Microemulsion capsule for cigarettes and preparation method thereof
Technical Field
The invention belongs to the technical field of cigarette product production, and relates to a preparation method of a novel cigarette capsule taking microemulsion as a core material.
Background
The cigarette flavoring is an important subject in the cigarette technology, is used for improving the smoking taste of the cigarette, covering offensive odor, increasing richness, moistening smoke, improving comfort, improving aftertaste and the like, and has a direct relation with the smoking feeling of consumers. The existing flavoring technologies mainly comprise tobacco shred flavoring, cigarette auxiliary material flavoring and the like, but the two flavoring technologies have obvious defects, for example, the fragrance is gradually weakened along with the time, so that the cigarette quality is reduced. The cigarette auxiliary material is flavored mainly by adding flavor-carrying core wires, particles, capsules (popping beads) and the like into the filter stick. The soft capsule for cigarettes is a cigarette flavoring mode popular in the industry in recent years, a certain amount of essence for cigarettes is sealed in a spherical soft capsule through a certain means, and then the capsule for cigarettes is added into a cigarette filter stick, so that a consumer can timely break the capsule to release aroma components in the smoking process, and the effects of improving smoking taste, increasing taste and the like are achieved.
In the current market, most of the capsule wall materials are hydrophilic substances, and the core liquid almost has no exception and takes oil-soluble essence and lipid solvent as essence diluents. Therefore, it is a hot point to develop a technology capable of encapsulating water-soluble essence capsules, such as: CN 104305521A discloses a method for preparing a round capsule, which comprises coating aqueous solution with wax and coagulant aid as wall materials by cooling and coagulating, and then sequentially coating powder and hydrophilic film layer to make the capsule round; CN 201410059720 applied by tobacco industry llc in north of huo discloses a three-layer water capsule; CN 201510352940 applied by Limited liability company of cigarette industry in Yunnan discloses a preparation method of a composite encapsulation capsule, which uses an amphiphilic natural polymer material to directly wrap water or an aqueous solution to prepare a soft capsule with a water-in-inner layer.
However, although the oil-containing capsule in the prior art forms a mature technology, the wall material of the oil-containing capsule is limited, so that the oil-containing capsule cannot be used for coating a core liquid with a water-soluble component; and the industry has not appeared a reliable water-containing capsule technology which can form industrialization. The invention organically combines the characteristics of the oil-containing capsule and the water-containing capsule, overcomes the defects of the oil-containing capsule and the water-containing capsule, realizes the simultaneous addition of oil-soluble essence and water-soluble essence, greatly widens the material selection range of the essence, and enriches the flavor blending and application of the capsule for cigarettes.
The invention discloses a preparation method of a cigarette capsule taking water-in-oil microemulsion as core liquid, which is used for preparing various types of nano-particles or microcapsules, wherein the microemulsion is increasingly focused on various industries in recent years, CN 101167706A, CN 101811014A, CN 102601833A, EP 1021085A 1 takes the emulsion as a dispersion system for preparing various types of nano-particles or microcapsules, CN201310123729, CN201610070603 and CN201610070602 disclose that water-based substances and oil-based substances are combined together in the form of microemulsion in the cosmetic field, and the microemulsions disclosed by CN201510495025, CN 201508249 and CN201310163543 are used in the food industry, but the microemulsions have not yet realized relevant application in the cigarette industry.
Disclosure of Invention
In order to solve the technical problems, the invention provides a novel cigarette capsule containing oil-soluble essence and water-soluble essence and a preparation method thereof.
The invention organically combines the characteristics of the oil-containing capsule and the water-containing capsule, can realize the simultaneous addition of oil-soluble essence and water-soluble essence, greatly widens the material selection range of the essence, and enriches the flavor blending and application range of the capsule for cigarettes.
In one aspect of the invention, the novel capsule for the cigarette is provided, the novel capsule for the cigarette is composed of 10-30 parts by weight of capsule wall materials and 30-70 parts by weight of core materials, and the capsule is transparent or semitransparent elastic spheroids with the particle size of 2.5-4 mm. The bursting strength of the capsule is preferably 0.5-2.5kg, and the wall thickness of the capsule is preferably 0.1-0.5 mm.
According to a preferred embodiment of the invention, the capsule takes the water-in-oil reverse microemulsion as a core material and takes the biomass gum or the synthetic resin as a capsule wall material. The density of the water-in-oil reverse micelle microemulsion core material is preferably 0.8-1.1g/cm3And contains a compound surfactant, a cosurfactant, an oil phase, oil-soluble essence, water and water-soluble essence/alcohol-soluble essence.
Preferably, the water phase of the capsule core material water-in-oil type reverse microemulsion contains water, water-soluble essence/alcohol-soluble essence.
Preferably, the oil phase of the capsule core material water-in-oil reverse microemulsion contains oil and oil-soluble essence.
On the other hand, the invention also provides a preparation method of the capsule, which comprises the step of adding the prepared core material and wall material into a dripping pill device according to the proportion to form the capsule with the wall material wrapping the microemulsion core liquid.
According to a preferred embodiment of the invention, the water-in-oil reverse microemulsion core material can be prepared by the following steps: uniformly mixing the oily components, the oil-soluble essence and the compound surfactant according to a proportion to form an oil phase; uniformly mixing the cosurfactant, water and the water-soluble essence or the alcohol-soluble essence to form a water phase, dropwise adding the water phase into the oil phase dispersed by the normal ultrasound, and continuously dispersing (preferably for about 10min) after uniform mixing to form the transparent or semitransparent water-in-oil reverse microemulsion.
According to a preferred embodiment of the invention, the water-in-oil reverse microemulsion core material comprises the following components in percentage by mass: the oil phase comprises 30-70% of water phase and 70-30% of water phase, and comprises an oily component, oil-soluble essence and a compound surfactant; the water phase comprises water, water-soluble essence or alcohol-soluble essence, and cosurfactant.
According to a preferred embodiment of the invention, in the oil phase, the mass percentage of the oily component, the oil-soluble essence and the compound surfactant is 60-79%, 0.01-1% and 40-20%.
The oily component can be one or more of hydrocarbon oil, laurinol glyceride, isopropyl myristate, isopropyl palmitate, isooctyl palmitate, caprylic/capric glyceride, animal and vegetable oil, and silicone oil.
The compound surfactant can be one or more of soybean phospholipid, sorbitan sesquiglyceride, isostearic acid/diglycerol succinate, glyceryl trinexanoleate, Tween80 and Span 80.
The oil-soluble essence can be at least one of sweet orange oil, lemon oil, peppermint oil, olive oil, jasmine essential oil, oil-soluble coffee essence and various edible essences.
According to another preferred embodiment of the invention, the water phase component comprises 40-60% by mass of water, 0.01-20% by mass of water-soluble essence or alcohol-soluble essence and 40-20% by mass of cosurfactant.
The water-soluble essence can be one or more of honey, sweetener, tobacco extract, licorice extract, red date extract, fig extract, tea extract, hop extract, plum extract, blackcurrant extract, apple extract and the like.
The alcohol soluble essence can be at least one of furanone, damascenone, megastigmatrienone, cis-jasmone, solanone or methyl cyclopentenone, maltol or eugenol, dihydroactinidiolide or gamma-undecalactone, phenylacetaldehyde or vanillin, 2, 3-dimethylpyrazine or 2-acetylpyridine.
The cosurfactant may be at least one of propylene glycol, glycerol, ethanol, polyethylene glycol 400, phenethyl alcohol, etc.
According to another preferred embodiment of the invention, the preparation method of the biomass rubber wall material for the cigarette capsule comprises the following steps: weighing biomass glue with different components in proportion, adding the biomass glue into hot water at 60-80 ℃, continuously stirring, dissolving the biomass glue in water bath at 60-80 ℃ fully, and then preserving heat and standing to obtain the biomass glue wall material liquid.
The biomass wall material for the cigarette capsule can be as follows: one or more of gelatin, locust bean gum, xanthan gum, carrageenan, konjac gum, guar gum and starch.
According to a preferred embodiment of the present invention, the synthetic resin preparation method used for the capsule for tobacco comprises: mixing synthetic resin, copolymer and ketone compound at a certain proportion, heating at 50-60 deg.C, stirring, standing for more than 2 hr, cooling, removing bubbles, and storing in dark place to obtain the capsule wall material solution.
According to another preferred embodiment of the invention, the synthetic resin wall material for the cigarette capsule comprises bisphenol A epoxy acrylic resin, other resins and/or ketone compounds.
The other resin can comprise one or more of acrylic resin, PE, pinene resin, phenolic epoxy acrylic resin, epoxidized oil acrylate, aromatic and aliphatic polyurethane acrylic resin, polyester acrylic resin, amino acrylic resin, maleic anhydride copolymer and ketone compound.
The ketone compound can be one or more of 2-hydroxy-2-methyl-1-phenyl-ketone, 1-hydroxycyclohexyl phenyl ketone, 2-methyl-2- (4-morpholinyl) -1- [4- (methylthio) phenyl ] -1-acetone and 2-hydroxy-2-methyl-1- [4- (2-hydroxyethoxy) phenyl ] -1-acetone. The ketone compound is used as a cross-linking agent of the synthetic resin to promote the curing and molding of the capsule.
In a particularly preferred embodiment, the capsule for cigarette of the invention is carried out by a capsule dripping method (biomass gum can be preferably used as a wall material), and the capsule dripping method comprises the following steps: the prepared core material and wall material liquid are respectively filled into a core liquid tank and a glue pot according to the proportion of 70-90% and 10-30%, the capsule wall material liquid and the microemulsion core liquid are dripped into cooling oil at the temperature of 10-20 ℃ by a constant delivery pump through a concentric circular dripper of a dripping pill device, the core liquid is shrunk into a spherical shape under the action of internal polymerization, the outer layer wraps the wall material liquid, the spherical shape is slowly dropped in protective liquid, the capsule wall material liquid is gradually cooled and solidified and formed in the dropping process, water-in-oil reverse microemulsion core liquid is hermetically wrapped, then a screen is used for separating a wet capsule from the protective liquid, the collected wet capsule uses oil absorption paper to absorb surface oil and then is thrown into a rotating cage, the capsule wall material liquid is dried at 300rpm for 4-10h, the drying is accelerated by using a fan during the period, the drying of the glue skin is completed, the dried capsule is taken out and rinsed twice by pure alcohol and then is placed in a ventilating place for 1-2h, and the alcohol is volatilized to obtain the biomass glue.
The cooling liquid can be at least one of water, propylene glycol, glycerol, sorbitol, silicone oil, rapeseed oil, paraffin oil and mineral oil.
According to another preferred mode of the invention, the capsule for cigarettes of the invention is carried out by a capsule dropping method (which can preferably adopt a synthetic resin formulation as a wall material), and the capsule dropping method comprises the following steps: respectively filling prepared core material and wall material liquid into a core liquid tank and a glue pot according to the proportion of 70-90% and 10-30%, dripping the prepared capsule wall material liquid and the prepared water-in-oil reversed-phase microemulsion liquid core liquid into a protective liquid through a concentric circle dropper of a pill dropping device by a quantitative pump, shrinking the core liquid into a spherical shape under the action of internal polymerization force, wrapping the wall material liquid at the outer layer, forming a spherical shape by the two, slowly dropping the spherical shape in the protective liquid, applying light source irradiation in the dropping process, gradually finishing cross-linking, curing, wrapping and sealing the core liquid to form a capsule under the action of single or common factors of illumination and cooling, then separating and collecting the capsule and the protective liquid by using a screen, washing by using an ethanol solution with the concentration of 90% by volume, and air-drying to obtain the synthetic resin wall material-microemulsion core material capsule.
The light source is at least one of a fluorescent lamp, an incandescent lamp, an ultraviolet lamp, an LED lamp or a searchlight with the power of 50-1000 w.
Compared with the prior art, the capsule for the cigarette prepared by the invention can well wrap the water-soluble essence, the alcohol-soluble essence and the oil-soluble essence, and the obtained capsule core material has stable property, good water locking performance of the wall material and moderate pressure value. The capsule can enrich the fragrance of the cigarette capsule to a great extent, increase the smoke moistening feeling to a certain extent and improve the smoking quality of cigarettes; and the preparation process is simple and easy to implement, the material is safe and environment-friendly, and the method is suitable for continuous industrial production.
Detailed Description
The present invention will be described in more detail below with reference to specific embodiments, but the embodiments of the present invention are not limited to the following embodiments.
Example 1
The diameter of the capsule for cigarettes is 3.5-4.0mm, the capsule is a mint-kiwi fruit flavor capsule, and the wall material is biomass glue. Wherein the core material accounts for 90% of the capsule proportion, and the rubber needs to be dried subsequently.
The preparation method comprises the following steps:
preparing a capsule core material: uniformly mixing isopropyl palmitate, peppermint oil, soybean phospholipid and ethanol according to a weight ratio of 100:20:17:13 to form a solution A, preparing water, dihydroactinidiolide and n-butyl alcohol according to a mass ratio of 10:1:6 to form a solution B, and uniformly mixing the A, B solution according to a mass ratio of 5:3 to form transparent or semitransparent water-in-oil reverse microemulsion.
Preparing a capsule wall material: preparing carrageenan, locust bean gum, guar gum and starch into uniformly mixed powder according to the mass ratio of 1:1:0.5:0.1, continuously stirring, uniformly dispersing in hot water, keeping the mass ratio of the powder to the water of 1:70, and preserving the heat at 80 ℃.
And (3) dropping to form: respectively filling the prepared core material and wall material liquid into a glue pot and a core liquid pot of a pill dropping machine according to the mass ratio of 3:1, dripping the prepared capsule wall material liquid and the water-in-oil reverse microemulsion liquid core into cooling oil at the temperature of 10-20 ℃ by a quantitative pump through concentric circle drippers of a pill dropping device, gradually cooling and solidifying the capsule in the falling process, hermetically wrapping the water-in-oil reverse microemulsion liquid core, and adjusting the parameters of equipment to ensure that the particle size of the capsule is between 3.5-4.0 mm.
And (3) drying: separating the wet capsules from the protective liquid by using a screen, sucking surface oil of the collected wet capsules by using oil absorption paper, putting the wet capsules into a rotating cage, drying at 200-300rpm for 4-10h, blowing air by using a fan to accelerate drying, taking out the dried capsules, rinsing the dried capsules with alcohol for two times, putting the capsules in a ventilation place for 1-2h, and volatilizing the alcohol to obtain a biomass capsule wall material-microemulsion core material capsule sample.
Example 2
The capsule for cigarette of the embodiment has a diameter of 2.5-3.0mm, and is a sweet orange-honey flavor capsule, and the wall material is synthetic resin, wherein the core material accounts for about 85%.
The preparation method comprises the following steps:
preparing a capsule core material: uniformly mixing cyclohexane, sweet orange oil, sorbitan sesquioleate and n-butanol according to the weight ratio of 100:15:22:15 to form a solution A, water, honey and PEG-400 according to the mass ratio: preparing solution B from the mixture at a ratio of 12:1:8, and uniformly mixing the A, B solution at a ratio of 3:2 to form transparent or semitransparent water-in-oil reverse microemulsion.
Preparing a capsule wall material: uniformly mixing bisphenol A epoxy resin and acrylic resin in a mass ratio of 1:1.5, adding 0.05 mass percent of 1-hydroxycyclohexyl phenyl ketone, heating at the temperature of 50 ℃, and storing in a dark place.
And (3) dropping to form: the prepared core material and wall material liquid are respectively filled into a glue pot and a core liquid tank of a pill dropping machine according to the mass ratio of 6:1, the prepared capsule wall material liquid and the water-in-oil reverse microemulsion liquid core are dripped into cooling oil at the temperature of 10-20 ℃ by a quantitative pump through concentric circle drippers of a pill dropping device, the capsule wall material is gradually cooled and solidified to form after being irradiated by an external light source in the falling process, the water-in-oil reverse microemulsion liquid core is hermetically wrapped, and the size of the capsule is adjusted within the range of 2.5-3.0mm by adjusting equipment parameters. And collecting the obtained capsule, namely the synthetic resin wall material-microemulsion core material capsule sample.
Example 3
In the embodiment, the diameter of the capsule for cigarettes is 2.5-3.0mm, the capsule is a lemon-lavender flavor capsule, the wall material is biomass glue, and the core material accounts for about 85% of the proportion of the capsule.
The preparation method comprises the following steps:
preparing a capsule core material: uniformly mixing glycerol triacetate, lemon oil, Tween80 and Span80 according to the weight ratio of 98:12:18:16 to form a solution A; water, lavender extract and n-amyl alcohol in a mass ratio of: 12:0.5:6 to form a solution B, and uniformly mixing the A, B solution according to the ratio of 4:3 to form transparent or semitransparent water-in-oil reverse microemulsion;
preparing a capsule wall material: preparing gelatin, carrageenan, guar gum and starch into uniformly mixed powder according to the mass ratio of 3:1:0.5:0.2, continuously stirring, uniformly dispersing in hot water, keeping the mass ratio of the powder to the water of 1:65, and preserving the heat at 80 ℃.
And (3) dropping to form: the prepared core material and wall material liquid are respectively filled into a glue pot and a core liquid tank of a pill dropping machine according to the mass ratio of 3.5:1, the prepared capsule wall material liquid and the water-in-oil reverse microemulsion liquid core are dripped into cooling oil at the temperature of 10-20 ℃ by a quantitative pump through concentric circle drippers of a pill dropping device, the capsule is gradually cooled, solidified and formed in the falling process, the water-in-oil reverse microemulsion liquid core is hermetically wrapped, and the particle size of the capsule is between 2.5-3.0mm by adjusting equipment parameters.
And (3) drying: separating the wet capsule from the protective liquid by using a screen, sucking surface oil in the collected wet capsule by using oil absorption paper, putting the wet capsule into a rotating cage, drying the wet capsule at the speed of 300rpm for 4 to 10 hours at 200-10 rpm, blowing air by using a fan to accelerate drying during the drying process, taking out the dried capsule, rinsing the dried capsule by using alcohol twice, putting the capsule in a ventilation place for 1 to 2 hours, and volatilizing the alcohol to obtain a biomass capsule wall material-microemulsion core material capsule sample
Example 4
In the embodiment, the diameter of the capsule for cigarettes is 2.5-3.0mm, the capsule is a jasmine-aloe flavor capsule, the wall material is a biomass gel, and the core material accounts for about 85% of the proportion of the capsule.
The preparation method comprises the following steps:
preparing a capsule core material: uniformly mixing lauryl alcohol glyceride, jasmine essential oil, glyceryl triricinoleate and ethanol according to the weight ratio of 96:15:18:12 to form a solution A; water, aloe extract and propylene glycol according to the mass ratio: 12:1.5:5 to form a solution B, and evenly mixing the A, B solution according to the ratio of 4:3 to form transparent or semitransparent water-in-oil reverse microemulsion.
Preparing a capsule wall material: mixing konjac gum, guar gum and starch at a mass ratio of 5:2:0.2 to obtain uniformly mixed powder, continuously stirring, uniformly dispersing in hot water at a mass ratio of 1:70, and keeping the temperature at 80 ℃.
And (3) dropping to form: the prepared core material and wall material liquid are respectively filled into a glue pot and a core liquid tank of a pill dropping machine according to the mass ratio of 3.5:1, the prepared capsule wall material liquid and the water-in-oil reverse microemulsion liquid core are dripped into cooling oil at the temperature of 10-20 ℃ by a quantitative pump through concentric circle drippers of a pill dropping device, the capsule is gradually cooled, solidified and formed in the falling process, the water-in-oil reverse microemulsion liquid core is hermetically wrapped, and the particle size of the capsule is between 2.5-3.0mm by adjusting equipment parameters.
And (3) drying: separating the wet capsules from the protective liquid by using a screen, sucking surface oil of the collected wet capsules by using oil absorption paper, putting the wet capsules into a rotating cage, drying at 200-300rpm for 4-10h, blowing air by using a fan to accelerate drying, taking out the dried capsules, rinsing the dried capsules with alcohol for two times, putting the capsules in a ventilation place for 1-2h, and volatilizing the alcohol to obtain a biomass capsule wall material-microemulsion core material capsule sample.
Example 5
In the embodiment, the diameter of the capsule for cigarettes is 3.5-4.0mm, the capsule is an agilawood-tea fragrance capsule, the wall material is synthetic resin, and the core material accounts for about 90% of the weight of the capsule.
The preparation method comprises the following steps:
preparing a capsule core material: uniformly mixing isopropyl myristate, agilawood essence, isopropyl isostearate and Span80 according to a weight ratio of 96:5:22:15 to form a solution A; water, tea extract and isoamylol according to the mass ratio: 12:1.5:5 to form a solution B, and evenly mixing the A, B solution according to the ratio of 4:3 to form transparent or semitransparent water-in-oil reverse microemulsion.
Preparing a capsule wall material: the phenolic epoxy acrylic resin, the epoxidized oil acrylate and the linear low-density polyethylene are prepared according to the mass ratio of 3:2:0.5, are uniformly mixed, are heated at the temperature of 110 ℃, and are preserved under heat.
And (3) dropping to form: the prepared core material and wall material liquid are respectively filled into a glue pot and a core liquid tank of a pill dropping machine according to the mass ratio of 6:1, the prepared capsule wall material liquid and the water-in-oil reverse microemulsion liquid core are dripped into cooling oil at the temperature of 10-20 ℃ by a quantitative pump through concentric circle drippers of a pill dropping device, the capsule wall material is gradually cooled, solidified and formed in the falling process, the water-in-oil reverse microemulsion liquid core is hermetically wrapped, and the size of the capsule is adjusted within the range of 2.5-3.0mm by adjusting equipment parameters. And collecting the prepared capsule to obtain a synthetic resin wall material-microemulsion core material capsule sample.
Example 6
In the embodiment, the capsule for cigarettes is 3.5-40mm in diameter, is a dendrobium-tobacco capsule, the wall material is synthetic resin, and the core material accounts for about 90% of the capsule in proportion.
The preparation method comprises the following steps:
preparing a capsule core material: uniformly mixing caprylic acid/capric acid triglyceride, dendrobium essence, oleate and Tween80 according to the weight ratio of 96:10:22:15 to form a solution A; water, tobacco extract and isoamylol according to the mass ratio: preparing solution B from 15:2:3, and uniformly mixing the A, B solution according to the ratio of 4:3 to form transparent or semitransparent water-in-oil reverse microemulsion.
Preparing a capsule wall material: uniformly mixing aliphatic polyurethane acrylic resin, polyester acrylic resin and amino acrylic resin according to the mass ratio of 3:2:0.5, adding 0.03% of 2-hydroxy-2-methyl-1-phenyl-ketone by mass percent, stirring and heating at the temperature of 50 ℃, and storing in a dark place.
And (3) dropping to form: the prepared core material and wall material liquid are respectively filled into a glue pot and a core liquid tank of a pill dropping machine according to the mass ratio of 6:1, the prepared capsule wall material liquid and the water-in-oil reverse microemulsion liquid core are dripped into medium oil by a quantitative pump through concentric circle drippers of a pill dropping device, the capsule wall material is gradually solidified and formed under the irradiation of an external light source in the falling process, the water-in-oil reverse microemulsion liquid core is hermetically wrapped, and the size of the capsule is adjusted within the range of 3.5-4.0mm by adjusting equipment parameters. And collecting the prepared capsule to obtain a synthetic resin wall material-microemulsion core material capsule sample.
This written description uses examples to disclose the invention, including the best mode, and also to enable any person skilled in the art to make and use the invention. The patentable scope of the invention is defined by the claims, and not by the limitations of the claims. Such other examples are intended to be within the scope of the claims if they have structural elements that do not differ from the literal language of the claims, or if they include equivalent structural elements with insubstantial differences from the literal languages of the claims. All citations referred to herein are incorporated herein by reference to the extent that no inconsistency is made.