A method for preparing cigarette flavoring beads using a chemical film-forming process

Abstract

The application discloses a method for preparing a smoke burst ball by a chemical film forming method, and comprises the following steps: mixing and stirring essential oil or essence, sodium carboxymethyl cellulose, calcium lactate, gum arabic, ultrapure water, an emulsifying agent and a plasticizer to prepare an emulsion; then dispersing low acyl gellan gum according to a concentration ratio, and dissolving the low acyl gellan gum in the ultrapure water to prepare a forming liquid; dropping the prepared emulsion into the forming liquid and stirring; rinsing the formed wet capsules with deionized water, and separating the wet capsules from the deionized water; dissolving the calcium lactate in the ultrapure water according to a concentration ratio to prepare a solidification liquid; adding the rinsed wet capsules into the solidification liquid and stirring; and drying the rinsed wet capsules in a rotary air drying device to obtain the smoke burst ball. The smoke burst ball prepared by the method has the advantages of wide compatibility of essential oil solvents, low equipment requirement, short dripping process, small essence demand, small essence loss, stable and reliable product quality and the like, and is very suitable for essence research and development and technical updating iteration of the smoke burst ball.

Description

Technical Field

[0001] This invention relates to the field of tobacco flavor capsule preparation technology, and in particular to a method for preparing tobacco flavor capsules by chemical film formation. Background Technology

[0002] Cigarette flavor capsules, as a filter additive, not only improve the flavor of cigarette smoke but also optimize the user experience and enhance brand favorability in the market. The manufacturing process and physical properties of flavor capsules have attracted the attention of major companies. Currently, the main methods for preparing cigarette flavor capsules in the domestic market are physical film-forming methods and chemical film-forming methods.

[0003] Physical film-forming methods are suitable for mass production of flavor capsules, requiring a large initial feed volume. The main physical film-forming processes for cigarette flavor capsules include pulse-cutting and gravity-cutting. In the pulse-cutting process, the essential oil solvent is an olive oil system, while in the gravity-cutting process, it is a caprylic / capric triglyceride system. Due to compatibility issues between the flavor capsule core liquid and the capsule material, neither the pulse-cutting nor gravity-cutting processes can simultaneously be used for flavorings produced with one or more solvents such as olive oil, caprylic / capric triglycerides, propylene glycol, glycerol, ethanol, or water.

[0004] Chemical film-forming methods are suitable for the preparation of small quantities of flavor capsules, offering advantages such as wide compatibility with flavoring solvents, low equipment requirements, short dripping process, low flavoring demand, and minimal flavor loss. This makes them suitable for the research and development of flavorings for tobacco flavor capsules and for technological upgrades. Therefore, developing a new method for preparing tobacco flavor capsules to enrich the production methods of flavor capsules is particularly important. Summary of the Invention

[0005] The purpose of this invention is to provide a chemical film-forming method for preparing tobacco flavoring beads, which solves the problems of existing technologies such as single flavoring solvent, high equipment requirements, long dripping process, large demand for flavoring, easy loss of aroma, and unstable quality of finished product.

[0006] The above-mentioned technical objective of the present invention is achieved through the following technical solution:

[0007] A method for preparing cigarette flavor beads by chemical film formation includes the following steps;

[0008] Step 1: Prepare the emulsion: Mix 70-80 parts essential oil or fragrance, 1-3 parts sodium carboxymethyl cellulose, 2-5 parts calcium lactate, 0.5-2 parts gum arabic, 30-50 parts ultrapure water, 0.1-1 parts emulsifier, and 0.1-0.5 parts plasticizer to prepare the emulsion.

[0009] Step 2: Prepare the molding solution: Disperse the low-acyl gellan gum at a concentration of 0.2% to 0.4% and dissolve it in ultrapure water to prepare the molding solution, and stir at a speed of 10 to 15 rpm.

[0010] Step 3, wet capsule preparation: The prepared emulsion is dripped into the molding liquid of low acyl gellan gum at a rate of 5-8 drops per second, and the dripping is carried out while stirring. After the emulsion has been completely dripped, it is left to stand for 35-40 minutes while maintaining a stirring speed of 5-8 rpm.

[0011] Step 4: Collecting wet capsules: After rinsing the formed wet capsules 2-3 times with deionized water, separate the solid and liquid components.

[0012] Step 5: Preparation of curing solution; Dissolve calcium lactate in ultrapure water at a concentration of 1% to 3%, and keep the dissolved curing solution stirred at a speed of 8 to 12 rpm.

[0013] Step 6, Wet Capsule Curing: Add the rinsed wet capsules to the curing solution and keep stirring at 8-12 rpm for 5-10 minutes. After curing, rinse the wet capsules with deionized water 2-3 times to separate the solid and liquid.

[0014] Step 7, Finished Product Preparation: After rinsing, the wet capsules are placed in a rotary air-drying device and dried for a period of time. After sieving, light sorting and testing, tobacco flavoring capsules can be obtained.

[0015] Furthermore: the essential oil or fragrance solvent system includes one or more of olive oil, caprylic / capric triglyceride, isopropyl myristate, 1,2-propanediol-dipropylene glycol, ethanol, and water.

[0016] Furthermore, the emulsifier includes one or more of polyoxyethylene monolaurate, sucrose fatty acid ester, polyoxyethylene monostearate, polyoxyethylene oleate, and sodium oleate, and the HLB value of the emulsifier is 10.0 to 18.0.

[0017] Furthermore, the plasticizer includes at least one of di-n-butyl phthalate, tributyl acetyl citrate, and polyethylene glycol.

[0018] Furthermore, the ultrapure water has a conductivity ≤0.056μS / cm and a resistivity ≥18.2MΩ·cm at 35℃.

[0019] Further: In step one, the emulsion is stirred for 25 to 30 minutes using a stirrer at a speed of 1500 to 2000 rpm.

[0020] Furthermore: In step two, the temperature of the ultrapure water is 25℃~35℃ when preparing the molding solution.

[0021] Furthermore: In step three, the emulsion is delivered using a peristaltic pump and then dripped through a 304 stainless steel showerhead.

[0022] Furthermore: In step seven, the temperature in the rotary drying device is 25°C and the humidity is 35%.

[0023] Furthermore: In step seven, the working time of the rotary drying device is 1.5h to 2h and its rotation speed is 30 to 40 revolutions per minute.

[0024] In summary, the present invention has the following beneficial effects:

[0025] Firstly, the method of the present invention uses a chemical film-forming method to prepare cigarette-grade burst beads. Calcium ions react with a low-acyl gelling glue solution to produce an electrochemical cross-linking reaction, forming a stable rubber shell. The shell is then formed into capsules through natural growth. The wet capsules are collected, rinsed with a surface molding liquid, and then cured, rinsed, and dried. The moisture in the wet capsules evaporates from the rubber shell, thus obtaining the cigarette-grade burst beads.

[0026] Secondly, the method described in this invention is formed through natural growth, which is simple and convenient, has a high forming rate, uniform thickness of wet capsule shell, and controllable roundness and size of wet capsules.

[0027] Thirdly, this invention uses a dripping process at room temperature, which minimizes the loss of fragrance, results in a stable finished product without oil seepage, and provides a long-lasting fragrance. Attached Figure Description

[0028] Figure 1 This is a simplified process flow diagram of the preparation method of the present invention;

[0029] Figure 2 These are actual photographs of the emulsion prepared by the method of this invention;

[0030] Figure 3 These are actual photos of the capsule emulsification and molding process during the preparation of this invention;

[0031] Figure 4 These are actual photos of the wet capsules prepared according to the present invention;

[0032] Figure 5 These are actual photos of the finished cigarette capsules prepared according to this invention;

[0033] Figure 6 These are the detection results of embodiments 1-4 of the present invention. Detailed Implementation

[0034] The present invention will be further described in detail below with reference to the accompanying drawings.

[0035] In the description of this invention, it should be understood that the terms "upper", "lower", "left", "right", "front", "rear", "inner", "outer", etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings. They are only for the convenience of describing this invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on this invention.

[0036] Furthermore, terms such as "horizontal" and "vertical" do not imply that components must be absolutely horizontal or suspended, but rather that they can be slightly tilted. For example, "horizontal" simply means that its direction is more horizontal than "vertical," and does not mean that the structure must be completely horizontal, but can be slightly tilted.

[0037] Example 1, referring to Figure 1-5 A method for preparing cigarette flavoring beads using a chemical film-forming method includes the following steps:

[0038] Step 1: Prepare the emulsion: Add 30 parts of ultrapure water, 2 parts of calcium lactate, 1 part of sodium carboxymethyl cellulose, 0.5 parts of gum arabic, 0.1 parts of emulsifier with sucrose fatty acid ester as solvent and HLB value of 10.0, and 0.1 parts of plasticizer with polyethylene glycol as solvent to a beaker and mix until the solid is completely dissolved. Then, while stirring at 1500 rpm, add 80 parts of fragrance with caprylic / capric triglyceride as solvent and keep stirring for 25 minutes to prepare the emulsion.

[0039] Step 2: Prepare the molding solution: Disperse the low acyl gellan gum at a concentration of 0.2% and dissolve it in ultrapure water at 25°C to prepare the molding solution, and stir it with a stirrer at a speed of 10 rpm.

[0040] Step 3, wet capsule preparation: The prepared emulsion is delivered by a peristaltic pump and dripped through a 304 stainless steel shower head at a rate of 5 drops per second into the molding liquid of low acyl gellan gum, while stirring and dripping. After the emulsion has been completely dripped, it is left to stand for 35 minutes while maintaining a stirring speed of 5 rpm.

[0041] Step 4: Collecting wet capsules: After rinsing the formed wet capsules twice with deionized water, separate the solid and liquid components.

[0042] Step 5: Preparation of curing solution: Dissolve calcium lactate in ultrapure water at a concentration of 1%, and keep stirring the dissolved curing solution at a speed of 8 revolutions per minute.

[0043] Step 6, Wet Capsule Curing: Add the rinsed wet capsules to the curing solution and keep stirring at 8 rpm for 5 minutes. After curing, rinse the wet capsules twice with deionized water to separate the solid and liquid.

[0044] Step 7, Finished Product Preparation: Place the rinsed wet capsules into a rotary air dryer at a temperature of 25℃ and a humidity of 35% and dry them at a speed of 30 rpm for 1.5 hours. After drying, the capsules are sieved through a standard particle size sieve, manually sorted by light, and tested by equipment to obtain qualified product A that meets the requirements for physical properties such as particle size, pressure value, weight of single capsule, and roundness.

[0045] Example 2, refer to Figure 1-5 A method for preparing cigarette flavoring beads using a chemical film-forming method includes the following steps:

[0046] Step 1: Prepare the emulsion: Add 30 parts of ultrapure water, 3 parts of calcium lactate, 2 parts of sodium carboxymethyl cellulose, 1 part of gum arabic, 0.5 parts of emulsifier with polyoxyethylene monolaurate as solvent and HLB value of 10.0, and 0.1 parts of plasticizer with polyethylene glycol as solvent to a beaker and mix until the solid is completely dissolved. Then, while stirring at 1500 rpm, add 70 parts of fragrance with caprylic / capric glyceride as solvent and 10 parts of ultrapure water as solvent and keep stirring for 25 minutes to prepare the emulsion.

[0047] Step 2: Prepare the molding solution: Disperse the low acyl gellan gum at a concentration of 0.2% and dissolve it in ultrapure water at 30°C to prepare the molding solution, and stir it with a stirrer at a speed of 10 rpm.

[0048] Step 3, wet capsule preparation: The prepared emulsion is delivered by a peristaltic pump and dripped through a 304 stainless steel shower head at a rate of 6 drops per second into the molding liquid of low acyl gellan gum, while stirring and dripping. After the emulsion has been completely dripped, it is left to stand for 35 minutes while maintaining a stirring speed of 8 rpm.

[0049] Step 4: Collecting wet capsules: After rinsing the formed wet capsules twice with deionized water, separate the solid and liquid components.

[0050] Step 5: Preparation of curing solution: Dissolve calcium lactate in ultrapure water at a concentration of 1%, and keep stirring the dissolved curing solution at a speed of 10 rpm.

[0051] Step 6, Wet Capsule Curing: Add the rinsed wet capsules to the curing solution and keep stirring at 8 rpm for 10 minutes. After curing, rinse the wet capsules twice with deionized water to separate the solid and liquid.

[0052] Step 7, Finished Product Preparation: Place the rinsed wet capsules into a rotary air dryer at a temperature of 25℃ and a humidity of 35% and dry them at a speed of 35 rpm for 1.5 hours. After drying, the capsules are sieved through a standard particle size sieve, manually sorted by light, and tested by equipment to obtain qualified product B that meets the requirements for physical properties such as particle size, pressure value, weight of single capsule, and roundness.

[0053] Example 3, referring to Figure 1-5 A method for preparing cigarette flavoring beads using a chemical film-forming method includes the following steps:

[0054] Step 1: Prepare the emulsion: Add 35 parts ultrapure water, 3 parts calcium lactate, 2 parts sodium carboxymethyl cellulose, 1 part gum arabic, 0.8 parts emulsifier with sodium oleate as solvent and HLB value of 15.0, and 0.1 parts plasticizer with polyethylene glycol as solvent to a beaker and mix until the solid is completely dissolved. Then, while stirring at 2000 rpm, add 70 parts fragrance with caprylic / capric triglyceride as solvent, 5 parts ultrapure water as solvent and 5 parts ethanol as solvent and keep stirring for 30 minutes to prepare the emulsion.

[0055] Step 2: Prepare the molding solution: Disperse the low acyl gellan gum at a concentration of 0.2% and dissolve it in ultrapure water at 35°C to prepare the molding solution, and stir it with a stirrer at a speed of 15 rpm.

[0056] Step 3, wet capsule preparation: The prepared emulsion is delivered by a peristaltic pump and dripped through a 304 stainless steel shower head at a rate of 7 drops per second into the molding liquid of low acyl gellan gum, and the dripping is carried out while stirring. After the emulsion has been completely dripped, it is left to stand for 35 minutes while maintaining a stirring speed of 8 rpm.

[0057] Step 4: Collecting wet capsules: After rinsing the formed wet capsules three times with deionized water, separate the solid and liquid components.

[0058] Step 5: Preparation of curing solution: Dissolve calcium lactate in ultrapure water at a concentration of 1%, and keep stirring the dissolved curing solution at a speed of 12 rpm.

[0059] Step 6, Wet Capsule Curing: Add the rinsed wet capsules to the curing solution and keep stirring at 8 rpm for 10 minutes. After curing, rinse the wet capsules twice with deionized water to separate the solid and liquid.

[0060] Step 7, Finished Product Preparation: Place the rinsed wet capsules into a rotary air dryer at a temperature of 25℃ and a humidity of 35% and dry them at a speed of 40 rpm for 1.8 hours. After drying, the capsules are sieved through a standard particle size sieve, manually sorted by light, and tested by equipment to obtain qualified product C with physical properties such as particle size, pressure value, weight of single capsule, and roundness that meet the requirements.

[0061] Example 4, refer to Figure 1-5 A method for preparing cigarette flavoring beads using a chemical film-forming method includes the following steps:

[0062] Step 1: Prepare the emulsion: Add 50 parts ultrapure water, 5 parts calcium lactate, 3 parts sodium carboxymethyl cellulose, 4 parts gum arabic, 1 part emulsifier with polyoxyethylene monostearate as solvent and HLB value of 18.0, and 0.5 parts plasticizer with polyethylene glycol as solvent to a beaker and mix until the solid is completely dissolved. Then, while stirring at 2000 rpm, add 70 parts flavoring with caprylic / capric triglyceride as solvent, 5 parts ultrapure water as solvent and 5 parts olive oil as solvent and keep stirring for 30 minutes to prepare the emulsion.

[0063] Step 2: Prepare the molding solution: Disperse the low acyl gellan gum at a concentration of 0.2% and dissolve it in ultrapure water at 35°C to prepare the molding solution, and stir it with a stirrer at a speed of 15 rpm.

[0064] Step 3, wet capsule preparation: The prepared emulsion is delivered by a peristaltic pump and dripped through a 304 stainless steel shower head at a rate of 8 drops per second into the molding liquid of low acyl gellan gum, and the dripping is carried out while stirring. After the emulsion has been completely dripped, it is left to stand for 40 minutes while maintaining a stirring speed of 8 rpm.

[0065] Step 4: Collecting wet capsules: After rinsing the formed wet capsules three times with deionized water, separate the solid and liquid components.

[0066] Step 5: Preparation of curing solution: Dissolve calcium lactate in ultrapure water at a concentration of 3%, and keep stirring the dissolved curing solution at a speed of 12 rpm.

[0067] Step 6, Wet Capsule Curing: Add the rinsed wet capsules to the curing solution and keep stirring at 12 rpm for 10 minutes. After curing, rinse the wet capsules three times with deionized water to separate the solid and liquid.

[0068] Step 7, Finished Product Preparation: Place the rinsed wet capsules into a rotary air dryer at a temperature of 25℃ and a humidity of 35% and dry at a speed of 40 rpm for 2 hours. After drying, the capsules are sieved through a standard particle size sieve, manually sorted by light, and tested by equipment to obtain qualified product D with physical properties that meet the requirements, such as particle size, pressure value, weight of a single capsule, and roundness.

[0069] The finished tobacco capsules A, B, C, and D prepared in the four embodiments were tested for indicators such as particle size qualification rate, pressure value qualification rate, single capsule weight, and number of capsules per kilogram. The test results are as follows: Figure 6 As shown:

[0070] Table 1. Quality test results of popping bead samples

[0071]

[0072] The test results show that the molding method described in this invention has good adaptability to flavors with different solvents. The capsules are round and smooth, and no solid, droplet, off-center, hollow, bubble, trailing, sunken, or oil-seeping beads were found. All indicators of the finished capsules are within the ideal range. Except for product D prepared in Example 4, which was found to have severe capsule deformation during the drying process, resulting in more oval-shaped capsules, the yield of the other products is above 90%, which meets the technical requirements for the production of capsule cigarettes.

[0073] Thirteen sensory evaluation experts compared the finished tobacco capsules A, B, C, and D prepared in the four examples with their corresponding flavoring samples using a blind sensory evaluation method to find differences. The sensory evaluation results are shown in Table 2.

[0074] Table 2 Sensory Evaluation Results

[0075] Finished cigarette capsule number A B C D Differences in the evaluation of menthol capsules and flavorings Indifference Indifference Indifference Indifference

[0076] The evaluation results show that the preparation method described in this invention does not cause the loss of fragrance and can retain the characteristic fragrance of the fragrance to the greatest extent, which is more advantageous than the popping beads prepared by traditional physical methods.

[0077] The tobacco capsules A, B, C, and D prepared in the four examples were bottled and sealed in an environment with a temperature of 28°C and a humidity of 60% for three months to conduct a stability test. The appearance of the capsules was observed for any oil leakage, and the pressure value and sensory indicators of the capsules were tested. The results of the stability test are shown in Table 3.

[0078] Table 3. Stability Results After Three Months of Storage

[0079] Finished cigarette capsule number A B C D Appearance No oil seepage or deformation No oil seepage or deformation No oil seepage or deformation No oil seepage or deformation Pressure value (N) Decrease of 0.51 Decrease of 0.69 Decrease of 0.31 Decrease of 0.58 odor No odor or mold No odor or mold No odor or mold No odor or mold

[0080] Stability tests show that after three months of storage, the popping beads prepared by the method described in this invention show no oil seepage or deformation, the pressure value decreases by 0.31-0.69N, and there is no off-odor or mold, meeting the requirements for storage and use.

[0081] This specific embodiment is merely an explanation of the present invention and is not intended to limit the invention. After reading this specification, those skilled in the art can make inventive modifications to this embodiment as needed, but as long as they are within the scope of the claims of the present invention, they are protected by patent law.

Claims

1. A method for preparing a smoking explosion ball by a chemical film formation method, characterized by, The method comprises the following steps: Step one, preparing emulsion: 70-80 parts of essential oil or fragrance, 1-3 parts of sodium carboxymethyl cellulose, 2-5 parts of calcium lactate, 0.5-4 parts of gum arabic, 30-50 parts of ultrapure water, 0.1-1 parts of emulsifier, 0.1-0.5 parts of plasticizer are stirred and mixed to prepare emulsion, the ultrapure water has an electrical conductivity of ≤0.056 μS / cm and an electrical resistivity of ≥18.2 MΩ·cm at 35℃, the emulsifier comprises one or more of polyoxyethylene monolaurate, sucrose fatty acid ester, polyoxyethylene monostearate, polyoxyethylene oleyl ether, and sodium oleate, and the HLB value of the emulsifier is 10.0-18.0; Step two, preparing forming liquid: low acyl gellan gum is dispersed at a concentration of 0.2%-0.4% and then dissolved in ultrapure water at a temperature of 25-35℃ to prepare the forming liquid, and stirring is performed at a speed of 10-15 revolutions per minute; Step three, preparing wet capsules: the prepared emulsion is added dropwise into the forming liquid of low acyl gellan gum at a speed of 5-8 drops per second, and the step of stirring while adding dropwise is performed, after the emulsion is completely added, the wet capsules are placed in a stirring state at a speed of 5-8 revolutions per minute for 35-40 minutes; Step four, collecting wet capsules: the formed wet capsules are rinsed with deionized water for 2-3 times and then solid-liquid separated; Step five, preparing solidification liquid: calcium lactate is fully dissolved in ultrapure water at a concentration of 1%-3%, and the prepared solidification liquid is stirred at a speed of 8-12 revolutions per minute; Step six, solidifying wet capsules: the rinsed wet capsules are added into the solidification liquid, and after being placed in a stirring state at a speed of 8-12 revolutions per minute for 5-10 minutes, the solidified wet capsules are rinsed with deionized water for 2-3 times and then solid-liquid separated; Step seven, preparing finished products: the rinsed wet capsules are placed in a rotary air drying device for a period of time, and then screened, light selected, and detected to obtain the smoke bursting beads.

2. The method of claim 1, wherein the method is characterized by: The essential oil or fragrance solvent system comprises one or more of olive oil, caprylocaproyl glycerol, isopropyl myristate, ethanol, and water.

3. The method of claim 1, wherein the method is characterized by: The plasticizer comprises at least one of di-n-butyl phthalate, acetyl tributyl citrate, and polyethylene glycol.

4. The method of claim 1, wherein the method is characterized by: In step one, the emulsion is stirred in a stirrer at a speed of 1500-2000 revolutions per minute for 25-30 minutes.

5. The method of claim 1, wherein the method is characterized by: In step three, the emulsion is delivered by a peristaltic pump and then dripped through a 304 stainless steel shower head.

6. The method of claim 1, wherein the method is characterized by: In step seven, the temperature in the rotary air drying device is 25℃, and the humidity is 35%.

7. The method of claim 1, wherein the method is characterized by: In step seven, the working time of the rotary air drying device is 1.5-2 hours, and the speed thereof is 30-40 revolutions per minute.

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