CN116406816A - A kind of water-soluble core material pop-up beads for cigarettes and preparation method thereof - Google Patents

Abstract

The invention discloses a water-soluble core material popping beads for cigarettes and a preparation method thereof. The popping beads are composed of an outer wall material, an inner wall material and a core material, the outer wall material is gelatin, and the outer wall material is gelatin. The inner wall material is a blend containing hydrophobic material, wax material, long-chain lipid and interface adhesive. The interface adhesive is selected from at least one of nano-mica sheets, nano-calcium carbonate, and oleic acid amide, and the core material is selected from a mixed solution or a solvent composed of essence and/or natural extracts and solvents; The popping beads use gelatin as the outer wall material to provide strength and ensure the roundness of the popping beads, while the inner wall material provides hydrophobicity. At the same time, the interface binder is used to increase the melt index of the blend and increase the outer wall material and inner wall material. The bonding force of the wall materials, this three-layer structure not only solves the problems of the strength and roundness of the popping beads while ensuring the moisture content, but also improves the qualified rate of product preparation. The preparation method of the present invention uses a three-layer dripper for one-time curing and molding, which is simple and controllable.

Description

A kind of water-soluble core material pop-up beads for cigarettes and preparation method thereof

technical field

The invention belongs to the technical field of cigarettes, and in particular relates to a water-soluble core material cigarette popping beads and a preparation method thereof.

Background technique

Popping bead cigarettes continue to be favored in the cigarette market because they can also provide various preset flavors in addition to the smoke aroma provided by conventional tobacco combustion. The reduction of tar will significantly affect the taste of the smoke, and the addition of popping beads can make up for this shortcoming. In the current pop-pear cigarettes on the market, the pop-pear flavors are mainly oil-soluble. Although the aroma of the oil can be removed by multiple means, the oil is generally relatively viscous, and it will block the transmission of the smoke aroma after soaking in the cigarette butt. , At the same time, there are fewer types of oil-soluble flavors, which cannot meet the needs of different people. Although water-soluble flavor popping beads perfectly avoid these two shortcomings, the water-soluble flavor popping beads currently on the market are not yet popular, which is related to the difficulty in preparing water-soluble flavor popping beads.

Domestic research on water-soluble popping beads for cigarettes has also achieved fruitful results in recent years, but the mechanism or process conditions based on these studies are often too ideal. Chinese patent CN109222226 A discloses a cigarette packaged with hydrogel beads. Capsules and methods for their preparation. The scheme of this patent is to form a water-soluble flavor pop-up ball with hydrogel beads and a hydrophobic coating layer coated on the outside. First, the aqueous solution of sodium alginate is used to complex with Ca ions to form a hydrogel, and then the hydrophobic coating is sprayed. The material is atomized and evenly sprayed onto the surface of the hydrogel. Although this method can prepare water-soluble flavor popping beads, there are many deficiencies. Firstly, after the sodium alginate hydrogel is pinched and popped, it is easy to block the cigarette butt, affect the circulation of smoke, and reduce the mouthfeel of cigarettes; secondly, the sodium alginate hydrogel and The stable coexistence of water-soluble flavors is a big problem; finally, the spraying process of the outer hydrophobic material is complicated and requires high standards.

Chinese patent CN110973699 A discloses a water popping pearl and a preparation method thereof. This patent selects water-soluble essence, calcium chloride and xanthan gum as the core material, drips the core material into the wall material glue solution prepared by using sodium alginate and paraffin as raw materials, and then reacts the sodium alginate in the wall material through fatty amine. Perform ion adsorption and hydrophobic modification to obtain water-soluble flavor popping beads. However, this patent is too idealistic. First of all, the surface tension of the core material can be improved by xanthan gum, but it also means that the types of core material flavors can be selectively reduced. Secondly, the core material is dripped into the wall material glue. Although the wall material is demulsified, the surface will be covered with a layer of unbroken latex, which not only increases the cost, but also brings difficulties for subsequent cleaning. Therefore, although this method is feasible, there are disadvantages such as low degree of automation and high cost.

Chinese patent CN107361392 B discloses a three-layer water-containing capsule and its preparation method. This patent uses a phase-change oil layer as the inner layer to wrap the water-containing core material, and then wraps the oil layer with natural animal and plant glue to achieve the water-wrapping function. However, the material used in the grease layer of this patent generally has the aroma of lipid materials. At the same time, the wall thickness of the grease layer reaches 1.5mm, which is close to half of the diameter of the entire capsule. The use of core material explosive beads.

Chinese patent CN110419775 A discloses a kind of anti-leakage water blasting beads and its preparation method. The patent is a three-layer capsule structure, the outer rubber layer is a polyacrylic resin layer, and the inner rubber layer is a photosensitive resin layer. The material of the rubber layer is light-cured, and the pop-up beads are cured during the dripping process, and then after post-treatment, the glue is sprayed twice to cover the polyacrylic resin layer, so that the water-pocket beads produced have better sealing performance. However, this patent requires secondary treatment, and the process is cumbersome. At the same time, the glue solution needs to be protected from light during the preparation and dripping of the inner layer glue solution, which greatly limits the production conditions of the process.

Chinese patent CN113367379 A discloses a kind of tobacco product, and the mouth stick of this product contains water popping beads. The patent adopts a double-layer coating method, and the inner coating layer and the outer coating layer are sequentially coated on the surface of the inner core. The product obtained has good water retention and the pressure value also meets the industry standard. However, this coating method needs to be carried out in stages. For example, the coating of the inner layer needs to be cycled and alternately coated, and the staged process increases the risk of contamination of the inner core and the entire product. At the same time, after the inner layer is coated, it needs to be placed in hot water for heat preservation and curing, and part of the coating layer wax oil will appear uneven due to the influence of surface tension.

To sum up, although some theoretical and method explorations have been made in the field of water-soluble core material explosion beads in China, the process is often cumbersome, impractical, and cannot be practically applied. In the prior art, due to the consideration of the strength of the wall material and the roundness of the drop, it is often impossible to make it in one step, and the secondary treatment method is generally used, which brings inconvenience to production and application.

Contents of the invention

In view of the deficiencies and current situation of the prior art, the first object of the present invention is to provide a water-soluble core material cigarette popping beads; the second purpose of the present invention is to provide a water-soluble core material cigarette popping beads material Methods. The preparation method provided by the invention has simple process, safe, reliable and environment-friendly raw materials, and low cost, and can be widely used in the technical field of cigarettes.

In order to achieve the above object, the present invention provides the following technical solutions:

The invention discloses a water-soluble core material popping bead for cigarettes. The popping bead is composed of 1-2 parts by weight of the outer layer wall material, 8-29 parts by weight of the inner layer wall material, and 70-90 parts by weight of the core material , the outer wall material is gelatin, the core material is selected from a mixture of essence and/or natural extracts and polar solvents or a polar solvent; the inner wall material is composed of hydrophobic materials, wax materials , a blend of long-chain lipids and an interface adhesive, wherein the hydrophobic material is an ethylene-vinyl acetate copolymer, and the interface adhesive is selected from nano-mica sheets, nano-calcium carbonate, and oleic acid amide at least one.

The water-soluble core material popping beads for cigarettes of the present invention has a three-layer concentric spherical capsule structure, wherein gelatin is used as the outer wall material to provide strength and ensure the roundness of the popping beads, while the inner wall material provides hydrophobicity. While ensuring the moisture content, the structure not only solves the problem of the strength of the popping beads, but also improves the qualified rate of product preparation. Of course, the proportion by weight of the popping ball material will have a certain impact on the performance of the material. Within the scope of the present invention, the performance of the final popping ball material is optimal, and if the proportion of the outer wall material is too low, it will As a result, the strength of the popping beads is too low, variable and unable to provide a "pinching" feel. When the mass ratio of the outer wall material is too high, the strength of the popping beads will be too high and cannot be crushed.

In the present invention, the inner layer wall material is based on hydrophobic material, considering that the core material is an aqueous solution, which boils at 100°C under standard atmospheric pressure, which is not conducive to the inclusion process. Therefore, adding waxes will reduce the melting point of the blend. It can increase the melt index of the blend and reduce the viscosity of the blend. When the viscosity of the wall material glue is too high, the dripping sample will appear "tailing" phenomenon, and the roundness of the obtained product cannot be guaranteed. While waxes are added, the melt index of the blend can be increased, and the viscosity of the blend can be reduced, thereby avoiding the "tailing" phenomenon in the dripping sample due to the excessive viscosity of the wall material glue, resulting in The roundness of the product cannot be guaranteed. In addition, a small amount of interface binder is added to increase the melt index of the blend and increase the bonding force between the outer wall material and the inner wall material, which can better improve the compatibility and fit of the inner and outer wall materials. The strength of the popping bead material is improved, and the end groups of the added long-chain fat are mainly hydroxyl and carboxyl groups, which can form hydrogen bonds with the outer layer of gelatin to further enhance the performance of the popping bead material, which can further improve the performance of the popping bead material. strength.

In a preferred solution, the wax material is at least one selected from paraffin wax, polyethylene wax, paraffin wax, and microcrystalline wax.

In a preferred embodiment, the long-chain lipids are selected from at least one of stearic acid, stearyl alcohol, and oleic acid.

In a preferred solution, in the inner wall material, hydrophobic material: wax material: long-chain lipid: interface adhesive = 15-25: 69.5-85: 0-10: 0-0.5 by mass ratio.

The inventors found that controlling the mass ratio of the hydrophobic material to the waxy material within the above-mentioned range will result in the highest qualified rate of final popping beads and the strongest crushing strength.

Further preferably, in the inner wall material, in terms of mass ratio, hydrophobic material: wax material: long-chain lipid: interface adhesive = 15-25: 69.5-85: 3-7: 0.3-0.7.

In a preferred scheme, the interface adhesive is a mixture of nano-mica sheet, nano-calcium carbonate, and oleic acid amide, and in the interface-binding agent, by mass ratio: nano-mica sheet: nano-calcium carbonate: oleic acid amide=0 ～2: 0～2: 0～2; preferably 1～2: 1～2: 1～2.

The interface binding agent selected by the present invention, the nano-calcium carbonate and the surface of the nano-mica sheet are rich in hydroxyl groups, etc., can form hydrogen bond interactions with the carboxyl and amino glues of the outer layer gelatin molecules, and increase the interaction force between the inner layer and the outer layer , making the inner and outer layers more tightly bonded. However, oleic acid amide can provide cations, and ion adsorption occurs with carboxyl anions in the outer layer of gelatin glue, thereby increasing the interface between the outer layer and the inner layer to a certain extent, and improving the strength of the popping beads. However, when the interface binder of the above formula is used according to the above ratio, finally under the synergistic effect of nano-mica sheet, nano-calcium carbonate, and oleic acid amide, the bead-popping performance is optimal, but the amount of the interface binder needs to be effectively controlled. When the interface binder is added too much, because it cannot be uniformly dispersed in the blended hydrophobic wall material glue, it will destroy the film-forming and uniformity of the hydrophobic wall material, and reduce the qualified rate and crushing strength of the sample. Of course, there are many nano-materials rich in hydroxyl groups. However, through a large number of experiments, the present invention finds that only the addition of nano-calcium carbonate and nano-mica sheets can improve performance. For example, the inventor also tried nano-dioxide Silicon, then added did not bring about an increase in performance, but rather a decrease in performance.

In a preferred scheme, the polar solvent is at least one selected from water, ethanol, propylene glycol, and glycerol.

The types of essence and natural extracts are not limited in the present invention, and water-soluble or alcohol-soluble essences or natural extracts commonly used in the present technology can be used. Such as natural green tea extract, rose essence, jasmine essence, mint essence, sandalwood essence, pineapple essence and lemon essence etc.

The invention discloses a method for preparing water-soluble core material popping beads for cigarettes, comprising the following steps: adding gelatin to water, heating to obtain outer layer wall material glue, and preparing wax materials, long-chain lipids, and hydrophobic materials according to the designed ratio , interface binder mixed and melted to obtain the inner wall material glue, the essence and/or natural extracts are mixed with polar solvents, and heated to obtain the core material; then the outer layer wall material glue, the inner wall material glue, The core material is dripped into the cooling liquid through the outer layer, middle layer and inner layer of the three-layer dripper, solidified and dried to obtain the water-soluble core material cigarette popping beads.

The preparation method of the present invention is to obtain the water-soluble core material cigarette popping beads through three-layer coating dripping, after the outer layer glue, the inner wall material glue and the core material are dripped into the cooling liquid through the three-layer dripper, Rapid cooling and solidification. After contacting the cooling liquid, the temperature of the outer layer of glue drops rapidly below the freezing point to solidify, and the inner layer of wall material glue also solidifies quickly due to the ambient temperature dropping below the freezing point, covering the core material. The pills are discharged from the dropping pill machine through the cooling liquid circulation system, and the popping beads are collected and washed to remove the residual cooling liquid on the surface. After drying, the water-soluble core material popping beads for cigarettes are obtained.

In a preferred solution, gelatin is added to water, stirred at 60° C. to 85° C. for 1 to 2 hours, and then ultrasonicated for 30 minutes to 60 minutes to obtain the outer wall material glue.

In the present invention, after adding gelatin to deionized water, stir fully under heating conditions, continue to stir after the gelatin fully absorbs water, until the aqueous solution is uniform in texture without hard lumps, and then ultrasonically discharge the bubbles generated by stirring to obtain the outer wall material glue , heat preservation, stand-by.

In a preferred solution, the mass ratio of the gelatin to water is 4-6:94-96.

In a preferred solution, the viscosity of the outer wall material glue is 20m·Pas-400m·Pas.

Further preferably, the viscosity of the outer wall material glue is 250 m·Pas˜400 m·Pas.

In the present invention, on the one hand, the air bubbles in the gelatin can be eliminated by heating. The existence of the air bubbles will cause defects in the dripping product, which is unqualified. The performance of the beads is the best, because the viscosity is too high, it will cause "tailing" phenomenon in the dripping process, and the roundness cannot be guaranteed, and the viscosity is too small, it will cause the solid content of the glue to be too low, and the strength of the outer wall material is not enough.

The preferred solution is to mix wax materials, long-chain lipids, hydrophobic materials, and interface binders according to the designed ratio, heat to 120°C-140°C for 2-3 hours, melt to obtain the mixture, and then cool down to 80°C-100°C °C, preferably 90 °C to 100 °C, to obtain the inner wall material glue.

In a preferred solution, the viscosity of the inner wall material glue is 50m·Pas-300m·Pas.

Further preferably, the viscosity of the inner wall material glue is 200m·Pas˜300m·Pas.

In a preferred solution, the temperature of the core material is 60°C to 80°C, preferably 70°C to 80°C.

In the actual operation process, preheat the three-layer dripper dripping pill machine first, set the temperature of each component, and add the preheated outer wall material glue, inner wall material glue and core material respectively. In the corresponding glue tank, set the appropriate flow rate, the core material, the melted inner wall material glue and the outer wall material glue are collected at the outlet of the three-layer dripper through the glue pipe and dripped in by the three-layer dripper In the cooling liquid, when in contact with the cooling liquid, under the action of surface tension, the mixed droplets are cooled to form water-soluble core material popping beads for cigarettes. The solidified explosive beads are discharged from the dropping pill machine through the cooling circulation system, the washing liquid washes off the residual cooling liquid on the surface, and the product is collected and air-dried.

In a preferred solution, the temperature of the three-layer dripper is 75°C-90°C, preferably 80°C-85°C.

In the present invention, the temperature of the three-layer dripper needs to be effectively controlled. If the temperature of the dripper is too high, it will cause the core material to boil, and defects such as air bubbles will appear in the inner core of the pop-up beads obtained by dripping. If the temperature is too low, the inner layer of glue will The liquid cannot reach the molten state and cannot be dripped.

In a preferred solution, the outer wall material glue, the inner wall material glue, and the core material are 10-20r/min: 2-10r/min: 0.5-5r/min, preferably 13-17r/min: 3~7r/min: Drop into the cooling liquid at a dropping speed of 1~3r/min.

The inventors found that controlling the dripping speed of the outer layer wall material glue, the inner layer wall material glue, and the core material within the above-mentioned range can ensure that the particles are full and uniform and control the thickness of the inner layer and the outer layer of the wall material, so that the popping beads The strength of the pellets is most suitable.

Preferably, the cooling liquid is liquid paraffin oil.

The inventors found that the gelatin of the outer layer can be cooled and solidified only by using a hydrophobic cooling liquid, while the use of liquid paraffin oil can ensure that the outer layer of wall material is fully solidified and does not cause odor.

In a preferred scheme, the temperature of the cooling liquid is 5°C to 25°C, preferably 20°C to 25°C.

In the actual operation process, after solidification, it is washed with ethanol aqueous solution, and then dried in cold air at 20°C to 25°C to obtain popping beads. The mass ratio of ethanol:water is preferably 95:5.

Beneficial effect:

1. The raw materials of the wall material described in the present invention are non-toxic and harmless, and the cost is low, which is convenient for packaging and transportation. The preparation method of the inner wall material glue is simple, and the target product can be obtained by heating, melting and blending in one pot, without the need for catalysts, initiators, etc., which not only reduces the cost, simplifies the difficulty of preparation, but also protects the environment.

2. In practical application, the present invention adopts the above-mentioned optimum material ratio, and the solution obtained under the above-mentioned optimum conditions is used as the wall material, and water and aqueous solution are used as the core material. Under the action, a large number of water-soluble core material explosive beads are produced efficiently; the product is automatically collected through the circulation of the cooling system, and the degree of automation is high. The finished product has full and uniform granules, moderate thickness of the wall material, high pass rate, and the strength and water content meet the standards for popping beads for cigarettes. In practical application, the wall material has the advantages of simple production process, low production cost, no environmental pollution, and easy realization of large-scale industrial production.

Description of drawings

Fig. 1 is the photograph of the prepared quick-fried bead sample of embodiment 1, can find out from it, quick-fried bead particle is plump and uniform, and surface is smooth and smooth,

Fig. 2 is the crushing strength of the sample, as can be seen from the figure, the crushing strength of the embodiment is better than that of the comparative example.

Fig. 3 is the qualified rate of sample, as can be seen from the figure, the qualified rate of embodiment sample is all greater than 90%, is obviously better than comparative example sample qualified rate.

Fig. 4 is the average particle diameter of the sample, as can be seen from the figure, the average particle diameter fluctuation of the example sample is small, and the average particle diameter fluctuation of the comparative example sample is large.

Detailed ways

The present invention is specifically described below by way of examples. It is necessary to point out that the following examples are only used to further illustrate the present invention, and cannot be interpreted as limiting the protection scope of the present invention, and those skilled in the art can make some non-essential improvements according to the content of the present invention above and adjust.

The comparison of the performance evaluation of the pop-up beads prepared by each embodiment

(1) The passing rate of popping beads adopts random sampling method, and randomly checks 100 popping beads to check whether the appearance is broken and the roundness.

(2) The diameter of the popping beads is measured with a vernier caliper, and at least 20 balls are randomly measured.

(3) The crushing strength of popping beads is measured by micro pressure sensing equipment, and at least 20 beads are randomly tested.

Example 1

Take 50g of gelatin, slowly add 950g of deionized water and stir for 1 hour, heat in a water bath at 85°C, after the gelatin is completely dissolved in water, ultrasonically remove the bubbles generated by stirring at 85°C for half an hour to obtain a viscosity of 350m Pas Gelatin, continue to keep warm, set aside.

Take 74.5g of paraffin, heat at 130°C and stir for 20 minutes. After the paraffin is completely melted, add 20g of ethylene-vinyl acetate copolymer and 5g of stearic acid into the molten paraffin oil. After continuing to heat for 20 minutes, after melting, mechanically stir and add 0.5g nanometer mica flakes until the mixture is uniform. Lower the temperature of the oil bath to 95°C to obtain a glue solution for the inner wall material with a viscosity of 237m·Pas, ready for use.

Take 150 g of natural green tea extract aqueous solution and heat to 75°C. Pour the core material, the inner layer blended glue solution and the outer layer wall material glue solution into the preheated dripping pill machine storage tank respectively, keep warm and let stand. Adjust the pumping flow rate of glue and core material, and start collecting after the flow rate is suitable. Flow rate setting parameters: outer layer glue: inner wall material glue: core material = 15:4:3, unit: r/min.

Under the action of gravity, drip the outer layer, middle layer, and inner layer of the outer layer, middle layer, and inner layer of the three-layer dripper with a temperature of 85°C into the cooling liquid respectively, and the dropping temperature is In liquid paraffin oil at 20°C, due to the effect of surface tension, the outer layer of glue is closed to form a sealed pop-up bead, and the outer layer of gelatin meets liquid paraffin oil, rapidly cools and solidifies to form a solidified pop-up bead. The beads were collected, washed repeatedly with aqueous ethanol, and dried.

The average crushing strength of the obtained samples can reach 1.83kgf, the average particle size is 3.42mm, uniform and regular, round and full, and the qualified rate can reach 97%.

Comparative example 1

Other conditions are the same as in Example 1, only 0.5g of nano-mica flakes are not added.

The average crushing strength of the obtained sample is only 1.52kgf, the average particle size is 3.49mm, the wall thickness is uneven and the roundness is poor, and the pass rate is only 83%.

Example 2

Take 50g of gelatin, slowly add 950g of deionized water and stir for 1 hour, heat in a water bath at 85°C, after the gelatin is completely dissolved in water, ultrasonically remove the bubbles generated by stirring at 85°C for half an hour to obtain a viscosity of 350m Pas Gelatin, continue to keep warm, set aside.

Take 74.5g of polyethylene wax, heat at 130°C and stir for 20 minutes, after the polyethylene wax is completely melted, add 20g of ethylene-vinyl acetate copolymer and 5g of stearyl alcohol into the molten polyethylene wax. After continuing to heat for 20 minutes, after melting, mechanically stir and add 0.5g of nano-calcium carbonate until uniformly mixed. Lower the temperature of the oil bath to 95°C to obtain a glue solution for the inner wall material with a viscosity of 269m·Pas, ready for use.

Take 150 g of natural green tea extract aqueous solution and heat to 75°C. Pour the core material, the inner layer blended glue solution and the outer layer wall material glue solution into the preheated dripping pill machine storage tank respectively, keep warm and let stand. Adjust the pumping flow rate of glue and core material, and start collecting after the flow rate is suitable. Flow rate setting parameters: outer layer glue: inner wall material glue: core material = 15:4:3, unit: r/min.

Under the action of gravity, drip the outer layer, middle layer, and inner layer of the outer layer, middle layer, and inner layer of the three-layer dripper with a temperature of 85°C into the cooling liquid respectively, and the dropping temperature is In liquid paraffin oil at 20°C, due to the effect of surface tension, the outer layer of glue is closed to form a sealed pop-up bead, and the outer layer of gelatin meets liquid paraffin oil, rapidly cools and solidifies to form a solidified pop-up bead. The beads were collected, washed repeatedly with aqueous ethanol, and dried.

The average crushing strength of the obtained samples can reach 1.72kgf, the average particle size is 3.51mm, uniform and regular, round and full, and the qualified rate can reach 93%.

Comparative example 2

Other conditions are identical with embodiment 2, only do not add 0.5g nano calcium carbonate.

The average crushing strength of the obtained sample is only 1.32kgf, the average particle size is 3.31mm, the wall thickness is uneven and the roundness is poor, and the qualified rate is only 79%.

Example 3

Take 50g of gelatin, slowly add 950g of deionized water and stir for 1 hour, heat in a water bath at 85°C, after the gelatin is completely dissolved in water, ultrasonically remove the bubbles generated by stirring at 85°C for half an hour to obtain a viscosity of 350m Pas Gelatin, continue to keep warm, set aside.

Take 74.5g of insect wax, heat at 130°C and stir for 20 minutes, after the insect wax is completely melted, add 20g of ethylene-vinyl acetate copolymer and 5g of oleic acid into the melted insect wax. After continuing to heat for 20 minutes, after melting, mechanically stir and add 0.5 g of oleic acid amide until the mixture is uniform. Lower the temperature of the oil bath to 95°C to obtain a glue solution for the inner wall material with a viscosity of 282m·Pas, ready for use.

Take 150 g of natural green tea extract aqueous solution and heat to 75°C. Pour the core material, the inner layer blended glue solution and the outer layer wall material glue solution into the preheated dripping pill machine storage tank respectively, keep warm and let stand. Adjust the pumping flow rate of glue and core material, and start collecting after the flow rate is suitable. Flow rate setting parameters: outer layer glue: inner wall material glue: core material = 15:4:3, unit: r/min.

Under the action of gravity, drip the outer layer, middle layer, and inner layer of the outer layer, middle layer, and inner layer of the three-layer dripper with a temperature of 85°C into the cooling liquid respectively, and the dropping temperature is In liquid paraffin oil at 20°C, due to the effect of surface tension, the outer layer of glue is closed to form a sealed pop-up bead, and the outer layer of gelatin meets liquid paraffin oil, rapidly cools and solidifies to form a solidified pop-up bead. The beads were collected, washed repeatedly with aqueous ethanol, and dried.

The average crushing strength of the obtained samples can reach 1.87kgf, the average particle size is 3.47mm, uniform and regular, round and full, and the qualified rate can reach 92%.

Comparative example 3

Other conditions were the same as in Example 3, except that 0.5 g of oleic acid amide was not added.

The average crushing strength of the obtained sample is only 1.37kgf, the average particle size is 3.57mm, the wall thickness is uneven and the roundness is poor, and the qualified rate is only 86%.

Example 4

Take 50g of gelatin, slowly add 950g of deionized water and stir for 1 hour, heat in a water bath at 85°C, after the gelatin is completely dissolved in water, ultrasonically remove the bubbles generated by stirring at 85°C for half an hour to obtain a viscosity of 350m Pas Gelatin, continue to keep warm, set aside.

Take 74.5g of microcrystalline wax, heat it at 130°C and stir for 20 minutes, and then add 20g of ethylene-vinyl acetate copolymer and 5g of oleic acid into the molten microcrystalline wax after the microcrystalline wax is completely melted. After continuing to heat for 20 minutes, after melting, mechanically stir and add 0.5 g nano-mica flakes until the mixture is uniform. Lower the temperature of the oil bath to 95°C to obtain a glue solution for the inner wall material with a viscosity of 271m·Pas, ready for use.

Take 150 g of natural green tea extract aqueous solution and heat to 75°C. Pour the core material, the inner layer blended glue solution and the outer layer wall material glue solution into the preheated dripping pill machine storage tank respectively, keep warm and let stand. Adjust the pumping flow rate of glue and core material, and start collecting after the flow rate is suitable. Flow rate setting parameters: outer layer glue: inner wall material glue: core material = 15:4:3, unit: r/min.

Under the action of gravity, drip the outer layer, middle layer, and inner layer of the outer layer, middle layer, and inner layer of the three-layer dripper with a temperature of 85°C into the cooling liquid respectively, and the dropping temperature is In liquid paraffin oil at 20°C, due to the effect of surface tension, the outer layer of glue is closed to form a sealed pop-up bead, and the outer layer of gelatin meets liquid paraffin oil, rapidly cools and solidifies to form a solidified pop-up bead. The beads were collected, washed repeatedly with aqueous ethanol, and dried.

The average crushing strength of the obtained samples can reach 1.73kgf, the average particle size is 3.41mm, uniform and regular, round and full, and the qualified rate can reach 96%.

Comparative example 4

Other conditions are the same as in Example 4, except that the nano-mica sheet addition is 1.5g.

The average crushing strength of the obtained sample is only 1.51kgf, the average particle size is 3.37mm, the wall thickness is uneven and the roundness is poor, and the qualified rate is only 82%.

Example 5

Take 50g of gelatin, slowly add 950g of deionized water and stir for 1 hour, heat in a water bath at 85°C, after the gelatin is completely dissolved in water, ultrasonically remove the bubbles generated by stirring at 85°C for half an hour to obtain a viscosity of 350m Pas Gelatin, continue to keep warm, set aside.

Take 74.5g of paraffin, heat at 130°C and stir for 20 minutes. After the paraffin is completely melted, add 20g of ethylene-vinyl acetate copolymer and 5g of stearyl alcohol into the molten paraffin. After continuing to heat for 20 minutes, after melting, mechanically stir and add 0.2g nano-mica flakes, 0.2g nano-calcium carbonate and 0.2g oleic acid amide, until the mixture is uniform. Lower the temperature of the oil bath to 95°C to obtain a glue solution for the inner wall material with a viscosity of 237m·Pas, ready for use.

Take 150 g of natural green tea extract aqueous solution and heat to 75°C. Pour the core material, the inner layer blended glue solution and the outer layer wall material glue solution into the preheated dripping pill machine storage tank respectively, keep warm and let stand. Adjust the pumping flow rate of glue and core material, and start collecting after the flow rate is suitable. Flow rate setting parameters: outer layer glue: inner wall material glue: core material = 15:4:3, unit: r/min.

Under the action of gravity, drip the outer layer, middle layer, and inner layer of the outer layer, middle layer, and inner layer of the three-layer dripper with a temperature of 85°C into the cooling liquid respectively, and the dropping temperature is In liquid paraffin oil at 20°C, due to the effect of surface tension, the outer layer of glue is closed to form a sealed pop-up bead, and the outer layer of gelatin meets liquid paraffin oil, rapidly cools and solidifies to form a solidified pop-up bead. The beads were collected, washed repeatedly with aqueous ethanol, and dried.

The average crushing strength of the obtained samples can reach 1.81kgf, the average particle size is 3.41mm, uniform and regular, round and full, and the qualified rate can reach 98%.

Example 6

Other conditions are the same as in Example 5, except that only 0.3 g of nano-mica flakes and 0.3 g of oleic acid amide are added to the interface binding agent.

The average crushing strength of the obtained sample is only 1.76kgf, the average particle size is 3.44mm, and the qualified rate is 97%.

Example 7

Other conditions were the same as in Example 5, except that 10 g of stearyl alcohol was added to the long-chain lipids.

The average crushing strength of the obtained sample can reach 1.74kgf, the average particle size is 3.43mm, and the qualified rate is 90%.

Example 8

Other conditions were the same as in Example 5, except that no long-chain lipids were added.

The average crushing strength of the obtained samples can reach 1.71kgf, the average particle size is 3.42mm, and the qualified rate is 90%.

It can be seen from the examples that the average particle diameters of the samples in the examples are all between 3.40 mm and 3.50 mm, which shows that the dripping machine works smoothly and the process parameters are well adjusted. However, the particle size of the comparative samples fluctuated significantly.

And under the condition that EVA accounts for (20%), see from embodiment 1,2,3 and corresponding comparison example result, add interfacial binding agent such as nano-mica sheet, nano-calcium carbonate and oleic acid amide, can comparatively obviously enhance explosion-proof effect. The crushing strength of beads is improved, and the product qualification rate is also improved. This is because these interfacial binders, such as nano-calcium carbonate and nano-mica sheets, are rich in hydroxyl groups, which can form hydrogen bond interactions with the carboxyl and amino glues of the outer gelatin molecules, increasing the interaction between the inner and outer layers. Make the inner and outer layers more tightly bonded. When oleic acid amide is added as an interface binder, since oleic acid amide can provide cations, ion adsorption occurs with carboxyl anions in the outer gelatin glue, thereby increasing the interface between the outer layer and the inner layer to a certain extent. The obtained popping beads particles are also improved to a certain extent. From Example 4 and Comparative Example 4, it can be found that the addition of the interface binding agent can improve the performance compared to the sample without addition. However, when the interface binder is added too much, it will not be uniformly dispersed in the blended hydrophobic wall material glue, which will destroy the film-forming and uniformity of the hydrophobic wall material, and reduce the qualified rate and crushing strength of the sample. From Example 5 and Example 6, it can be found that the combination of various interface binders can improve the performance of the bead blasting, because the interface binders form a synergistic effect. The presence of synergy was also confirmed by the slight decrease in intensity when the species was reduced. From Example 5, Example 7 and Example 8, it can be found that the presence of long-chain lipids further improves the performance of the pop-up beads, because the end groups of long-chain lipids are mainly hydroxyl and carboxyl groups, which can be combined with external Layers of gelatin form hydrogen bonds, increasing strength to a certain extent. When there are too many long-chain lipids, the targeting sites in gelatin that can generate hydrogen bonds are occupied by long-chain lipids, making it difficult to form hydrogen bonds with the interface binder, which instead leads to a decrease in the strength of the beads. Therefore, under consideration of comprehensive factors such as industrialization costs, simply blending 20% EVA with waxes and long-chain lipids, and then adding 0.5% of the total mass of the blended glue as an interface binder can significantly increase product strength and improve sample qualification rate , Reduce the cost waste caused by the unqualified rate.

Claims (10)

1. A water-soluble core material popping pearl for cigarettes, characterized in that: the popping pearl consists of 1 to 2 parts by weight of the outer wall material, 8 to 29 parts by weight of the inner wall material, 70 to 90 parts by weight The core material composition, the outer wall material is gelatin, the core material is selected from the mixture of essence and/or natural extracts and polar solvents or polar solvents; the inner wall material is composed of hydrophobic materials , a blend of waxy materials, long-chain lipids, and interfacial adhesives, wherein the hydrophobic material is ethylene-vinyl acetate copolymer, and the interfacial adhesive is selected from nano-mica sheets, nano-calcium carbonate, oil At least one of acid amides. 2. A kind of water-soluble core material popping beads for cigarettes according to claim 1, characterized in that: the wax material is selected from at least one of solid paraffin, polyethylene wax, insect wax, and microcrystalline wax; The long-chain lipids are selected from at least one of stearic acid, stearyl alcohol, and oleic acid; In the inner wall material, in terms of mass ratio, hydrophobic material: wax material: long-chain lipid: interface adhesive = 15-25: 69.5-85: 0-10: 0-0.5. 3. A kind of water-soluble core material cigarette popping beads according to claim 1, characterized in that: The interface adhesive is a mixture of nano-mica sheet, nano-calcium carbonate, and oleic acid amide. In the interface-binding agent, by mass ratio: nano-mica sheet: nano-calcium carbonate: oleic acid amide=0～2:0 ～2: 0～2. 4 . The water-soluble core material popping beads for cigarettes according to claim 1 , wherein the polar solvent is selected from at least one of water, ethanol, propylene glycol, and glycerin. 5. according to the preparation method of a kind of water-soluble core material cigarette popping beads described in any one of claims 1-4, it is characterized in that: comprising the following steps: adding gelatin into water, heating to obtain outer layer wall material glue, Mix waxy materials, long-chain lipids, hydrophobic materials, and interfacial binders according to the designed ratio, and melt to obtain the inner wall material glue; mix essence and/or natural extracts with polar solvents, and heat to obtain the core material; Then the outer wall material glue, the inner wall material glue, and the core material are dripped into the cooling liquid through the middle, outer, middle, and inner layers of the three-layer dripper respectively, solidified and dried to obtain the water-soluble core material cigarette popping beads. 6. the preparation method of a kind of water-soluble core material cigarette popping beads according to claim 5, is characterized in that: Add gelatin to water, stir at 60°C to 85°C for 1 to 2 hours, and then sonicate for 30 to 60 minutes to obtain the outer wall material glue; The mass ratio of the gelatin to water is 4-6:94-96; The viscosity of the outer wall material glue is 20m·Pas˜400m·Pas. 7. the preparation method of a kind of water-soluble core material cigarette popping beads according to claim 5, is characterized in that: Mix wax materials, long-chain lipids, hydrophobic materials, and interface binders according to the designed ratio, heat to 120°C-140°C for 2-3 hours, melt to obtain a mixture, and then cool down to 80°C-100°C. The viscosity of the inner wall material glue is 50m·Pas～300m·Pas; The temperature of the core material is 60°C-80°C. 8. the preparation method of a kind of water-soluble core material cigarette popping beads according to claim 5, is characterized in that: The temperature of the three-layer dripper is 75°C-90°C. 9. the preparation method of a kind of water-soluble core material cigarette popping beads according to claim 5, is characterized in that: The outer wall material glue, the inner wall material glue, and the core material are dripped into the cooling liquid at a rate of 10-20r/min: 2-10r/min: 0.5-5r/min. 10. The preparation method of a kind of water-soluble core material cigarette popping beads according to claim 5, characterized in that: Described coolant is liquid paraffin oil; The temperature of the cooling liquid is 5°C to 25°C.

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