Cigarette essence blasting bead and preparation method thereof

Abstract

The invention relates to a cigarette essence blasting bead and a preparation method thereof, and belongs to the technical field of essence blasting bead preparation. The prepared hollow mesoporous nano silicon dioxide has a very stable structure, heat resistance and pH value change resistance, the essential oil embedding advantage of the hollow mesoporous nano silicon dioxide is that the hollow cavity provides a storage space for the essential oil, and the hollow mesoporous nano silicon dioxide serving as an inorganic material has higher mechanical strength compared with a high-molecular polymer material, so that the hollow mesoporous nano silicon dioxide can be used for preparing essential oil. Essential oil effective component leakage caused by capsule breakage in the storage process can be prevented, and the retention property, durability and stability of the essential oil are improved; secondly, due to the fact that the pore diameter of mesopores is 2-20 nm, the microcapsule has excellent slow release performance on essence or essential oil, loading and releasing are difficult due to the fact that the pore diameter is too small, and due to the fact that the pore diameter is too large, the microcapsule is inevitably interfered by the external environment more easily, and the slow release performance and the stability of the microcapsule are too poor, and therefore the slow release performance and the stability of the microcapsule are too poor due to the introduction of the mesoporous nano-silica; the slow release performance of the capsule wall material is improved.

Description

Technical Field

[0001] The invention relates to a cigarette flavor bursting bead and a preparation method thereof, belonging to the technical field of flavor bursting bead preparation. Background Art

[0002] In recent years, the market recognition of slim cigarettes has gradually increased. Compared with conventional cigarettes, slim cigarettes have a smaller circumference and lower tar content. At the same time, the reduced amount of tobacco leads to a lower aroma than conventional cigarettes. Flavoring can effectively supplement the aroma of slim cigarettes and make up for the lack of satisfaction caused by the reduction in tobacco use. As a new technology for flavoring cigarettes, the addition of popping beads can enhance the flavor of cigarettes and enrich the taste level. It provides a more direct means of perceptual support for the construction of cigarette categories and has become an important idea for promoting the supply-side structural reform of cigarette products. Although domestic popping bead cigarettes have developed rapidly in recent years and the types of popping beads have become increasingly diverse, there are few research reports on related products, especially wall materials. With the expansion of popping bead cigarettes in the international market, in order to avoid the influence of objective factors such as religious taboos and mad cow disease, the animal gelatin in the popping bead wall material should be replaced with plant glue. At the same time, the popping bead wall material is easy to absorb moisture, which leads to leakage, adhesion, and significant changes in pressure values. The mechanical strength is poor, which is not conducive to the long-distance sea transportation of popping beads or popping bead cigarettes. There are great quality risks. In addition, the sustained-release effect of the essential oil in the popping beads is poor, and it can only be relatively strong in the first few puffs of the cigarette, and may even disappear completely afterwards.

[0003] In view of the above-mentioned defects, the designer actively conducts research and innovation in order to create a cigarette flavor bursting bead and a preparation method thereof, so as to make it more valuable for industrial use. Summary of the invention

[0004] In order to solve the above technical problems, the purpose of the present invention is to provide a cigarette flavor bursting bead and a preparation method thereof.

[0005] A cigarette flavor popping bead of the present invention comprises a popping bead core material and a primary coating layer coated on the surface of the popping bead core material;

[0006] The blasting bead core material comprises hollow mesoporous nano-silica and essential oil;

[0007] The primary coating layer is obtained by coating the surface of the blasting bead core material with a colloid liquid and then drying it;

[0008] The colloidal liquid comprises the following raw materials by weight:

[0009] 15-20 parts of sodium alginate;

[0010] 30-35 parts of pullulan;

[0011] 3-5 parts of modified vegetable gum;

[0012] 0.10-0.15 parts of glycerol;

[0013] 150-200 parts of deionized water;

[0014] The modified vegetable gum is prepared by mixed reaction of agar, gelatin, guar gum, ethanol solution and glutaric anhydride.

[0015] Furthermore, a secondary coating layer is provided on the surface of the primary coating layer.

[0016] The secondary coating layer is formed by modifying the surface of the primary coating core material with polydopamine and then depositing nano-silicon dioxide on the surface.

[0017] A method for preparing cigarette flavor burst beads, the specific preparation steps are:

[0018] (1) mixing the primary coated core material and a dopamine hydrochloride solution with a mass concentration of 5 mg / L at a mass ratio of 1:20, standing at 25-30° C. for 24-48 hours, filtering and separating to obtain a filter residue, and obtaining a polydopamine modified explosive bead rough body;

[0019] (2) γ-aminopropyltriethoxysilane and 95% ethanol solution are mixed at a mass ratio of 1:50 to obtain a coupling agent liquid, nano-silica and the coupling agent liquid are mixed at a mass ratio of 1:100 to obtain a suspension, the above-mentioned polydopamine modified popping beads are added to the suspension at a mass ratio of 1:100, and the reaction is carried out at a constant temperature of 80° C. with magnetic stirring for 8 to 10 hours, wherein 1% of the mass of the suspension of ethylene glycol diglycidyl ether is added when the reaction is carried out for 4 hours. After the reaction is completed, the filter residue is separated by filtration, rinsed with deionized water for 3 to 5 times, and then freeze-dried to finally obtain the tobacco flavor popping beads.

[0020] Furthermore, the preparation steps of the primary coated core material are:

[0021] (1) by weight, 1 to 2 parts of agar, 3 to 5 parts of gelatin, 5 to 10 parts of guar gum and 200 to 300 parts of 70% ethanol solution are weighed and mixed to obtain a mixed solution, the mixed solution and glutaric anhydride are mixed at a mass ratio of 20:1, the pH is adjusted to 7.5, and the mixture is kept warm at 50 to 60° C. for 3 to 5 hours. After the reaction is completed, the residue is separated by filtration to obtain a filter residue, and the residue is rinsed with deionized water for 3 to 5 times to obtain a modified vegetable gum;

[0022] (2) weighing 15 to 20 parts of sodium alginate, 30 to 35 parts of pullulan, 3 to 5 parts of modified vegetable gum, 0.10 to 0.15 parts of glycerol and 150 to 200 parts of deionized water by weight, mixing them, charging them into a reaction kettle, heating them to 75 to 85° C., stirring the sol at a speed of 160 to 200 r / min for 30 to 40 minutes to obtain a colloidal liquid;

[0023] (3) The bead core material and the colloidal liquid are mixed in a mass ratio of 1:10 and stirred for coating. After the coating is completed, the filter residue is separated by filtration and freeze-dried to obtain a primary coated core material.

[0024] Furthermore, the colloidal liquid comprises, by weight, 18 parts of sodium alginate, 33 parts of pullulan, 4 parts of modified vegetable gum, 0.13 parts of glycerol and 180 parts of deionized water;

[0025] After mixing, the mixture is put into a reaction kettle, heated to 80°C, stirred at 180 r / min, and the sol reaction time is 35 min.

[0026] Furthermore, the preparation steps of the popping bead core material are:

[0027] (1) 10 to 15 parts of hexadecyltrimethylammonium bromide are weighed and dissolved in 6000 to 6500 parts of deionized water, 6 to 10 parts of NaOH are added, and the mixture is stirred at 80 to 85° C. and 200 to 250 r / min for 2 to 3 hours, and then 80 to 90 parts of ethyl orthosilicate are added, and the mixture is stirred at 80 to 85° C. and 200 to 250 r / min for 8 to 9 hours. After the reaction, the solution is centrifuged at 8500 r / min, and the precipitate is collected. The surfactant template is washed off with deionized water and anhydrous ethanol, and the mixture is dried in an oven to obtain hollow mesoporous nano-silica;

[0028] (2) The essential oil and the hollow mesoporous nano-silica are mixed in a mass ratio of 100:1 and placed in an ultrasonic oscillator. After ultrasonic oscillation at a frequency of 25 to 35 kHz, the mixture is immersed in the mixture for 10 to 12 hours. After ultrasonic oscillation, the residue is separated by filtration and freeze-dried to obtain the popping bead core material.

[0029] Furthermore, the essential oil is peppermint essential oil.

[0030] By means of the above scheme, the present invention has at least the following advantages:

[0031] (1) The hollow mesoporous nano-silica prepared by the present invention has a very stable structure, is heat-resistant, and is resistant to changes in pH. The advantage of hollow mesoporous nano-silica for embedding essential oils lies in the hollow cavity inside it, which provides storage space for the essential oils. In addition, as an inorganic material, it has higher mechanical strength than high molecular polymer materials, which can prevent the capsule from being damaged during storage and causing leakage of the effective ingredients of the essential oils, thereby improving the retention, durability, and stability of the essential oils. Secondly, since the mesopore diameter is 2-20 nm, it has excellent performance in the sustained release of essences or essential oils. Too small an aperture will lead to difficulties in loading and releasing, while too large an aperture will inevitably lead to microcapsules being more susceptible to interference from the external environment, so that the sustained release performance and stability of the microcapsules are too poor. Therefore, the introduction of mesoporous nano-silica improves the sustained release performance of the capsule wall material.

[0032] (2) The present invention modifies the plant gum raw material by esterification, so that the hydrophilicity of the plant gum becomes weaker, which can prevent the wall material from absorbing water during storage and reduce the hygroscopicity of the wall material. At the same time, after the plant gum is esterified, its lipophilicity is improved, and it can be used to wrap the mesoporous essential oil microspheres once, which can more firmly adsorb the essential oil, improve its wrapping effect, prolong the release time of the essential oil, improve the sustained release effect, and also prevent the leakage of the essential oil, thereby improving its retention, durability and stability;

[0033] (3) The present invention uses a dopamine solution self-polymerization reaction to deposit a layer of polydopamine coating on the surface of the wood. Secondly, under the joint action of silane coupling agent γ-aminopropyl triethoxysilane and epoxy crosslinking agent ethylene glycol diglycidyl ether, nano-silica is fixed on the wood surface in the form of covalent bonds to obtain a surface-modified blasting bead product. Nano-silica is used for surface repair. On the one hand, inorganic silica materials can be used to increase the resistance and strength of the surface of the blasting bead material, thereby improving its retention, durability and stability. On the other hand, nano-silica is used to form surface synapses to increase the surface contact angle of the blasting bead material, thereby improving its waterproofness and avoiding the problem of adhesion caused by moisture absorption of the blasting bead, thereby improving its retention and durability.

[0034] (4) The present invention achieves the best colloid gel quality and improves the waterproof and mechanical properties of the product through a specific raw material ratio; the best plant glue viscosity can be obtained by controlling the specific sol temperature, thereby improving the stability of the glue liquid mixed phase system; and the rheological properties of the glue liquid can be changed by controlling the stirring rate, thereby achieving the best mechanical properties of the glue liquid.

[0035] The above description is only an overview of the technical solution of the present invention. In order to more clearly understand the technical means of the present invention and implement it according to the contents of the specification, the preferred embodiments of the present invention are described in detail as follows. DETAILED DESCRIPTION

[0036] The following examples are used to illustrate the present invention, but are not intended to limit the scope of the present invention.

[0037] Preparation of blasting bead core material:

[0038] (1) 10 to 15 parts of hexadecyltrimethylammonium bromide are weighed and dissolved in 6000 to 6500 parts of deionized water, 6 to 10 parts of NaOH are added, and the mixture is stirred at 80 to 85° C. and 200 to 250 r / min for 2 to 3 hours, and then 80 to 90 parts of ethyl orthosilicate are added, and the mixture is stirred at 80 to 85° C. and 200 to 250 r / min for 8 to 9 hours. After the reaction, the solution is centrifuged at 8500 r / min, and the precipitate is collected. The surfactant template is washed off with deionized water and anhydrous ethanol, and the mixture is dried in an oven to obtain hollow mesoporous nano-silica;

[0039] (2) The essential oil and hollow mesoporous nano-silica are mixed in a mass ratio of 100:1 and placed in an ultrasonic oscillator. After ultrasonic oscillation at a frequency of 25 to 35 kHz, the mixture is immersed in the mixture for 10 to 12 hours. After ultrasonic oscillation, the residue is separated by filtration and freeze-dried to obtain the popping bead core material. The essential oil is peppermint essential oil.

[0040] The hollow mesoporous nano-silica prepared by the present invention has a very stable structure, is heat-resistant, and is resistant to pH changes. The advantage of the hollow mesoporous nano-silica for embedding essential oils lies in the hollow cavity inside it, which provides storage space for the essential oils. Moreover, as an inorganic material, it has higher mechanical strength than high molecular polymer materials, which can prevent the capsule from being damaged during storage and causing leakage of effective components of the essential oils, thereby improving the retention, durability, and stability of the essential oils. Secondly, since the mesopore diameter is 2-20 nm, it has excellent performance in sustained release of essences or essential oils. Too small an aperture will lead to difficulties in loading and releasing, while too large an aperture will inevitably lead to microcapsules being more easily disturbed by the external environment, so that the sustained release performance and stability of the microcapsules are too poor. Therefore, the introduction of mesoporous nano-silica improves the sustained release performance of the capsule wall material.

[0041] Primary coating preparation:

[0042] (3) by weight, 1 to 2 parts of agar, 3 to 5 parts of gelatin, 5 to 10 parts of guar gum and 200 to 300 parts of 70% ethanol solution are weighed and mixed to obtain a mixed solution, the mixed solution and glutaric anhydride are mixed at a mass ratio of 20:1, the pH is adjusted to 7.5, and the mixture is heated at 50 to 60° C. for 3 to 5 hours. After the reaction is completed, the residue is separated by filtration, and the residue is rinsed with deionized water for 3 to 5 times to obtain a modified vegetable gum;

[0043] The present invention modifies the plant gum raw material by esterification, so that the hydrophilicity of the plant gum becomes weaker, which can prevent the wall material from absorbing water during storage and reduce the hygroscopicity of the wall material. At the same time, after the plant gum is esterified and modified, its lipophilicity is improved, and the plant gum is used to wrap the mesoporous essential oil microspheres once, which can more firmly adsorb the essential oil, improve the wrapping effect, prolong the release time of the essential oil, improve the sustained release effect, and also prevent the leakage of the essential oil, thereby improving its retention, durability and stability.

[0044] (4) 15 to 20 parts of sodium alginate, 30 to 35 parts of pullulan, 3 to 5 parts of modified plant gum, 0.10 to 0.15 parts of propylene glycol and 150 to 200 parts of deionized water are weighed by weight, mixed and loaded into a reactor, heated to 75 to 85° C., stirred at a speed of 160 to 200 r / min for 30 to 40 minutes to obtain a colloidal liquid; the present invention achieves the best colloidal gel quality and improves the waterproof and mechanical properties of the product through a specific raw material ratio; the best plant gum viscosity can be obtained by controlling the specific sol temperature, the stability of the mixed phase system of the glue liquid can be improved, and the rheological properties of the glue liquid can be changed by controlling the stirring rate, thereby achieving the best mechanical properties of the glue liquid;

[0045] (5) mixing the bead core material and the colloidal liquid in a mass ratio of 1:10, stirring and coating, filtering and separating to obtain a filter residue after the coating, and freeze-drying to obtain a primary coated core material;

[0046] Secondary coating preparation:

[0047] (6) mixing the primary coated core material and a dopamine hydrochloride solution with a mass concentration of 5 mg / L at a mass ratio of 1:20, standing at 25-30° C. for 24-48 hours, filtering and separating to obtain a filter residue, and obtaining a polydopamine modified explosive bead rough body;

[0048] (7) γ-aminopropyltriethoxysilane and 95% ethanol solution are mixed at a mass ratio of 1:50 to obtain a coupling agent liquid, nano-silica and the coupling agent liquid are mixed at a mass ratio of 1:100 to obtain a suspension, the above-mentioned polydopamine modified popping beads are added to the suspension at a mass ratio of 1:100, and the reaction is carried out at a constant temperature of 80° C. with magnetic stirring for 8 to 10 hours, wherein 1% of the mass of the suspension is added with ethylene glycol diglycidyl ether when the reaction is carried out for 4 hours. After the reaction is completed, the filter residue is separated by filtration, rinsed with deionized water for 3 to 5 times, and then freeze-dried to finally obtain the tobacco flavor popping beads.

[0049] A layer of polydopamine coating is deposited on the surface of the wood by self-polymerization reaction of dopamine solution. Secondly, under the joint action of silane coupling agent γ-aminopropyltriethoxysilane and epoxy cross-linking agent ethylene glycol diglycidyl ether, nano-silica is fixed on the wood surface in the form of covalent bonds to obtain a surface-modified blasting bead product. Nano-silica is used for surface repair. On the one hand, inorganic silica materials can be used to increase the resistance and strength of the surface of the blasting bead material, improve its retention, durability and stability. On the other hand, nano-silica is used to form surface synapses, increase the surface contact angle of the blasting bead material, improve its waterproofness, avoid the problem of adhesion caused by moisture absorption of the blasting beads, and improve its retention and durability.

[0050] Example 1

[0051] (1) 10 parts of hexadecyltrimethylammonium bromide were weighed and dissolved in 6000 parts of deionized water, 6 parts of NaOH were added, and the mixture was stirred at 80°C at a speed of 200-250 r / min for 2 h, and then 80 parts of tetraethyl orthosilicate were added, and the mixture was stirred at 80°C at a speed of 200 r / min for 8 h. After the reaction, the solution was centrifuged at a speed of 8500 r / min, and the precipitate was collected. The surfactant template was washed with deionized water and anhydrous ethanol, and the mixture was dried in an oven to obtain hollow mesoporous nano-silica;

[0052] (2) mixing the essential oil and the hollow mesoporous nano-silica in a mass ratio of 100:1 and placing them in an ultrasonic oscillator, ultrasonically oscillating them at a frequency of 25 kHz for 10 hours, filtering and separating the residue after ultrasonic oscillation, and freeze-drying them to obtain the popping bead core material;

[0053] (3) by weight, 1 part agar, 3 parts gelatin, 5 parts guar gum and 200 parts of 70% ethanol solution were weighed and mixed to obtain a mixed solution, the mixed solution and glutaric anhydride were mixed at a mass ratio of 20:1, the pH was adjusted to 7.5, and the mixture was kept warm at 50° C. for 3 h. After the reaction was completed, the residue was separated by filtration, and the residue was rinsed with deionized water for 3-5 times to obtain a modified vegetable gum;

[0054] (4) 15 parts of sodium alginate, 30 parts of pullulan, 3 parts of modified vegetable gum, 0.10 parts of glycerol and 150 parts of deionized water were weighed, mixed and loaded into a reaction kettle, heated to 75° C., and stirred at a speed of 160 r / min for 30 min to obtain a colloidal liquid;

[0055] (5) Mixing the bead core material and the colloidal liquid at a mass ratio of 1:10 and stirring for coating, filtering and separating to obtain a filter residue after coating, freeze-drying to obtain a primary coated core material, mixing the primary coated core material and a dopamine hydrochloride solution with a mass concentration of 5 mg / L at a mass ratio of 1:20, standing at 25° C. for 24 h, filtering and separating to obtain a filter residue, and obtaining a polydopamine modified bead rough body;

[0056] (6) γ-aminopropyltriethoxysilane and 95% ethanol solution are mixed at a mass ratio of 1:50 to obtain a coupling agent liquid, nano-silica and the coupling agent liquid are mixed at a mass ratio of 1:100 to obtain a suspension, the above-mentioned polydopamine modified popping beads are added to the suspension at a mass ratio of 1:100, and the reaction is carried out at a constant temperature of 80° C. with magnetic stirring for 8 hours, wherein 1% of the mass of the suspension of ethylene glycol diglycidyl ether is added when the reaction is carried out for 4 hours. After the reaction is completed, the filter residue is separated by filtration, rinsed with deionized water 3 times, and then freeze-dried to finally obtain tobacco flavor popping beads.

[0057] Example 2

[0058] (1) 11 parts of hexadecyltrimethylammonium bromide were weighed and dissolved in 6100 parts of deionized water, 7 parts of NaOH were added, and the mixture was stirred at 81°C and 210 r / min for 3 h, and then 82 parts of tetraethyl orthosilicate were added, and the mixture was stirred at 81°C and 210 r / min for 8 h. After the reaction, the solution was centrifuged at 8500 r / min, and the precipitate was collected. The surfactant template was washed with deionized water and anhydrous ethanol, and the mixture was dried in an oven to obtain hollow mesoporous nano-silica;

[0059] (2) mixing the essential oil and the hollow mesoporous nano-silica in a mass ratio of 100:1 and placing them in an ultrasonic oscillator, ultrasonically oscillating them at a frequency of 26 kHz for 10 hours, filtering and separating the residue after ultrasonic oscillation, and freeze-drying them to obtain the popping bead core material;

[0060] (3) by weight, 1 part agar, 3 parts gelatin, 57 parts guar gum and 220 parts of 70% ethanol solution were weighed and mixed to obtain a mixed solution, the mixed solution and glutaric anhydride were mixed at a mass ratio of 20:1, the pH was adjusted to 7.5, and the mixture was kept warm at 52° C. for 3 h. After the reaction was completed, the residue was separated by filtration, and the residue was rinsed with deionized water for 3-5 times to obtain a modified vegetable gum;

[0061] (4) 16 parts of sodium alginate, 31 parts of pullulan, 4 parts of modified vegetable gum, 0.11 parts of glycerol and 160 parts of deionized water were weighed, mixed and loaded into a reaction kettle, heated to 78° C., and stirred at a speed of 170 r / min for 32 minutes to obtain a colloidal liquid;

[0062] (5) Mixing the popping bead core material and the colloidal liquid at a mass ratio of 1:10 and stirring for coating, filtering and separating to obtain a filter residue after the coating is completed, freeze-drying to obtain a primary coated core material, mixing the primary coated core material and a dopamine hydrochloride solution with a mass concentration of 5 mg / L at a mass ratio of 1:20, standing at 26° C. for 28 h, filtering and separating to obtain a filter residue, and obtaining a polydopamine modified popping bead rough body;

[0063] (6) γ-aminopropyltriethoxysilane and 95% ethanol solution are mixed at a mass ratio of 1:50 to obtain a coupling agent liquid, nano-silica and the coupling agent liquid are mixed at a mass ratio of 1:100 to obtain a suspension, the above-mentioned polydopamine modified popping beads are added to the suspension at a mass ratio of 1:100, and the reaction is carried out at a constant temperature of 80° C. with magnetic stirring for 8 hours, wherein 1% of the mass of the suspension of ethylene glycol diglycidyl ether is added when the reaction is carried out for 4 hours. After the reaction is completed, the filter residue is separated by filtration, rinsed with deionized water 3 times, and then freeze-dried to finally obtain tobacco flavor popping beads.

[0064] Example 3

[0065] (1) 13 parts of hexadecyltrimethylammonium bromide were weighed and dissolved in 6300 parts of deionized water, 8 parts of NaOH were added, and the mixture was stirred at 83°C and 230 r / min for 2 h, and then 85 parts of tetraethyl orthosilicate were added, and the mixture was stirred at 83°C and 230 r / min for 8 h. After the reaction, the solution was centrifuged at 8500 r / min, and the precipitate was collected. The surfactant template was washed with deionized water and anhydrous ethanol, and the mixture was dried in an oven to obtain hollow mesoporous nano-silica;

[0066] (2) mixing the essential oil and the hollow mesoporous nano-silica in a mass ratio of 100:1 and placing them in an ultrasonic oscillator, ultrasonically oscillating them at a frequency of 30 kHz for 11 hours, filtering and separating the residue after ultrasonic oscillation, and freeze-drying them to obtain the popping bead core material;

[0067] (3) Weigh 2 parts of agar, 4 parts of gelatin, 8 parts of guar gum and 250 parts of 70% ethanol solution by weight to obtain a mixed solution, mix the mixed solution with glutaric anhydride at a mass ratio of 20:1, adjust the pH to 7.5, and heat at 55° C. for 4 hours. After the reaction is completed, filter and separate to obtain a residue, and rinse with deionized water 4 times to obtain a modified vegetable gum;

[0068] (4) Weigh 18 parts of sodium alginate, 33 parts of pullulan, 4 parts of modified vegetable gum, 0.13 parts of glycerol and 180 parts of deionized water by weight, mix them and put them into a reaction kettle, heat them to 80° C., stir the sol at a speed of 180 r / min for 35 min to obtain a colloidal liquid;

[0069] (5) Mixing the bead core material and the colloidal liquid at a mass ratio of 1:10 and stirring for coating, filtering and separating to obtain a filter residue after coating, freeze-drying to obtain a primary coated core material, mixing the primary coated core material and a dopamine hydrochloride solution with a mass concentration of 5 mg / L at a mass ratio of 1:20, standing at 28° C. for 36 h, filtering and separating to obtain a filter residue, and obtaining a polydopamine modified bead rough body;

[0070] (6) γ-aminopropyltriethoxysilane and 95% ethanol solution are mixed at a mass ratio of 1:50 to obtain a coupling agent liquid, nano-silica and the coupling agent liquid are mixed at a mass ratio of 1:100 to obtain a suspension, the above-mentioned polydopamine modified popping beads are added to the suspension at a mass ratio of 1:100, and the reaction is carried out at a constant temperature of 80° C. with magnetic stirring for 9 hours, wherein 1% of the mass of the suspension of ethylene glycol diglycidyl ether is added when the reaction is carried out for 4 hours. After the reaction is completed, the filter residue is separated by filtration, rinsed with deionized water 4 times, and then freeze-dried to finally obtain tobacco flavor popping beads.

[0071] Example 4

[0072] (1) 14 parts of hexadecyltrimethylammonium bromide were weighed and dissolved in 6400 parts of deionized water, 9 parts of NaOH were added, and the mixture was stirred at 84°C and 240 r / min for 3 h, and then 88 parts of ethyl orthosilicate were added, and the mixture was stirred at 84°C and 240 r / min for 9 h. After the reaction, the solution was centrifuged at 8500 r / min, and the precipitate was collected. The surfactant template was washed with deionized water and anhydrous ethanol, and the mixture was dried in an oven to obtain hollow mesoporous nano-silica;

[0073] (2) mixing the essential oil and the hollow mesoporous nano-silica in a mass ratio of 100:1 and placing them in an ultrasonic oscillator, ultrasonically oscillating them at a frequency of 32 kHz for 11 hours, filtering and separating the residue after ultrasonic oscillation, and freeze-drying them to obtain the popping bead core material;

[0074] (3) 2 parts of agar, 4 parts of gelatin, 9 parts of guar gum and 280 parts of 70% ethanol solution were weighed and mixed to obtain a mixed solution, the mixed solution was mixed with glutaric anhydride at a mass ratio of 20:1, the pH was adjusted to 7.5, and the mixture was kept warm at 58° C. for 4 hours. After the reaction was completed, the residue was separated by filtration, and the residue was rinsed with deionized water 5 times to obtain a modified vegetable gum;

[0075] (4) 19 parts of sodium alginate, 34 parts of pullulan, 4 parts of modified vegetable gum, 0.14 parts of glycerol and 180 parts of deionized water were weighed, mixed and loaded into a reaction kettle, heated to 78° C., and stirred at a speed of 180 r / min for 38 min to obtain a colloidal liquid;

[0076] (5) Mixing the bead core material and the colloidal liquid at a mass ratio of 1:10 and stirring for coating, filtering and separating to obtain a filter residue after coating, freeze-drying to obtain a primary coated core material, mixing the primary coated core material and a dopamine hydrochloride solution with a mass concentration of 5 mg / L at a mass ratio of 1:20, standing at 29° C. for 40 h, filtering and separating to obtain a filter residue, and obtaining a polydopamine modified bead rough body;

[0077] (6) γ-aminopropyltriethoxysilane and 95% ethanol solution are mixed at a mass ratio of 1:50 to obtain a coupling agent liquid, nano-silica and the coupling agent liquid are mixed at a mass ratio of 1:100 to obtain a suspension, the above-mentioned polydopamine modified popping beads are added to the suspension at a mass ratio of 1:100, and the reaction is carried out at a constant temperature of 80° C. with magnetic stirring for 10 hours, wherein 1% of the mass of the suspension of ethylene glycol diglycidyl ether is added when the reaction is carried out for 4 hours. After the reaction is completed, the filter residue is separated by filtration, rinsed with deionized water 5 times, and then freeze-dried to finally obtain tobacco flavor popping beads.

[0078] Example 5

[0079] (1) 15 parts of hexadecyltrimethylammonium bromide were weighed and dissolved in 6500 parts of deionized water, 10 parts of NaOH were added, and the mixture was stirred at 85°C and 250 r / min for 3 h, and then 90 parts of tetraethyl orthosilicate were added, and the mixture was stirred at 85°C and 250 r / min for 9 h. After the reaction, the solution was centrifuged at 8500 r / min, and the precipitate was collected. The surfactant template was washed with deionized water and anhydrous ethanol, and the mixture was dried in an oven to obtain hollow mesoporous nano-silica;

[0080] (2) mixing the essential oil and the hollow mesoporous nano-silica in a mass ratio of 100:1 and placing them in an ultrasonic oscillator, ultrasonically oscillating them at a frequency of 35 kHz for 12 hours, filtering and separating the residue after ultrasonic oscillation, and freeze-drying them to obtain the popping bead core material;

[0081] (3) Weigh 2 parts of agar, 5 parts of gelatin, 10 parts of guar gum and 300 parts of 70% ethanol solution by weight to obtain a mixed solution, mix the mixed solution with glutaric anhydride at a mass ratio of 20:1, adjust the pH to 7.5, and heat at 60° C. for 5 hours. After the reaction is completed, filter and separate to obtain a residue, and rinse with deionized water 5 times to obtain a modified vegetable gum;

[0082] (4) Weigh 20 parts of sodium alginate, 35 parts of pullulan, 5 parts of modified vegetable gum, 0.15 parts of glycerol and 200 parts of deionized water by weight, mix them and put them into a reaction kettle, heat them to 85° C., stir the sol at a speed of 200 r / min for 40 minutes to obtain a colloidal liquid;

[0083] (5) Mixing the bead core material and the colloidal liquid at a mass ratio of 1:10 and stirring for coating, filtering and separating to obtain a filter residue after coating, freeze-drying to obtain a primary coated core material, mixing the primary coated core material and a dopamine hydrochloride solution with a mass concentration of 5 mg / L at a mass ratio of 1:20, standing at 30° C. for 48 h, filtering and separating to obtain a filter residue, and obtaining a polydopamine modified bead rough body;

[0084] (6) γ-aminopropyltriethoxysilane and 95% ethanol solution are mixed at a mass ratio of 1:50 to obtain a coupling agent liquid, nano-silica and the coupling agent liquid are mixed at a mass ratio of 1:100 to obtain a suspension, the above-mentioned polydopamine modified popping beads are added to the suspension at a mass ratio of 1:100, and the reaction is carried out at a constant temperature of 80° C. with magnetic stirring for 10 hours, wherein 1% of the mass of the suspension of ethylene glycol diglycidyl ether is added when the reaction is carried out for 4 hours. After the reaction is completed, the filter residue is separated by filtration, rinsed with deionized water 5 times, and then freeze-dried to finally obtain tobacco flavor popping beads.

[0085] Comparison example

[0086] Comparative Example 1

[0087] The preparation method of this comparative example is basically the same as that of Example 1 of the present invention, except that the hollow mesoporous nano-silica of the present invention is not used to load and encapsulate the essential oil, but the modified plant gum is directly used to encapsulate it. The other preparation processes are the same, and the essential oil bursting beads are also prepared;

[0088] Comparative Example 2

[0089] The preparation method of this comparative example is basically the same as that of Example 1 of the present invention, except that microporous nano-silica is used instead of the hollow mesoporous nano-silica of the present invention to load and encapsulate the essential oil. Other preparation processes are the same, and the essential oil bursting beads are also prepared;

[0090] Comparative Example 3

[0091] The preparation method of this comparative example is basically the same as that of Example 1 of the present invention, except that macroporous nano-silica is used instead of the hollow mesoporous nano-silica of the present invention to load and encapsulate the essential oil. Other preparation processes are the same, and the essential oil bursting beads are also prepared;

[0092] Comparative Example 4

[0093] The preparation method of this comparative example is basically the same as that of Example 1 of the present invention, except that the original plant gum component is used instead of the modified plant gum of the present invention. The other preparation processes are the same, and the flavor bursting beads are also prepared;

[0094] Comparative Example 5

[0095] The preparation method of this comparative example is basically the same as that of Example 1 of the present invention, except that polydopamine and nano-silicon dioxide are not used to prepare the secondary coating layer. Other preparation processes are the same, and flavor burst beads are also prepared;

[0096] The performance test experiments were carried out on Examples 1-5 of the present invention and Comparative Examples 1-5, respectively. The specific test results are shown in Table 2 and Table 3:

[0097] Detection method:

[0098] Waterproof test: weigh 100g of the tested bead wall material, put it in a greenhouse with a relative humidity of 70%, take it out after standing for 24 hours, weigh the weight M of the bead wall material after standing, and calculate the moisture absorption rate of the bead wall material. The moisture absorption rate = (M-100) / 100×100%. The higher the moisture absorption rate, the worse the waterproof property.

[0099] Mechanical strength test: 100 blasting bead wall materials of the same size were randomly selected, and the four key physical indicators of the blasting beads, namely, pressure resistance, strength, indentation and particle size, were tested using a special comprehensive tester for blasting beads. The qualified rate was calculated and converted into scores according to Table 1.

[0100] Sustained release test: Refer to the standards GB / T22838.5-2009 and GB / T22838.15-2009 to screen the cigarette quality and draw resistance of conventional cigarettes. Take out the filter rod in each cigarette filter, put the bursting beads with a particle size of 3.5mm in the filter rod and install the filter rod into the filter (store the bursting beads in a cool place at room temperature for 3 months). The bursting beads are filled at a distance of 15mm from the mouth end. Before smoking conventional cigarettes containing bursting beads of different particle sizes, crush the bursting beads. According to GB / T16450-2004, use the RM20H turntable smoking machine to smoke the test cigarettes, with a smoking capacity of 35mL, a smoking duration of 2s, and a smoking interval of 30s. Each group of cigarettes was smoked five times, and the particulate matter in the mainstream smoke of the cigarettes was collected with a Cambridge filter. After weighing, the Cambridge filter was quickly taken out, and the collector was wiped with absorbent cotton and placed in a stoppered conical flask, and 30 mL of ethanol working solution was added. The collected filter tips were cut along the longitudinal axis and placed in a stoppered conical flask, and the scissors were wiped with absorbent cotton and placed in the conical flask, and 30 mL of isopropanol working solution was added. After the conical flasks were sealed separately, the extraction was oscillated for 30 minutes, and the extract was passed through a needle filter membrane and analyzed by GC-MS. Analytical conditions: Chromatographic column: HP-5MS elastic quartz capillary column (60m×0.25mm×0.25μm); injection volume: 1.0μL; injection port temperature: 250℃; heating program: 50℃ (2min) 4℃ / min250℃ (50min); carrier gas: helium (99.999%); carrier gas control mode: constant flow mode; flow rate: 1.0mL / min; split ratio: 10:1; transmission line temperature: 280℃; ion source temperature: 230℃; quadrupole temperature: 150℃; ionization mode: EI; electron energy: 70eV; scanning mode: SIM; scanning range: 35-550amu; solvent delay: 4min.

[0101] Table 1 Mechanical properties score table of blasting bead wall materials

[0102]

[0103]

[0104] The specific test results are shown in Table 2 and Table 3

[0105] Table 2 Performance test results of the embodiment

[0106]

[0107] It can be seen from the test data in the above table that in Examples 1-5 of the present invention, the moisture resistance and mechanical properties of the flavor bursting beads are gradually improved and then reduced, and reach the optimal value in Example 3. This is because the present invention achieves the best colloid gel quality and improves the waterproof and mechanical properties of the product through a specific raw material ratio, and achieves the best effect under the ratio of Example 3; the optimal plant glue viscosity can be obtained by controlling the specific sol temperature, the stability of the glue mixed phase system is improved, and the rheology of the glue is changed by controlling the stirring rate, thereby achieving the best glue mechanical properties.

[0108] In Examples 1-5, the quality of essential oil suction decreased with the increase of the number of suctions, but each suction had a considerable suction volume, which proved that the bursting beads of the present invention had better sustained release performance and could continuously provide suction fragrance;

[0109] The above test results confirm that the technical solution of the present invention is highly feasible and can be applied in production.

[0110] Table 3 Performance test results of control example

[0111]

[0112] The performance of the control example 1 of the present invention and the embodiment 1 of the present invention are compared. Since the control example 1 does not use the hollow mesoporous nano-silica of the present invention to load and encapsulate the essential oil, but directly uses modified plant gum to coat it, the other preparation processes are the same, and the essence bursting beads are also prepared. The mechanical strength and sustained-release performance of the final bursting beads are significantly reduced. The performance of the control examples 2 and 3 is compared with the embodiment 1 of the present invention. Since the control examples 2 and 3 use microporous nano-silica and macroporous nano-silica instead of the hollow mesoporous nano-silica of the present invention to load and encapsulate the essential oil, the other preparation processes are the same, and the essence bursting beads are also prepared. As a result, the mechanical properties of the final bursting beads are not significantly changed, but the sustained-release performance is reduced compared with that of embodiment 1. This confirms that the present invention The hollow mesoporous nano-silica prepared in the present invention has a very stable structure, is heat-resistant and resistant to pH changes. The advantage of hollow mesoporous nano-silica for encapsulating essential oils lies in the hollow cavity inside it, which provides storage space for the essential oils. Moreover, as an inorganic material, it has higher mechanical strength than high molecular polymer materials, which can prevent the capsule from being damaged during storage and causing leakage of the effective ingredients of the essential oils, thereby improving the retention, durability and stability of the essential oils. Secondly, since the mesopore diameter is 2-20nm, it has excellent performance in the sustained release of flavors or essential oils. Too small an aperture will lead to difficulties in loading and releasing, while too large an aperture will inevitably make the microcapsules more susceptible to interference from the external environment, so that the sustained release performance and stability of the microcapsules are too poor. Therefore, the introduction of mesoporous nano-silica improves the sustained release performance of the capsule wall material.

[0113] Then, the performance of the control example 4 and the embodiment 1 of the present invention are compared. Since the control example 4 uses the original plant gum component instead of the modified plant gum of the present invention, the other preparation processes are the same, and the flavor bursting beads are also prepared, which ultimately leads to the prepared bursting beads, and the moisture resistance and sustained release are reduced. It can be confirmed that the present invention modifies the plant gum raw material by esterification, so that the hydrophilicity of the plant gum is weakened, which can prevent the wall material from absorbing moisture during storage and reduce the hygroscopicity of the wall material. At the same time, after the plant gum is esterified and modified, its lipophilicity is improved, and it is wrapped once for the mesoporous essential oil microspheres, which can more firmly adsorb the flavor essential oil, improve its wrapping effect, prolong the essential oil release time, improve the sustained release effect, and also prevent the leakage of the essential oil, improve its retention, durability and stability;

[0114] Finally, the performance of the control example 5 of the present invention and the embodiment 1 is compared. Since the control example 5 does not use polydopamine and nano-silicon dioxide for secondary coating preparation, other preparation processes are the same, and the flavor bursting beads are also prepared; resulting in significantly reduced moisture resistance and mechanical strength of the final bursting beads, which can confirm that the present invention uses the self-polymerization reaction of dopamine solution to deposit a layer of polydopamine coating on the surface of wood. Secondly, under the joint action of silane coupling agent γ-aminopropyltriethoxysilane and epoxy cross-linking agent ethylene glycol diglycidyl ether, nano-silicon dioxide is fixed to the wood surface in the form of covalent bonds to obtain a surface-modified bursting bead product. Nano-silicon dioxide is used for surface repair. On the one hand, inorganic silica materials can be used to increase the resistance and strength of the surface of the bursting bead material, improve its retention, durability and stability, and on the other hand, nano-silicon dioxide is used to form surface synapses to increase the surface contact angle of the bursting bead material, thereby improving its waterproofness and avoiding the problem of adhesion caused by moisture absorption of the bursting beads, thereby improving its retention and durability.

[0115] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. It should be pointed out that a person skilled in the art can make several improvements and modifications without departing from the technical principles of the present invention, and these improvements and modifications should also be regarded as within the scope of protection of the present invention.

Claims

1. A cigarette flavor bursting bead, characterized by: It includes a blasting bead core material and a primary coating layer coated on the surface of the blasting bead core material; The blasting bead core material comprises hollow mesoporous nano-silica and essential oil; The primary coating layer is obtained by coating the surface of the blasting bead core material with a colloid liquid and then drying it; The colloidal liquid comprises the following raw materials by weight: 15-20 parts of sodium alginate; 30-35 parts of pullulan; 3-5 parts of modified vegetable gum; 0.10-0.15 parts of glycerol; 150-200 parts of deionized water; The modified vegetable gum is prepared by mixed reaction of agar, gelatin, guar gum, ethanol solution and glutaric anhydride.

2. The cigarette flavoring bead according to claim 1, characterized in that: A secondary coating layer is also provided on the surface of the primary coating layer; The secondary coating layer is formed by modifying the surface of the primary coating core material with polydopamine and then depositing nano-silicon dioxide on the surface.

3. A method for preparing cigarette flavor burst beads, characterized in that The specific preparation steps are: (1) mixing the primary coated core material and a dopamine hydrochloride solution with a mass concentration of 5 mg / L at a mass ratio of 1:20, standing at 25-30° C. for 24-48 hours, filtering and separating to obtain a filter residue, and obtaining a polydopamine modified explosive bead rough body; (2) γ-aminopropyltriethoxysilane and 95% ethanol solution are mixed at a mass ratio of 1:50 to obtain a coupling agent liquid, nano-silica and the coupling agent liquid are mixed at a mass ratio of 1:100 to obtain a suspension, the above-mentioned polydopamine modified popping beads are added to the suspension at a mass ratio of 1:100, and the reaction is carried out at a constant temperature of 80° C. with magnetic stirring for 8 to 10 hours, wherein 1% of the mass of the suspension of ethylene glycol diglycidyl ether is added when the reaction is carried out for 4 hours. After the reaction is completed, the filter residue is separated by filtration, rinsed with deionized water for 3 to 5 times, and then freeze-dried to finally obtain the tobacco flavor popping beads.

4. The method for preparing cigarette flavor burst beads according to claim 3, characterized in that: The preparation steps of the primary coated core material are: (1) by weight, 1 to 2 parts of agar, 3 to 5 parts of gelatin, 5 to 10 parts of guar gum and 200 to 300 parts of 70% ethanol solution are weighed and mixed to obtain a mixed solution, the mixed solution and glutaric anhydride are mixed at a mass ratio of 20:1, the pH is adjusted to 7.5, and the mixture is kept warm at 50 to 60° C. for 3 to 5 hours. After the reaction is completed, the residue is separated by filtration to obtain a filter residue, and the residue is rinsed with deionized water for 3 to 5 times to obtain a modified vegetable gum; (2) weighing 15 to 20 parts of sodium alginate, 30 to 35 parts of pullulan, 3 to 5 parts of modified vegetable gum, 0.10 to 0.15 parts of glycerol and 150 to 200 parts of deionized water by weight, mixing them, charging them into a reaction kettle, heating them to 75 to 85° C., stirring the sol at a speed of 160 to 200 r / min for 30 to 40 minutes to obtain a colloidal liquid; (3) The bead core material and the colloidal liquid are mixed in a mass ratio of 1:10 and stirred for coating. After the coating is completed, the filter residue is separated by filtration and freeze-dried to obtain a primary coated core material.

5. The method for preparing cigarette flavor burst beads according to claim 4, characterized in that: The colloidal liquid comprises, by weight, 18 parts of sodium alginate, 33 parts of pullulan, 4 parts of modified vegetable gum, 0.13 parts of glycerol and 180 parts of deionized water; After mixing, the mixture is put into a reaction kettle, heated to 80°C, stirred at 180 r / min, and the sol reaction time is 35 min.

6. The method for preparing cigarette flavor burst beads according to claim 4, characterized in that: The preparation steps of the popping bead core material are: (1) 10 to 15 parts of hexadecyltrimethylammonium bromide are weighed and dissolved in 6000 to 6500 parts of deionized water, 6 to 10 parts of NaOH are added, and the mixture is stirred at 80 to 85° C. and 200 to 250 r / min for 2 to 3 hours, and then 80 to 90 parts of ethyl orthosilicate are added, and the mixture is stirred at 80 to 85° C. and 200 to 250 r / min for 8 to 9 hours. After the reaction, the solution is centrifuged at 8500 r / min, and the precipitate is collected. The surfactant template is washed off with deionized water and anhydrous ethanol, and the mixture is dried in an oven to obtain hollow mesoporous nano-silica; (2) The essential oil and the hollow mesoporous nano-silica are mixed in a mass ratio of 100:1 and placed in an ultrasonic oscillator. After ultrasonic oscillation at a frequency of 25 to 35 kHz, the mixture is immersed in the mixture for 10 to 12 hours. After ultrasonic oscillation, the residue is separated by filtration and freeze-dried to obtain the popping bead core material.

7. The method for preparing cigarette flavor burst beads according to claim 6, characterized in that: The essential oil is peppermint essential oil.

Images