9, 201910314412.5, 201810885888.X, 201811016014.7), etc.

[0004] However, the existing aroma slow-release granule manufacturing technology has some defects: (1) The granules obtained by ordinary extrusion, spray drying, ball forming machine granulation and the like are small in size, low in roundness and slightly poor in hardness; if the particle size or roundness is to be improved, the production cycle will be greatly extended; if the hardness of the particles is to be guaranteed, the density will increase and the flavor adsorption capacity will decrease; (2) Although the particle size and roundness of the particles obtained by the improved large particle granulation method are significantly improved, the production cycle is as long as 2-4 days and the batch preparation capacity is weak. In addition, the particles prepared by the prior art are dull in color, or colorless / light in color, or have poor color uniformity, so the appearance is poor and is not suitable for making visual filters.

[0005] On the other hand, as people's living standards continue to improve, today's consumers are paying more and more attention to the visual enjoyment of products while pursuing the smell and physiological satisfaction of cigarettes. Therefore, how to better highlight the aroma and appearance personality of the product and attract consumers' attention has become an important consideration for newly launched products.

[0006] Therefore, how to provide a filter flavoring and fragrance-enhancing product that can better highlight the aroma and appearance personality of the product and has a simple and fast preparation process has become a problem that needs to be solved urgently. Summary of the invention

[0007] In view of the deficiencies in the prior art, the object of the present invention is to provide a method for preparing colored sustained-release fragrance beads, as well as a product and application thereof. The colored sustained-release fragrance beads provided by the present invention are uniform, the particle size is intuitively visible, the roundness is full, and the color is bright. The product is endowed with distinctive characteristics through visual particles, and is matched with the fragrance characteristics to enhance consumers' cognition of the product fragrance; and the fragrance release is uniform and smooth, and will not introduce bad odors or increase the harmfulness of smoke.

[0008] In order to achieve the purpose of the invention, the present invention adopts the following technical solutions:

[0009] In a first aspect, the present invention provides a method for preparing colored sustained-release scented beads, the preparation method comprising the following steps:

[0010] (1) mixing an inorganic material, an ionic surfactant and water, stirring, and filtering to obtain a first material;

[0011] (2) mixing the first material obtained in step (1), a thickener, a pigment, an auxiliary agent and water to obtain a suspension;

[0012] (3) adding the suspension obtained in step (2) dropwise to the calcium salt solution and allowing to stand to obtain a second material;

[0013] (4) washing and calcining the second material obtained in step (3) to obtain visualized particles;

[0014] (5) Mixing the visualized particles obtained in step (4) with flavors and / or spices to obtain the colored sustained-release fragrance beads.

[0015] The above method adopts the method of adding suspension droplets into calcium salt solution to make the suspension droplets expand and solidify into particles. The solidified particles not only have a higher porosity than the stirred granulated adsorption material, which is beneficial to the storage and sustained release of the flavor components; the expansion and solidification operation also leaves an operational space for the addition of other materials, and other materials without adsorption pores can also construct particle pores during the particle expansion process, thereby reducing the influence of adding other substances on the particle flavor sustained release effect; the final prepared product has good appearance effect, high particle size and uniformity, low crushing rate, high product quality, high biosafety, and good flavoring effect; at the same time, the preparation method is simple and easy to operate, and the time period for manufacturing spherical particles is much shorter than that of the existing method.

[0016] The use of ionic surfactants to modify inorganic materials can greatly enhance the material's ability to adsorb pigments, making them less likely to be washed away or fade, thereby giving the particles the desired bright color and maintaining long-term stability.

[0017] In the present invention, in step (1), the inorganic material includes any one of bentonite, kaolin, molecular sieve, illite, silicon dioxide or aluminum oxide, or a combination of at least two thereof.

[0018] Preferably, the bentonite includes any one of montmorillonite, white clay or modified bentonite, or a combination of at least two of them.

[0019] Preferably, in step (1), the ionic surfactant is a cationic surfactant.

[0020] Preferably, in step (1), the ionic surfactant comprises any one of hexadecyltrimethylammonium bromide, dodecyltrimethylammonium bromide, dioctadecyldimethylammonium bromide or hexadecyldimethylethylammonium bromide, or a combination of at least two thereof.

[0021] In the present invention, in step (1), the mass ratio of the inorganic material to the ionic surfactant is (5-20):1 (wherein, "5-20" can be 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, etc.).

[0022] Preferably, in step (1), based on the sum of the masses of the inorganic material and the ionic surfactant being 1 g, the volume of water is 5-20 mL (for example, 5 mL, 7 mL, 9 mL, 11 mL, 13 mL, 15 mL, 17 mL, 19 mL, 20 mL, etc.).

[0023] Preferably, in step (1), the stirring time is 2-6 h (for example, 2 h, 2.5 h, 3 h, 3.5 h, 4 h, 4.5 h, 5 h, 5.5 h, 6 h, etc.).

[0024] Preferably, in step (1), the filtering and drying further comprises washing with water.

[0025] In the present invention, in step (2), the thickener comprises a food grade thickener.

[0026] Preferably, in step (2), the thickener comprises any one of sodium alginate, gum arabic, cyclodextrin or carrageenan, or a combination of at least two thereof.

[0027] Preferably, in step (2), the pigment comprises food grade pigment.

[0028] Preferably, in step (2), the auxiliary agent includes any one of baking soda, starch or cellulose, or a combination of at least two of them.

[0029] In the present invention, by adding additives such as baking soda, starch, cellulose, etc., the viscosity of the suspension can be adjusted, thereby adjusting the appearance and hardness of the particles; and combined with the subsequent calcination treatment, the adsorption performance of the particles can be improved, and the fragrance intensity and sustained release ability can be improved.

[0030] In the present invention, in step (2), the mass ratio of the first material to the thickener is (5-20):1 (wherein, "5-20" can be 5, 7, 9, 11, 13, 15, 17, 19, 20, etc.).

[0031] Preferably, in step (2), the mass ratio of the first material and the pigment is (30-300):1 (wherein, "30-300" can be 30, 50, 70, 90, 110, 130, 150, 180, 200, 220, 250, 270, 290, 300, etc.), preferably (30-250):1, and further preferably (50-200):1.

[0032] Preferably, in step (2), the mass ratio of the first material to the auxiliary agent is (2-20):1 (wherein, "2-20" can be 2, 4, 6, 8, 10, 12, 14, 16, 18, 20, etc.).

[0033] In the present invention, in step (3), the mass concentration of the calcium salt solution is 0.5-15% (for example, it can be 0.5%, 1%, 3%, 5%, 7%, 9%, 11%, 13%, 15%, etc.).

[0034] Preferably, the calcium salt comprises calcium chloride.

[0035] Preferably, in step (3), the rate of dripping is 10-120 drops / minute (for example, 10 drops / minute, 20 drops / minute, 30 drops / minute, 40 drops / minute, 50 drops / minute, 60 drops / minute, 70 drops / minute, 80 drops / minute, 90 drops / minute, 100 drops / minute, 110 drops / minute, 120 drops / minute, etc.), and the volume of each drop of suspension is 0.04-0.1 mL (for example, 0.04 mL, 0.05 mL, 0.06 mL, 0.07 mL, 0.08 mL, 0.09 mL, 0.1 mL, etc.). Preferably, in step (3), the standing time is at least 30 min (for example, 30 min, 40 min, 50 min, 60 min, 70 min, 80 min, 90 min, etc.).

[0036] In the present invention, in step (4), the calcination temperature is 900-1500°C (for example, it can be 900°C, 1000°C, 1100°C, 1200°C, 1300°C, 1400°C, 1500°C, etc.), and the time is 1-3h (for example, it can be 1h, 1.2h, 1.4h, 1.6h, 1.8h, 2h, 2.2h, 2.4h, 2.6h, 2.8h, 3h, etc.).

[0037] In the present invention, in step (5), the essence includes any one of sweet orange oil, wolfberry oil or allyl caproate, or a combination of at least two of them.

[0038] Preferably, in step (5), the fragrance comprises synthetic fragrance and / or plant extract.

[0039] Preferably, the synthetic flavor comprises sucralose and / or vanillin.

[0040] Preferably, the plant extract comprises rosemary powder.

[0041] Preferably, the plant extract is colorless, light-colored, or has a color that is the same as or similar to that of the pigment.

[0042] Preferably, in step (5), the specific step of mixing includes spraying the essence onto the surface of the visualized particles or immersing the visualized particles in a fragrance solution.

[0043] In a second aspect, the present invention provides a colored sustained-release scented bead prepared according to the preparation method described in the first aspect.

[0044] In a third aspect, the present invention provides a use of the colored sustained-release fragrance beads according to the second aspect in the preparation of cigarettes.

[0045] Compared with the prior art, the present invention has the following beneficial effects:

[0046] (1) By adopting the method of adding suspension droplets to calcium salt solution, the suspension droplets are expanded and solidified into particles. The solidified particles not only have a higher porosity than the stirred granulated adsorption material, which is beneficial to the storage and sustained release of the flavor components; but also the expansion and solidification operation leaves room for the addition of other materials. Other materials without adsorption pores can also construct particle pores during the particle expansion process, thereby reducing the effect of adding other substances on the sustained release effect of the particle flavor; the final product prepared has good appearance, high particle size and uniformity, low breakage rate, high product quality, high biosafety, and good flavoring effect; at the same time, the preparation method is simple and easy to operate, and the time period for manufacturing spherical particles is much shorter than the existing method.

[0047] (2) The present invention uses an ionic surfactant to modify the inorganic material. The particle size, uniformity and crushing rate of the visualized sustained-release particles obtained after the modification meet the requirements, the color is richer and stable and not easy to fade, the biological safety is higher, and there is not much negative impact on the fragrance quality.

[0048] (3) In the present invention, by adding additives such as baking soda, starch or cellulose, the viscosity of the suspension can be adjusted, thereby adjusting the appearance and hardness of the particles; and combined with the subsequent calcination treatment, the adsorption performance of the particles can be improved, and the fragrance intensity and sustained release ability can be improved.

[0049] (4) The colored slow-release fragrance beads provided by the present invention are uniform, the particle size is intuitively visible, the roundness is full, and the color is bright. The visualized particles give the product a distinct feature, and match the fragrance feature to strengthen consumers' cognition of the product fragrance; and the fragrance release is uniform and gentle, without introducing bad odors or increasing the harmfulness of smoke. Thus, through good fragrance slow-release ability and outstanding fragrance intensity, as well as the association of color and fragrance features, visually strengthening the memory of taste, the fragrance characteristics and personalized characteristics of the new product are strengthened, which not only achieves the goal of overcoming the increasingly serious problem of market product homogeneity, but also can give consumers a better product experience and increase the added value of the product. BRIEF DESCRIPTION OF THE DRAWINGS

[0050] Figure 1 This is the appearance picture of the colored sustained-release fragrance beads provided in Example 1.

[0051] Figure 2 This is the appearance picture of the colored sustained-release fragrance beads provided in Example 2.

[0052] Figure 3 This is the appearance picture of the colored sustained-release fragrance beads provided in Example 3.

[0053] Figure 4 This is the appearance picture of the comparison sample of the colored sustained-release fragrance beads provided in Example 1.

[0054] Figure 5 This is the appearance picture of the comparison sample of the colored sustained-release fragrance beads provided in Example 2.

[0055] Figure 6 This is the appearance picture of the comparison sample of the colored sustained-release fragrance beads provided in Example 3.

[0056] Figure 7 It is a schematic diagram of the structure of the visualized filter cigarette prepared in the sensory evaluation.

[0057] Figure 8 This is a visual image of the appearance of a filter cigarette produced during the sensory evaluation. DETAILED DESCRIPTION

[0058] The technical solution of the present invention is further described below by specific implementation methods. It should be understood by those skilled in the art that the embodiments are only to help understand the present invention and should not be regarded as specific limitations of the present invention.

[0059] In the following examples, orange pigment was purchased from Jiangsu Yiheyuan Biotechnology Co., Ltd., bright blue pigment was purchased from Jiangsu Yiheyuan Biotechnology Co., Ltd., red pigment was purchased from Wilton, CTAB was purchased from Shanghai Bio Biotechnology Co., Ltd., and flavors and essential oils were purchased from Shenzhen Boton Flavors Co., Ltd.

[0060] Example 1

[0061] This embodiment provides a colored sustained-release scented bead, the preparation method of which is as follows:

[0062] (1) Mixing montmorillonite and CTAB powder in a mass ratio of 10:1 to obtain a solid mixture; then mixing the solid mixture with water in a solid-liquid ratio of 1:10 (g:mL), stirring for 4 hours, washing with water for multiple times, and filtering to obtain a first material.

[0063] (2) dissolving sodium alginate (the mass ratio of the first material to sodium alginate is 10:1) in water to obtain a sodium alginate aqueous solution; dispersing the first material with water to form a suspension containing the first material, and then mixing the suspension containing the first material with the sodium alginate aqueous solution; then adding orange pigment (the mass ratio of the first material to the orange pigment is 150:1) and auxiliary agent soda ash (the mass ratio of the first material to the soda ash is 20:1) and stirring evenly to obtain a suspension.

[0064] (3) dropping the suspension into an aqueous solution containing 8% (m / V) CaCl2 (60 drops / min, each drop having a volume of 0.08 mL), leaving it for 40 min, and then taking it out to obtain a second material;

[0065] (4) washing the second material with water for several times, and calcining the washed second material at 1000° C. for 2 h to obtain visualized particles;

[0066] (5) Visualize the particles and spray them with sweet orange oil, and then dry them in the shade to obtain colored slow-release fragrance beads. Figure 1 shown.

[0067] Example 2

[0068] This embodiment provides a colored sustained-release scented bead, the preparation method of which is as follows:

[0069] (1) Kaolin and hexadecyl dimethyl ethyl ammonium bromide are mixed uniformly at a mass ratio of 5:1 to obtain a solid mixture; the solid mixture is then mixed with water at a solid-liquid ratio of 1:20 (g:mL), stirred for 2 hours, washed with water multiple times, and filtered to obtain a first material.

[0070] (2) dissolving gum arabic (the mass ratio of the first material to the gum arabic is 5:1) in water to obtain an arabic gum aqueous solution; dispersing the first material with water to form a suspension containing the first material, and then mixing the suspension containing the first material with the arabic gum aqueous solution; then adding brilliant blue pigment (the mass ratio of the first material to the brilliant blue pigment is 30:1) and auxiliary starch (the mass ratio of the first material to the starch is 10:1) and stirring evenly to obtain a suspension.

[0071] (3) dropping the suspension into an aqueous solution containing 0.5% (m / V) CaCl2 (10 drops / minute, each drop having a volume of 0.1 mL), leaving it for 50 minutes and then taking it out to obtain a second material;

[0072] (4) washing the second material with water for several times, and calcining the washed second material at 900° C. for 3 h to obtain visualized particles;

[0073] (5) Spray the visualized particles with wolfberry oil and dry them in the shade to obtain colored slow-release fragrance beads. Figure 2 shown.

[0074] Example 3

[0075] This embodiment provides a colored sustained-release scented bead, the preparation method of which is as follows:

[0076] (1) Illite and dioctaalkyl dimethyl ammonium bromide are mixed uniformly at a mass ratio of 20:1 to obtain a solid mixture; the solid mixture is then mixed with water at a solid-liquid ratio of 1:5 (g:mL), stirred for 6 hours, washed with water multiple times, and filtered to obtain a first material.

[0077] (2) dissolving cyclodextrin (the mass ratio of the first material to the cyclodextrin is 20:1) in water to obtain a cyclodextrin aqueous solution; dispersing the first material with water to form a suspension containing the first material, and then mixing the suspension containing the first material with the cyclodextrin aqueous solution; then adding red pigment (the mass ratio of the first material to the red pigment is 200:1) and auxiliary cellulose (the mass ratio of the first material to the cellulose is 2:1) and stirring evenly to obtain a suspension.

[0078] (3) dropping the suspension into an aqueous solution containing 15% (m / V) CaCl2 (120 drops / min, each drop having a volume of 0.04 mL), leaving it for 60 min, and then taking it out to obtain a second material;

[0079] (4) washing the second material with water for several times, and calcining the washed second material at 1500° C. for 1 h to obtain visualized particles;

[0080] (5) Visualization: The granules are soaked in sucralose solution and dried in the shade to obtain colored sustained-release fragrance beads. Figure 3 shown.

[0081] Example 4

[0082] This embodiment provides a colored sustained-release scented bead, which is different from the embodiment 1 only in that, in step (3), except that the dripping parameters are 160 drops / minute and the volume of each drop is 0.14 mL, the rest is the same as the embodiment 1.

[0083] Comparative Example 1

[0084] This comparative example provides a comparative sample of colored sustained-release scent beads, which is prepared by a common granulation method. The preparation method is as follows:

[0085] Mix montmorillonite with sodium alginate, sodium carbonate and water (the proportion of each material is the same as that in Example 1, and the amount of water added is such that the slurry becomes a paste) to obtain a slurry; stir the mixture for 2 hours by a stirring granulation method, and then granulate it on a swing granulator; soak the obtained particles in an orange pigment solution, dry them, and then mix them with menthol to obtain the colored slow-release fragrance beads comparison sample. Its appearance is as follows Figure 4 shown.

[0086] Comparative Example 2

[0087] This comparative example provides a comparative sample of colored sustained-release scent beads, which is prepared by a spherical mold compression molding method. The preparation method is as follows:

[0088] Mix montmorillonite with sodium alginate, sodium carbonate and water and grind them (the ratio of each material is consistent with that in Example 1, and the amount of water added is to make the slurry into a paste) to obtain a slurry; sieve the slurry, and then pour the slurry into a spherical mold for compression molding, first dry it below 25°C for 24 hours, and then dry it at 45°C for 3 hours to obtain a spherical embryo; calcine the spherical embryo at 1300°C for 4 hours to obtain slow-release particles; soak the obtained particles in an orange pigment solution, dry them, and then mix them with menthol to obtain the colored slow-release fragrance beads comparison sample. Its appearance is as follows Figure 5 shown.

[0089] Comparative Example 3

[0090] This embodiment provides a comparative sample of colored sustained-release scent beads, which differs from embodiment 1 only in that step (1) is omitted and montmorillonite is directly used as the first material; step (4) is also different, and the specific steps of step (4) are: rinse the second material with water for several times, soak the rinsed second material in a 2% (m / V) acetic acid aqueous solution for 30 minutes, rinse it with water for several times, and then dry it to obtain visualized particles; the rest is the same as embodiment 1. Its appearance is as follows Figure 6 shown.

[0091] In the products of Examples 1-3, Example 1 (such as Figure 1 The particles in Example 2 (as shown) are light orange. Figure 2 The particles are green, and the particles in Example 3 (as shown) are green. Figure 3 The particles are light red. Figure 4 As shown in the figure, the morphology of the products is quite different, and they are not round and have a poor appearance. Figure 5 As shown in the figure, although the particles have good roundness and uniformity, the color of the particles is uneven, most of them are white, and some are light yellow to yellow, and the dyeing effect is poor; and the manufacturing cycle is as long as 3 days, and the mass production capacity is limited by the number of molds. Figure 6 As shown in the figure, although the roundness and uniformity of the particles are acceptable, the color of the particles is dark and uneven, most of the particles are plain, a few are light yellow, and the dyeing effect is poor. It can be found that the particles of the product of the present invention have better appearance, the particles are round and the difference is small, which can give the product a better color and improve the appearance, and can match the type of flavor to enhance the use experience.

[0092] Test Example 1

[0093] Appearance evaluation: particle size and roundness, particle crushing rate, particle color

[0094] The appearance properties of the products provided in Examples 1-4 and Comparative Examples 1-3 were evaluated by the following method:

[0095] (1) Particle size and roundness detection method: Place the colored slow-release fragrance beads and a steel ruler on a blue plate. Use a high-pixel imaging device to collect images, and then use Image J software to analyze the images to obtain the particle "projected area" (mm 2 ), the long diameter and short diameter of the particle projection, and then the particle size and roundness are obtained - the particle size is expressed by "particle projection area", and the particle roundness is expressed by "circle area ratio" ("circle area ratio = projection area / maximum circle area").

[0096] (2) Particle breakage rate test method: Place the colored slow-release fragrance beads in a box with a lid, and the volume of the particles accounts for less than 10% of the volume of the box. After the lid is closed, place the box in a rotating box, and then use the rotating box method according to the YC / T151.2-2001 standard to simulate the collision conditions that the particles may encounter during storage and transportation. After rotation, take out the particles in the box and sieve them, weigh and calculate the weight difference of the particles before and after rotation, so as to obtain the particle breakage rate during the rotation process. The particle breakage rate is used to evaluate the hardness of the particles and their applicability in production, storage and transportation.

[0097] (3) Color determination: Determine the color of the particles by comparing with the 24-color standard color card.

[0098] The results are shown in Table 1 below:

[0099] Table 1

[0100]

[0101] The above data show that the product provided by the present invention can significantly improve the particle size, particle uniformity, roundness and color uniformity of the product, reduce the crushing rate, and significantly improve the product quality compared with the common granulation method; at the same time, by controlling the dropping parameters, the roundness of the product can be significantly improved, and the appearance effect can be improved. Although the product appearance and quality in Comparative Example 2 are also excellent, the color between its particles is uneven; and the spherical mold compression molding method used has a long production cycle and weak batch preparation capability.

[0102] By comparing Example 1 and Example 4, it can be seen that the dropping parameters will affect the appearance of the particles, and both the uniformity and roundness of the particles will be affected.

[0103] By comparing Example 1 and Comparative Example 3, it can be seen that if both the ionic surfactant and the calcination treatment are not performed at the same time, the coloring effect of the particles will be affected. Under the same pigment dosage and process conditions, the color of the particles becomes significantly lighter.

[0104] Test Example 2

[0105] Safety evaluation: smoke composition detection and biosafety evaluation

[0106] The products provided in Examples 1-3 and Comparative Examples 1-3 (the added particle weight is between 0.135 and 0.145 g) are respectively placed in cavity filter cigarettes to prepare visualized filter cigarettes (the cigarette filter structure is: starting from the end of the filter, 15 mm tow segment + 5 mm cavity segment + 10 mm tow segment, the colored slow-release fragrance beads are completely filled into the cavity segment, and the structural schematic diagram is shown as follows Figure 7 As shown, the appearance is as follows Figure 8As shown in the figure, the smoke components released by the smoke sample and the blank sample (without any particles added and the filter tip is 30mm acetate filter) are tested during smoking, so as to compare and analyze the safety of the visualized particles. The test method is as follows:

[0107] (1) According to GB / T 19609-2004, GB / T 23203.1-2008 and GB / T 23355-2009, the tar, nicotine and moisture of cigarettes were measured. Then, according to the measurement methods of GB / T 23356-2009, GB / T 21130-2007, YC / T 253-2019, CRM N°75, YC / T 377-2019, YC / T 255-2008 and YC / T 254-2008, the release of seven harmful components in the mainstream smoke of cigarette samples, including CO, benzo[a]pyrene (B[a]P), HCN, NNK, ammonia, phenol and crotonaldehyde, was measured respectively. The harmfulness index H value of cigarette samples was calculated by using the Xie formula according to the method described in "Chemical Composition of Tobacco and Smoke". Since the physiological satisfaction of different cigarette samples is different, according to the evaluation method of WHO, the unit nicotine value is used to conduct a horizontal comparison of different samples ("value of a certain component per unit nicotine = detection value of the component / nicotine value").

[0108] (2) Conduct biological evaluation of smoke safety according to YQ / T 42-2013, YQ 3-2011 and YQ / T 43-2013.

[0109] The results of the analysis of the impact of particles on the harmfulness of flue gas are shown in Table 2 below:

[0110] Table 2

[0111]

[0112]

[0113] From the above data, it can be found that the colored sustained-release fragrance beads provided by the present invention will not bring negative impact on the cigarette samples, but improve the smoking safety of the cigarette samples to a certain extent. Although the relative release of phenol is increased, the relative release of NNK, ammonia, B[a]P and crotonaldehyde is significantly reduced, and there is also a certain selective reduction effect on CO, so that the unit nicotine H value has a significant decrease, reducing the harmfulness of the smoke; and the 24h cell IC50 of the smoke is significantly higher, indicating that the product can reduce the biological toxicity of the smoke to a certain extent.

[0114] Test Example 3

[0115] Sensory evaluation

[0116] The products provided in Examples 1-3 and Comparative Examples 1-3 were respectively placed in cavity filter cigarettes to prepare visualized filter cigarettes (the cigarette filter structure is: starting from the end of the filter, 15mm tow segment + 5mm cavity segment + 10mm tow segment, the colored slow-release fragrance beads are completely filled into the cavity segment, and the structural schematic diagram is shown as follows Figure 7 As shown, the appearance is as follows Figure 8 As shown; no particles were added to the blank sample, and the filter was a 30mm acetate filter). The aroma profile analysis method was used, and personnel with professional cigarette sensory evaluation qualifications evaluated the above cigarettes and blank samples and recorded the results. Scores were given for 13 indicators of smoke characteristics (according to the scoring standards formulated in YC / T497-2014), and the flavoring intensity and adaptability were evaluated. The scores were scored in increments of 0.5 points, using a 10-point system, and the final results were averaged, with 1 decimal place retained.

[0117] Among them: various indicators of smoke scoring are measured by smoke quality, such as: the lower the concentration of "impurity gas", the higher the score; the stronger the "power" but poor the comfort, the lower the score.

[0118] For the “fragrance intensity” item, the more obvious the external fragrance is, the higher the score; 1 to 3 points are perceptible, 4 to 6 points are obvious external fragrance, and 7 to 9 points are strong external fragrance.

[0119] For the “coordination” index, the better the coordination of cigarette smoke after the introduction of external flavor, the higher the score, and vice versa.

[0120] The results are shown in Table 3 below:

[0121] Table 3

[0122]

[0123] The above data show that the product provided by the present invention can effectively improve the quality of smoke, give cigarettes a more obvious external aroma, and have no significant negative impact on the coordination of smoke. In addition, due to the large amount of aroma components adsorbed and stored by the particles, the aroma intensity is too high during inhalation, which affects the aroma coordination and the quality of inhalation. This can be easily solved by reducing the amount of aroma beads in the filter.

[0124] Test Example 4

[0125] Evaluation of aroma sustained release ability:

[0126] The cigarette samples prepared by the above sensory evaluation were used as the object (the blank sample was flavored by spraying the filter with tow), and a rotary smoking machine (produced by Borgwaldt KC Instrument, model RM20H, equipped with a puff-by-puff detection module) was used to measure the tar, nicotine and moisture on the cigarette puff-by-puff smoke collection filter with reference to GB / T 19609-2004, GB / T 23203.1-2008, and GB / T 23355-2009. Referring to YC / T 286-2009, the content of flavor components on the cigarette puff-by-puff smoke collection filter was measured by adding menthol to the sample (the flavors and fragrances in all particles were replaced with an equal amount of menthol). The ratio of the puff-by-puff flavor component ratio (single puff flavor component content / total flavor component content) to the puff-by-puff tar ratio (single puff tar content / total tar content) was used to analyze the matching of the visualized particle flavor sustained release ability with the smoke. The test results are shown in Table 4 below:

[0127] Table 4

[0128]

[0129] According to the above data, it can be found that the sustained-release ability of the colored sustained-release fragrance beads provided by the present invention is well matched with the smoke concentration at each puff. Except for the first puff (ignition puff), the ratio of the concentration of the fragrance component to the tar concentration is stable in the range of 0.95-1.06, indicating that the fragrance sustained-release ability is good and meets the requirements of the flavor sustained-release material.

[0130] The applicant declares that the present invention illustrates the process method of the present invention through the above-mentioned embodiments, but the present invention is not limited to the above-mentioned process steps, that is, it does not mean that the present invention must rely on the above-mentioned process steps to be implemented. Those skilled in the art should understand that any improvement of the present invention, equivalent replacement of the raw materials selected by the present invention, addition of auxiliary components, selection of specific methods, etc., all fall within the protection scope and disclosure scope of the present invention.

Claims

1. A method for preparing colored sustained-release scented beads, characterized in that: The preparation method comprises the following steps: (1) mixing an inorganic material, an ionic surfactant and water, stirring, and filtering to obtain a first material; The inorganic material includes any one of bentonite, kaolin, molecular sieve, illite, silicon dioxide or aluminum oxide, or a combination of at least two thereof; The mass ratio of the inorganic material to the ionic surfactant is (5-20):1; (2) mixing the first material obtained in step (1), a thickener, a pigment, an auxiliary agent and water to obtain a suspension; The thickener includes any one of sodium alginate, gum arabic, cyclodextrin or carrageenan, or a combination of at least two thereof; The mass ratio of the first material to the thickener is (5-20):1; The mass ratio of the first material to the pigment is (30-300):1; The mass ratio of the first material to the auxiliary agent is (2-20):1; (3) adding the suspension obtained in step (2) dropwise into a calcium salt solution having a mass concentration of 0.5-15%, and allowing to stand to obtain a second material; The dripping rate is 10-120 drops / minute, and the volume of each drop of suspension is 0.04-0.1 mL; (4) washing and calcining the second material obtained in step (3) to obtain visualized particles; (5) Mixing the visualized particles obtained in step (4) with flavors and / or spices to obtain the colored sustained-release fragrance beads.

2. The preparation method according to claim 1, characterized in that: The bentonite includes any one of montmorillonite, white clay or modified bentonite or a combination of at least two of them.

3. The preparation method according to claim 1, characterized in that: In step (1), the ionic surfactant is a cationic surfactant.

4. The preparation method according to claim 1, characterized in that: In step (1), the ionic surfactant includes any one of hexadecyltrimethylammonium bromide, dodecyltrimethylammonium bromide, dioctadecyldimethylammonium bromide or hexadecyldimethylethylammonium bromide, or a combination of at least two thereof.

5. The preparation method according to claim 1, characterized in that: In step (1), the volume of water is 5-20 mL, based on the sum of the mass of the inorganic material and the ionic surfactant being 1 g.

6. The preparation method according to claim 1, characterized in that: In step (1), the stirring time is 2-6 h.

7. The preparation method according to claim 1, characterized in that: In step (1), the filtering and drying also includes washing with water.

8. The preparation method according to claim 1, characterized in that: In step (2), the thickener includes a food grade thickener.

9. The preparation method according to claim 1, characterized in that: In step (2), the pigment includes food grade pigment.

10. The preparation method according to claim 1, characterized in that: In step (2), the auxiliary agent includes any one of baking soda, starch or cellulose, or a combination of at least two of them.

11. The preparation method according to claim 1, characterized in that: The calcium salt includes calcium chloride.

12. The preparation method according to claim 1, characterized in that: In step (3), the standing time is at least 30 min.

13. The preparation method according to claim 1, characterized in that: In step (4), the calcination temperature is 900-1500°C and the calcination time is 1-3 h.

14. The preparation method according to claim 1, characterized in that: In step (5), the essence includes any one of sweet orange oil, wolfberry oil or allyl caproate, or a combination of at least two of them.

15. The preparation method according to claim 1, characterized in that: In step (5), the fragrance includes synthetic fragrance and / or plant extract.

16. The preparation method according to claim 15, characterized in that: The synthetic flavor includes sucralose and / or vanillin.

17. The preparation method according to claim 15, characterized in that: The plant extract includes rosemary powder.

18. The preparation method according to claim 1, characterized in that: In step (5), the specific step of mixing includes spraying the flavor onto the surface of the visualized particles or immersing the visualized particles in a flavor solution.

19. A colored sustained-release scented bead prepared according to the preparation method according to any one of claims 1 to 18.

20. Use of the colored sustained-release fragrance beads according to claim 19 in the preparation of cigarettes.

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