CN115316705A - Preparation method of colored slow-release fragrant bead, product and application thereof - Google Patents

Abstract

The invention provides a preparation method of colored slow-release incense beads, products and applications thereof. The preparation method comprises the following steps: mixing inorganic materials, ionic surfactants and water, stirring, and filtering to dryness to obtain a first material; The first material, thickener, pigment, auxiliary agent and water are mixed to obtain a suspension; the suspension is added dropwise to the calcium salt solution and placed to obtain a second material; the second material is washed and calcined in sequence, Obtaining visualized granules; mixing the visualized granules with essence and/or fragrance to obtain the colored slow-release fragrance beads. The colored slow-release fragrance beads provided by the invention have good appearance effect, high particle size and uniformity, low crushing rate, high product quality, high biological safety and good fragrance effect.

Description

A preparation method of colored slow-release fragrance beads and its products and applications

technical field

The invention belongs to the field of cigarette manufacturing, and in particular relates to a preparation method of colored slow-release fragrance beads and its product and application.

Background technique

With the promotion of tar reduction and harm reduction work, the tar content of cigarette smoke continues to decrease, and the requirements for cigarette flavoring and flavoring technology are getting higher and higher, which leads to the rapid development of research and development of filter flavoring and flavoring methods, including Perfuming technologies such as tow flavoring, incense thread, popping beads, dripping pills, microcapsules, and nanoparticles have been developed and applied. However, these technologies have certain disadvantages, such as poor long-term storage aroma stability of tow and incense sticks, high cost of pop-up beads and dripping pills and the introduction of other bad smells, and the safety of microcapsules and nanoparticles inhaled into the lungs. Hidden danger.

For this reason, the industry has recently developed a new technology of flavor slow-release particles, such as flavor slow-release agent particles for cigarette filters (201510300776.X, 201610488221.7), porous solid flavor beads for cigarettes (201910888311.9), large particle solid flavor beads cigarette filter sticks (201810886849.1, 2018000887493.3, 201810887483.X, 2019000314422.9, 201910314412.5, 201810885888.X, 201811016014.7), etc.

However, there are some defects in the existing aroma slow-release granule manufacturing technology: (1) adopt common extrusion method, spray drying method, pelletizing machine granulation method etc. to carry out granulation, the particle size of the gained granule is smaller, the roundness is lower , the hardness is slightly worse; if the particle size or roundness is to be increased, the production cycle will be greatly extended, and if the particle hardness is to be ensured, the density will increase and the essence adsorption capacity will decrease; (2) the improved large particle granulation method is adopted, although the obtained particle The particle size and roundness are obviously improved, but the production cycle is as long as 2-4 days, and the batch preparation capacity is weak. In addition, the particles prepared in the prior art have dull color, or colorless/light color, or poor color uniformity, so the appearance is not good, and they are not suitable for making visible filters.

On the other hand, with the continuous improvement of people's living standards, consumers are now paying more and more attention to the visual enjoyment of products while pursuing the smell of smoke and physical satisfaction. Therefore, how to better highlight the individuality of product aroma and appearance and attract consumers' attention has become an important consideration for new products.

Therefore, how to provide a filter-tip flavoring and flavoring product that can better highlight the product's aroma and appearance, and has a simple and fast preparation process has become an urgent problem to be solved.

Contents of the invention

Aiming at the deficiencies of the prior art, the object of the present invention is to provide a preparation method of colored slow-release fragrance beads and its products and applications. The colored slow-release fragrance beads provided by the invention are uniform, intuitively visible in particle size, full in roundness, and bright in color. The visualized particles endow the product with distinct characteristics and match with the aroma characteristics to strengthen consumers' awareness of the product's aroma; and the aroma is released evenly and gently, without introducing bad smell and increasing the hazard of smoke.

To achieve this purpose of the invention, the present invention adopts the following technical solutions:

In a first aspect, the present invention provides a method for preparing colored slow-release fragrance beads, the preparation method comprising the following steps:

(1) mixing the inorganic material, the ionic surfactant and water, stirring, and drying to obtain the first material;

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

(3) Add the suspension obtained in step (2) dropwise into the calcium salt solution, and place it to obtain the second material;

(4) Washing and calcining the second material obtained in step (3) in sequence to obtain visualized particles;

(5) Mixing the visualized granules obtained in step (4) with essence and/or spices to obtain the colored slow-release fragrance beads.

The above method adopts the method of adding the suspension liquid to the calcium salt solution dropwise, so that the suspension liquid droplets expand and solidify into particles. The solidified particles not only have a higher porosity than the agitated granulation adsorption material, but also facilitate The storage and slow release of fragrance components; and the expansion and solidification operation also leaves room for the addition of other materials, and other materials without adsorption pores can also build particle pores during the particle expansion process, thereby reducing the addition The influence of other substances on the slow-release effect of the granule fragrance; the final product prepared has good appearance, high particle size and uniformity, low crushing rate, high product quality, high biological safety, and good fragrance effect; at the same time, the preparation The method is simple and easy to operate, and the time period for manufacturing spherical particles is much shorter than the existing method.

The use of ionic surfactants to modify inorganic materials can greatly enhance the adsorption capacity of the materials for pigments, making them less likely to be eluted and faded, thus giving the particles the required bright colors and maintaining long-term stability.

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

Preferably, the bentonite includes any one or a combination of at least two of montmorillonite, clay or modified bentonite.

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

Preferably, in step (1), the ionic surfactant includes cetyltrimethylammonium bromide, dodecyltrimethylammonium bromide, double octadecyldimethylammonium bromide or Any one or a combination of at least two of cetyl dimethyl ethyl ammonium bromide.

In the present invention, in step (1), the mass ratio of the inorganic material and 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.).

Preferably, in step (1), the sum of the mass of the inorganic material and the ionic surfactant is 1g, and the volume of water is 5-20mL (such as 5mL, 7mL, 9mL, 11mL, 13mL, 15mL , 17mL, 19mL, 20mL, etc.).

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

Preferably, in step (1), water washing is also included before the filtering.

In the present invention, in step (2), the thickener includes a food-grade thickener.

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

Preferably, in step (2), the pigment includes food-grade pigment.

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

In the present invention, by adding auxiliary agents such as soda powder, starch, cellulose, etc., the viscosity of the suspension can be adjusted, thereby adjusting the appearance and hardness of the particles; combined with the subsequent calcination treatment, the adsorption performance of the particles can be improved, adding Fragrance intensity and sustained release ability are improved.

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.).

Preferably, in step (2), the mass ratio of the first material to 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, more preferably (50-200):1.

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

In the present invention, in step (3), the mass concentration of the calcium salt solution is 0.5-15% (such as 0.5%, 1%, 3%, 5%, 7%, 9%, 11%, 13% %, 15%, etc.).

Preferably, the calcium salt comprises calcium chloride.

Preferably, in step (3), the rate of said dropping is 10-120 drops/minute (for example can be 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.), the volume of each drop of suspension is 0.04-0.1mL (For example, it can be 0.04mL, 0.05mL, 0.06mL, 0.07mL, 0.08mL, 0.09mL, 0.1mL, etc.). Preferably, in step (3), the standing time is at least 30 minutes (for example, 30 minutes, 40 minutes, 50 minutes, 60 minutes, 70 minutes, 80 minutes, 90 minutes, etc.).

In the present invention, in step (4), the temperature of the calcination is 900-1500°C (such as 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.).

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

Preferably, in step (5), the fragrance includes synthetic fragrances and/or plant extracts.

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

Preferably, the plant extract comprises rosemary powder.

Preferably, the plant extract is colorless, light-colored or the same or similar to the color of the pigment.

Preferably, in step (5), the specific step of mixing includes spraying the essence on the surface of the visualized particles or immersing the visualized particles in the fragrance solution.

In the second aspect, the present invention provides a colored slow-release fragrance pearl prepared according to the preparation method described in the first aspect.

In a third aspect, the present invention provides an application of the colored slow-release fragrance beads according to the second aspect in the manufacture of cigarettes.

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

(1) By adopting the method of adding the suspension liquid dropwise to the calcium salt solution, the suspension liquid droplets expand and solidify into particles, and the solidified particles not only have higher porosity than the agitated granulation adsorption material, but also have It is conducive to the storage and slow release of fragrance components; and the expansion and curing operation also leaves room for the addition of other materials. Other materials without adsorption pores can also build particle pores during the particle expansion process, thereby reducing The effect of adding other substances on the slow-release effect of the granule fragrance; the final product prepared has good appearance, high particle size and uniformity, low crushing rate, high product quality, high biological safety, and good fragrance 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.

(2) The present invention uses an ionic surfactant to modify the inorganic material, and the particle size, uniformity, and crushing rate of the visualized sustained-release particles obtained after modification meet the requirements, and the color is richer and stable, not easy to fade, and biologically safe Higher sexiness, not too much negative impact on aroma quality.

(3) In the present invention, by adding additives such as soda powder, starch or cellulose, the viscosity of the suspension can be adjusted, so that the appearance and hardness of the particles can be adjusted; combined with the subsequent calcination treatment, the adsorption properties of the particles can be improved. Enhanced, improved flavoring intensity and sustained release capacity.

(4) The colored slow-release fragrance beads provided by the present invention are uniform, intuitively visible in particle size, full in roundness, and bright in color. Visible particles give the product distinctive features, and match with the fragrance characteristics to strengthen consumers' awareness of product fragrance; and The aroma is released evenly and smoothly, without introducing bad smell and increasing the hazard of smoke. Therefore, through good aroma slow-release ability and outstanding aroma intensity, as well as the correlation between color and aroma characteristics, and visually strengthen the memory of taste, to strengthen the aroma characteristics and personalized characteristics of new products, not only to overcome the increasingly serious homogeneity of market products The goal of the problem, and can give consumers a better product experience and increase the added value of the product.

Description of drawings

Fig. 1 is the appearance diagram of the colored slow-release fragrance beads provided in Example 1.

Figure 2 is an appearance view of the colored slow-release fragrance beads provided in Example 2.

Fig. 3 is an appearance diagram of the colored slow-release fragrance beads provided in Example 3.

Fig. 4 is the external appearance diagram of the colored slow-release fragrance beads comparative sample provided in Comparative Example 1.

Fig. 5 is the external appearance diagram of the colored slow-release fragrance beads comparative sample provided in Comparative Example 2.

Fig. 6 is the external appearance diagram of the colored slow-release fragrance beads comparative sample provided in comparative example 3.

Fig. 7 is a schematic structural view of the visualized filter-tipped cigarettes produced in the sensory evaluation.

Fig. 8 is an appearance diagram of a visualized filter cigarette produced in sensory evaluation.

Detailed ways

The technical solutions of the present invention will be further described below through specific embodiments. It should be clear to those skilled in the art that the embodiments are only for helping to understand the present invention, and should not be regarded as specific limitations on the present invention.

In the following examples, the orange pigment was purchased from Jiangsu Yiheyuan Biotechnology Co., Ltd., the bright blue pigment was purchased from Jiangsu Yiheyuan Biotechnology Co., Ltd., the red pigment was purchased from Wilton, and CTAB was purchased from Shanghai Boao Biotechnology Co., Ltd. Technology Co., Ltd., fragrances and essential oils were purchased from Shenzhen Bolton Fragrance Co., Ltd.

Example 1

This embodiment provides a kind of colored slow-release fragrance beads, the preparation method is as follows:

(1) Mix montmorillonite and CTAB powder uniformly at a mass ratio of 10:1 to obtain a solid mixture; then mix the solid mixture with water at a solid-to-liquid ratio of 1:10 (g:mL), Stir for 4 h, wash with water several times, and filter to dry to obtain the first material.

(2) Sodium alginate (the mass ratio of the first material and sodium alginate is 10:1) is dissolved in water to obtain an aqueous solution of sodium alginate; in addition, the first material is dispersed with water to form a suspension containing the first material, and then This suspension containing the first material is mixed with sodium alginate aqueous solution; Then add orange pigment (the mass ratio of the first material and orange pigment is 150:1) and auxiliary agent soda powder (the mass ratio of the first material and soda powder The mass ratio is 20:1) and stirred evenly to obtain a suspension.

(3) Drop the suspension into an aqueous solution containing 8% (m/V) CaCl ₂ (60 drops/min, the volume of each drop is 0.08mL), leave it for 40 minutes and take it out to obtain the second material;

(4) Rinse the second material with water several times, and calcinate the rinsed second material at 1000°C for 2 hours to obtain visualized particles;

(5) The visualized granules are sprayed with sweet orange oil and dried in the shade to obtain colored slow-release fragrance beads. Its appearance is shown in Figure 1.

Example 2

This embodiment provides a kind of colored slow-release fragrance beads, the preparation method is as follows:

(1) Mix kaolin and hexadecyldimethylethylammonium bromide uniformly at a mass ratio of 5:1 to obtain a solid mixture; then use a solid-to-liquid ratio of 1:20 (g:mL) The solid mixture was mixed with water, stirred for 2 h, washed several times with water, and filtered to obtain the first material.

(2) Gum Arabic (the mass ratio of the first material and gum Arabic is 5:1) is dissolved in water to obtain an aqueous solution of gum Arabic; in addition, the first material is dispersed with water to form a suspension containing the first material, and then the containing The suspension of the first material is mixed with the gum arabic aqueous solution; Then add the bright blue pigment (the mass ratio of the first material and the bright blue pigment is 30:1) and auxiliary starch (the mass ratio of the first material and the starch 10:1) and stirred evenly to obtain a suspension.

(3) Drop the suspension into an aqueous solution containing 0.5% (m/V) CaCl ₂ (10 drops/min, the volume of each drop is 0.1 mL), and take it out after standing for 50 minutes to obtain the second material;

(4) Rinse the second material with water several times, and calcinate the rinsed second material at 900°C for 3 hours to obtain visualized particles;

(5) Spray the visualized granules with wolfberry oil, and dry in the shade to obtain colored slow-release fragrance beads. Its appearance is shown in Figure 2.

Example 3

This embodiment provides a kind of colored slow-release fragrance beads, the preparation method is as follows:

(1) Mix illite and bis-octaalkyldimethylammonium bromide uniformly at a ratio of 20:1 by mass to obtain a solid mixture; The solid mixture was mixed with water, stirred for 6 h, washed several times with water, and filtered to obtain the first material.

(2) Dissolving cyclodextrin (the mass ratio of the first material to cyclodextrin is 20:1) in water to obtain an aqueous solution of cyclodextrin; and dispersing the first material with water to form a suspension containing the first material, and then Mix the suspension containing the first material with the cyclodextrin aqueous solution; then add red pigment (the mass ratio of the first material to the red pigment is 200:1) and auxiliary agent cellulose (the mass ratio of the first material to the cellulose The mass ratio is 2:1) and stirred evenly to obtain a suspension.

(3) Drop the suspension into an aqueous solution containing 15% (m/V) CaCl ₂ (120 drops/min, the volume of each drop is 0.04mL), leave it for 60 minutes and take it out to obtain the second material;

(4) Rinse the second material with water several times, and calcinate the rinsed second material at 1500° C. for 1 hour to obtain visualized particles;

(5) The visualized granules are soaked in a sucralose solution and dried in the shade to obtain colored slow-release fragrance beads. Its appearance is shown in Figure 3.

Example 4

This embodiment provides a kind of colored slow-release fragrance beads, and the only difference from Example 1 is that in step (3), except that the dropping parameters are 160 drops/minute, and the volume of each drop is 0.14mL, the rest are the same as in Example 1. unanimous.

Comparative example 1

This comparative example provides a comparison sample of colored slow-release fragrance beads, which is prepared by a common granulation method, and the preparation method is as follows:

Mix montmorillonite with sodium alginate, sodium carbonate, and water (the ratio of each material is consistent with that of Example 1, and the amount of water added is to make the slurry into a paste) to obtain a slurry; the mixture is stirred by stirring granulation method 2h, and then granulated on a swing granulator; the obtained granules were soaked in an orange pigment solution, dried, and then mixed with menthol to obtain the colored slow-release fragrance pearl comparison sample. Its appearance is shown in Figure 4.

Comparative example 2

This comparative example provides a kind of colored slow-release fragrance beads comparative sample, which is prepared by spherical mold compression molding method, and the preparation method is as follows:

Mix and grind montmorillonite with sodium alginate, sodium carbonate, and water (the ratio of each material is consistent with that of Example 1, and the amount of water added is to make the slurry into a paste) to obtain a slurry; the slurry is sieved, and then the Pour the slurry into a spherical mold and press the mold, first dry at 25°C for 24 hours, then dry at 45°C for 3 hours to obtain spherical embryo bodies; calcinate the spherical embryo bodies at 1300°C for 4 hours to obtain sustained-release granules; The obtained granules are soaked in an orange pigment solution, dried, and then mixed with menthol to obtain the colored slow-release fragrance beads as a comparison sample. Its appearance is shown in Figure 5.

Comparative example 3

The present embodiment provides a kind of coloring slow-release fragrance beads comparison sample, and the difference with embodiment 1 is only, lacks step (1), directly uses montmorillonite as the first material; Step (4) is also different, and step (4) The specific steps are: rinse the second material with water for several times, soak the rinsed second material with 2% (m/V) acetic acid aqueous solution for 30 minutes, then rinse with water for several times, and then dry to obtain visualized particles; Consistent with Example 1. Its appearance is shown in Figure 6.

In embodiment 1-3 product, embodiment 1 (as shown in Figure 1) particle is light orange, embodiment 2 (as shown in Figure 2) particle is green, embodiment 3 (as shown in Figure 3) particle is light red. The appearance of Comparative Example 1 is shown in Figure 4, and the shapes of the products are quite different, not round, and the appearance is poor. The appearance of Comparative Example 2 is shown in Figure 5. Although the roundness and uniformity of the particles are better, the color between the particles is not uniform, most of them are white, some are light yellow to yellow, and the dyeing effect is poor; and the manufacturing cycle is as long as 3 Today, mass production capacity is limited by the number of molds. The appearance of comparative example 3 is shown in Figure 6. Although the roundness and uniformity of the particles are acceptable, the color of the particles is dull and not uniform. Most of the particles are plain, and a small part is light yellow, and the dyeing effect is poor. It can be found that the appearance effect of the product particles of the present invention is better, the particles are round and the difference is small, it can give the product a better color, improve the appearance, and can match the feeling of the type of essence, and improve the user experience.

test case 1

Appearance evaluation: particle size and roundness, particle crushing rate, particle color

The products provided by Examples 1-4 and Comparative Examples 1-3 are evaluated for appearance properties, and the evaluation method is as follows:

(1) Detection method of particle size and roundness: put the colored slow-release fragrance beads and steel ruler on the blue flat plate. Use high-pixel imaging equipment to collect pictures, and then use Image J software to analyze the pictures, so as to obtain the "particle projected area" (mm ² ), the long diameter and short diameter of the particle projection, and then obtain the particle size and roundness—— The particle size is represented by "particle projected area", and the roundness of particles is represented by "circle area ratio"("circle area ratio=projected area/maximum circle area").

(2) Detection method of granule crushing rate: Put the colored slow-release fragrance beads into a box with a cover, and the volume of granules accounts for less than 10% of the volume of the box. After the box cover is closed, put the box into the rotating box, and then use the rotating box method to simulate the possible collision of the particles during storage and transportation according to the YC/T151.2-2001 standard. After the rotation, the particles in the box are taken out and sieved, weighed and calculated the weight difference of the particles before and after the rotation, so as to obtain the crushing rate of the particles during the rotation. The particle hardness and its applicability in production, storage and transportation are evaluated by particle crushing rate.

(3) Color judgment: compare the 24-color standard color card to judge the color of the particles.

The results are shown in Table 1 below:

Table 1

The above data show that the product provided by the present invention can significantly improve the particle size, particle uniformity, roundness and coloring uniformity of the product compared with the ordinary granulation method, reduce the crushing rate, and significantly improve product quality; at the same time, by controlling the dropping parameters It can significantly improve the roundness of the product and improve the appearance effect. In Comparative Example 2, although the appearance and quality of the product are relatively excellent, the color between the particles is not uniform; and the spherical mold compression molding method adopted has a long production cycle and weak batch preparation ability.

From the comparison of Example 1 and Example 4, it can be seen that the dropping parameters will affect the appearance of the particles, and the uniformity and roundness of the particles will be affected.

From the comparison of Example 1 and Comparative Example 3, it can be seen that the coloring effect of the particles will be affected if the ionic surfactant and the calcination treatment are not carried out at the same time, and the color of the particles will obviously become lighter under the same pigment dosage and process conditions.

test case 2

Safety evaluation: detection of smoke components and biosafety evaluation

Put the products provided by Examples 1-3 and Comparative Examples 1-3 (the weight of added particles is between 0.135～0.145g) into cavity filter cigarettes respectively to make visible filter cigarettes (cigarette filter structure is: from Starting from the end of the filter tip, 15mm tow section + 5mm cavity section + 10mm tow section, the colored slow-release fragrance beads are completely filled into the cavity section, the structural diagram is shown in Figure 7, and the appearance is shown in Figure 8), And the smoke components released during burning and smoking of it and the blank sample (without adding any particles, the filter tip is 30mm cellulose acetate filter) were tested, so as to compare and analyze the safety of the visualized particles. The detection method is as follows:

(1) According to GB/T 19609-2004, GB/T 23203.1-2008, GB/T 23355-2009, determine the tar, nicotine and moisture of cigarettes. Then according to 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 determination method , respectively measured the release of 7 harmful components such as CO, benzo[α]pyrene (B[a]P), HCN, NNK, ammonia, phenol and crotonaldehyde in the mainstream smoke of cigarette samples, and according to "Tobacco and Smoke The method described in "Chemical Composition" and the H value of the hazard index of the cigarette sample were calculated by using the Schaefer's formula. Because the physiological satisfaction of different cigarette samples is different, according to the evaluation method of WHO, the unit nicotine value is used to carry out the horizontal comparison of different samples ("a component value of a unit nicotine = the detected value of the component / nicotine value").

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

The analysis results of the impact of particles on the hazards of smoke are shown in Table 2 below:

Table 2

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

Test case 3

Sensory evaluation

Put the products provided by Examples 1-3 and Comparative Examples 1-3 into cavity filter cigarettes respectively to make visible filter cigarettes (cigarette filter structure is: from the end of the filter, 15mm tow section+5mm hollow Cavity section + 10mm tow section, colored slow-release fragrance beads are completely filled into the cavity section, its structural diagram is shown in Figure 7, and its appearance is shown in Figure 8; the blank sample does not add any particles, and the filter tip is 30mm acetate fiber filter). Using the aroma profile analysis method, the above-mentioned cigarettes and blank samples were smoked by personnel with professional cigarette sensory evaluation qualifications, and the results were recorded. Score 13 indicators of smoke characteristics (according to the scoring standard established by YC/T497-2014), and evaluate the flavoring intensity and adaptability. Scores are scored in increments of 0.5 points, using a 10-point system for scoring, and the final results are averaged with 1 decimal place.

Among them: the indicators of the smoke score are based on the quality of the smoke, such as: the lower the concentration of "miscellaneous gas", the higher the score; the higher the "energy" but poor comfort, the lower the score.

In the item "Fragrance Intensity", the more obvious the added fragrance, the higher the score; 1-3 points are perceived, 4-6 points are obvious, and 7-9 points are strong.

The "coordination" index, the better the smoke coordination of the cigarette after the introduction of flavoring, the higher the score, otherwise the score decreases.

The results are shown in Table 3 below:

table 3

The above data show that the product provided by the present invention can effectively improve the quality of smoke, endow cigarettes with more obvious added aroma and aroma, and have no great negative impact on the coordination of smoke. In addition, due to the large amount of adsorption and storage of aroma components in the particles, the intensity of aroma addition is too high during smoking, which affects the coordination of aroma and the quality of smoking evaluation. This can be easily solved by reducing the filling amount of fragrant beads in the filter.

Test case 4

Evaluation of aroma sustained-release ability:

The cigarette samples made by the above sensory evaluation were used as the object (the blank sample was sprayed with tow to carry out filter flavoring), using a rotary smoking machine (manufactured by Borgwaldt KC Instrument, model RM20H, equipped with a puff-by-puff detection module) , with reference to GB/T 19609-2004, GB/T 23203.1-2008, GB/T 23355-2009, to measure the tar, nicotine and moisture on the puff-by-puff smoke trapping filter of cigarettes. Referring again to YC/T 286-2009, the method of sample preparation with the addition of menthol (flavors and fragrances in all particles are replaced with an equal amount of menthol) was used to determine the content of flavor components on the puff-by-puff smoke trapping filter of cigarettes. Using the ratio of the proportion of aroma components (single-mouth aroma component content/total aroma component content) and mouth-to-mouth tar ratio (single mouth tar content/total tar content), the ratio between the flavor release ability of visualized particles and the smoke is analyzed. Matching, the test results are shown in Table 4 below:

Table 4

According to the above data, it can be found that the sustained-release ability of the coloring slow-release fragrance beads provided by the present invention has a good match with the concentration of puff smoke. The ratio is stable in the range of 0.95-1.06, indicating that the slow-release ability of fragrance is good, which meets the requirements of fragrance slow-release materials.

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

Claims (10)

1. a preparation method of colored slow-release fragrance pearl, is characterized in that, described preparation method comprises the following steps: (1) mixing the inorganic material, the ionic surfactant and water, stirring, and drying to obtain the first material; (2) mixing the first material, thickener, pigment, auxiliary agent and water obtained in step (1) to obtain a suspension; (3) Add the suspension obtained in step (2) dropwise into the calcium salt solution, and place it to obtain the second material; (4) Washing and calcining the second material obtained in step (3) in sequence to obtain visualized particles; (5) Mixing the visualized granules obtained in step (4) with essence and/or spices to obtain the colored slow-release fragrance beads. 2. preparation method according to claim 1, is characterized in that, in step (1), described inorganic material comprises any one in bentonite, kaolin, molecular sieve, illite, silicon dioxide or aluminum oxide or A combination of at least two; Preferably, the bentonite comprises any one or a combination of at least two of montmorillonite, clay or modified bentonite; Preferably, in step (1), the ionic surfactant is a cationic surfactant; Preferably, in step (1), the ionic surfactant includes cetyltrimethylammonium bromide, dodecyltrimethylammonium bromide, bis-octyldimethylammonium bromide or Any one or a combination of at least two of cetyl dimethyl ethyl ammonium bromide. 3. the preparation method according to claim 1 or 2, is characterized in that, in step (1), the mass ratio of described inorganic material and ionic surfactant is (5-20): 1; Preferably, in step (1), the volume of water is 5-20 mL based on 1 g of the sum of the mass of the inorganic material and the ionic surfactant; Preferably, in step (1), the stirring time is 2-6h; Preferably, in step (1), water washing is also included before the filtering. 4. according to the preparation method described in any one of claim 1-3, it is characterized in that, in step (2), described thickener comprises food-grade thickener; Preferably, in step (2), the thickener includes any one or a combination of at least two of sodium alginate, gum arabic, cyclodextrin or carrageenan; Preferably, in step (2), the pigment includes food-grade pigment; Preferably, in step (2), the auxiliary agent includes any one or a combination of at least two of soda ash, starch or cellulose. 5. according to the preparation method described in any one of claim 1-4, it is characterized in that, in step (2), the mass ratio of described first material and thickener is (5-20):1; Preferably, in step (2), the mass ratio of the first material to the pigment is (30-300):1; Preferably, in step (2), the mass ratio of the first material to the additive is (2-20):1. 6. The preparation method according to any one of claims 1-5, characterized in that, in step (3), the mass concentration of the calcium salt solution is 0.5-15%; Preferably, the calcium salt comprises calcium chloride; Preferably, in step (3), the dropping rate is 10-120 drops/minute, and the volume of each drop of suspension is 0.04-0.1 mL; Preferably, in step (3), the standing time is at least 30 minutes. 7. The preparation method according to any one of claims 1-6, characterized in that, in step (4), the temperature of the calcination is 900-1500°C, and the time is 1-3h. 8. according to the preparation method described in any one of claim 1-7, it is characterized in that, in step (5), described essence comprises any one in sweet orange oil, wolfberry oil or allyl hexanoate or at least a combination of the two; Preferably, in step (5), the spices include synthetic spices and/or plant extracts; Preferably, the synthetic flavor comprises sucralose and/or vanillin; Preferably, the plant extract comprises rosemary powder; Preferably, in step (5), the specific step of mixing includes spraying the essence on the surface of the visualized particles or immersing the visualized particles in the fragrance solution. 9. A colored slow-release fragrance pearl prepared according to the preparation method according to any one of claims 1-8. 10. An application of the colored slow-release fragrance beads according to claim 9 in the preparation of cigarettes.

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