CN113025425A - Perfuming microcapsule particle for cigarette, preparation method thereof and application of perfuming microcapsule particle in cigarette - Google Patents

Perfuming microcapsule particle for cigarette, preparation method thereof and application of perfuming microcapsule particle in cigarette Download PDF

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Publication number
CN113025425A
CN113025425A CN201911348567.7A CN201911348567A CN113025425A CN 113025425 A CN113025425 A CN 113025425A CN 201911348567 A CN201911348567 A CN 201911348567A CN 113025425 A CN113025425 A CN 113025425A
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parts
weight
perfuming
particles
essence
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CN201911348567.7A
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Inventor
吴志伟
凌孝存
邹兴平
郝天翊
张少瀚
叶晓青
吕乔
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Shenzhen Boton Flavors & Fragrances Co ltd
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Shenzhen Boton Flavors & Fragrances Co ltd
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Priority to CN201911348567.7A priority Critical patent/CN113025425A/en
Publication of CN113025425A publication Critical patent/CN113025425A/en
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    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B9/00Essential oils; Perfumes
    • C11B9/0003Compounds of unspecified constitution defined by the chemical reaction for their preparation
    • AHUMAN NECESSITIES
    • A24TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
    • A24DCIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
    • A24D3/00Tobacco smoke filters, e.g. filter-tips, filtering inserts; Filters specially adapted for simulated smoking devices; Mouthpieces for cigars or cigarettes
    • A24D3/02Manufacture of tobacco smoke filters
    • A24D3/0204Preliminary operations before the filter rod forming process, e.g. crimping, blooming
    • A24D3/0212Applying additives to filter materials
    • A24D3/0216Applying additives to filter materials the additive being in the form of capsules, beads or the like
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J13/00Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
    • B01J13/02Making microcapsules or microballoons
    • B01J13/04Making microcapsules or microballoons by physical processes, e.g. drying, spraying
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J13/00Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
    • B01J13/02Making microcapsules or microballoons
    • B01J13/04Making microcapsules or microballoons by physical processes, e.g. drying, spraying
    • B01J13/043Drying and spraying
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B9/00Essential oils; Perfumes
    • C11B9/0007Aliphatic compounds
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B9/00Essential oils; Perfumes
    • C11B9/0007Aliphatic compounds
    • C11B9/0015Aliphatic compounds containing oxygen as the only heteroatom

Abstract

The invention discloses perfuming microcapsule particles for cigarettes and a preparation method and application thereof in cigarettes, and the perfuming microcapsule particles are prepared by sequentially weighing 25-28 parts by weight of modified starch, 5.5-7.5 parts by weight of sodium caseinate, 22-25 parts by weight of maltodextrin, 6-9 parts by weight of beta-cyclodextrin, 5-7 parts by weight of Arabic gum, 4.5-7.5 parts by weight of glucose, 1-2 parts by weight of sucrose ester and 160 parts by weight of 120-plus-material water, shearing the particles by a water bath heating high-speed shearing machine, and dissolving wall materials to prepare wall material solution; adding 80-85 parts of essence into the wall material solution, heating in a water bath, shearing at a high speed, and mixing uniformly; after being stirred uniformly, the emulsion is homogenized and emulsified by a high-pressure homogenizer to prepare the emulsion; adding the emulsified emulsion into a filler of 118-146 parts of lactose and 175 parts of microcrystalline cellulose, and uniformly mixing to obtain a wet soft material; extruding and rounding to obtain the flavoring particles; the essence in the flavoring particles for the cigarettes is in a microcapsule state and plays a role in slow release of fragrance in the storage and use processes; the loss of essence content is less; the material is easy to obtain, the preparation process is simple and stable, and the method is suitable for large-scale industrial production.

Description

Perfuming microcapsule particle for cigarette, preparation method thereof and application of perfuming microcapsule particle in cigarette
Technical Field
The invention relates to the technical field of tobacco product flavoring, in particular to a flavoring microcapsule particle for cigarettes, a preparation method thereof and application thereof in cigarettes.
Background
Tobacco products usually adopt a flavoring method to achieve the purposes of improving the aroma characteristics of cigarettes, covering up miscellaneous flavors and endowing cigarettes with unique styles, thereby becoming an indispensable part in the tobacco industry. The cigarette flavor has the advantages that the stability and the persistence of the cigarette flavor are the same when a formula is continuously improved and novel cigarette flavor is developed, and the cigarette flavor is the focus of attention of scientific research personnel in scientific research institutions and enterprises. Most of the fragrant raw materials have low boiling points and are extremely easy to volatilize, the loss is serious in the long-term storage process, and because the cigarettes belong to the use characteristics of high-temperature smoking, the hot smoke can release the spices in the cigarettes in advance, so that the phenomena of thick fragrance in the early stage and slight fragrance release in the later stage are caused, and the product consumption quality is reduced.
The microcapsule technology is an important means for improving the stability of the essence, and a natural or synthetic high molecular compound is adopted to form a continuous film (wall or external phase) to completely coat the fragrant raw material (core material or internal phase) to be protected, so that the volatilization and dissipation of the fragrant components can be effectively prevented, meanwhile, the contact with the outside is isolated, the deterioration caused by chemical change is slowed down, and the stability of the fragrance material is improved.
However, in the existing manufacturing technology, when a manufacturer produces perfuming microcapsules, the manufacturer needs to purchase powder essence with smaller particle size from a corresponding upstream manufacturer, and then carries out secondary processing to obtain microcapsule particles, a transportation process and a storage process exist between the powder essence and the microcapsule particles, and the two processes can generate certain fragrance dissipation and moisture for the essence; moreover, the secondary processing requires a drying process, which completely fails to ensure the preservation of aroma components, so that smokers can feel no smell after smoking a mouth, and avoid worry 25041.
For example, the document of application No. CN201310488863.3 discloses a method for preparing microcapsule essence particles by wet granulation, which organically combines the microencapsulation technology and wet fluidized drying one-step granulation, and produces microcapsule essence particles with particle distribution of 20-100 meshes by groping of process conditions, selection of raw and auxiliary materials, adjustment of formula and control of yield, thereby overcoming the mutual influence of production processes and solving the contradiction between the raw and auxiliary materials of essence and the processes; however, the wet-method boiling drying temperature is high, which is not beneficial to the preservation of aroma components, and the granules prepared by the filler carboxymethyl cellulose and maltodextrin are sticky, and the granule forming effect is not good. Therefore, a process method which has more complete process, high fragrance and obvious particle fragrance and is suitable for large-scale production is urgently needed for manufacturers; and the micro-pills loaded with the fragrant substances in a certain amount or weight are only needed to be added into the cigarette filter, and the fragrant substances are released when the main stream smoke of the cigarette passes through, so that the aim of perfuming the filter is fulfilled, and the smoke volume and the richness of the cigarette are effectively improved.
Disclosure of Invention
Aiming at the defects in the technology, the invention provides the perfuming microcapsule particle for the cigarette and the preparation method thereof, the perfuming microcapsule particle can be used in the cigarette, more particularly can be added in a cigarette filter stick, and the microcapsule has rich and obvious fragrance; the storage is facilitated, and the overall process is simple; and the particle size is uniform and the particle fragrance is obvious only for the microcapsule.
In order to achieve the aim, the invention provides perfuming microcapsule particles for cigarettes, which comprise a composite wall material and a solid filler, wherein the composite wall material can be emulsified and embedded with an essence core material to form an oil-in-water film;
the composite wall material comprises the following components in parts by weight: 25-28 parts of modified starch, 5.5-7.5 parts of sodium caseinate, 22-25 parts of maltodextrin, 6-9 parts of beta-cyclodextrin, 5-7 parts of Arabic gum, 4.5-7.5 parts of glucose and 1-2 parts of sucrose ester;
80-85 parts of an essence core material which is oil-soluble essence;
the solid filler comprises the following components in parts by weight: lactose 118-146 parts and microcrystalline cellulose 146-175 parts.
Preferably, the composite wall material comprises the following components in parts by weight: 26-28 parts of modified starch, 5.5-7.5 parts of sodium caseinate, 22-25 parts of maltodextrin, 6-9 parts of beta-cyclodextrin, 5-7 parts of Arabic gum, 4.5-7.5 parts of glucose and 1-2 parts of sucrose ester;
80-85 parts of the essence core material;
the solid filler comprises the following components in parts by weight: 118 parts of lactose and 175 parts of microcrystalline cellulose.
Preferably, the composite wall material comprises the following components in parts by weight: 28 parts of modified starch, 5.5 parts of sodium caseinate, 22 parts of maltodextrin, 6 parts of beta-cyclodextrin, 7 parts of Arabic gum, 4.5 parts of glucose and 1 part of sucrose ester;
85 parts of the essence core material;
the solid filler comprises the following components in parts by weight: 118 parts of lactose and 175 parts of microcrystalline cellulose.
The invention also provides a preparation method of the flavoring microcapsule granules for cigarettes, which comprises the following steps:
(1) weighing 25-28 parts of modified starch, 5.5-7.5 parts of sodium caseinate, 22-25 parts of maltodextrin, 6-9 parts of beta-cyclodextrin, 5-7 parts of Arabic gum, 4.5-7.5 parts of glucose and 1-2 parts of sucrose ester in sequence according to parts by weight; dissolving the wall material in 160 parts of water by using a water bath heating high-speed shearing machine to obtain a wall material solution A;
(2) weighing 80-85 parts of essence core materials, adding the essence core materials into the wall material solution A obtained in the step (1), and uniformly mixing under water bath heating and high-speed shearing; then homogenizing and emulsifying by a high-pressure homogenizer to obtain emulsion B;
(3) weighing 118-146 parts of lactose and 146-175 parts of microcrystalline cellulose; adding the emulsion B prepared in the step (2) into lactose and microcrystalline cellulose, and uniformly mixing to prepare a wet soft material C;
(4) and (3) putting the wet soft material C obtained in the step (3) into a screen, performing extrusion molding by using an extrusion rounding machine to obtain a strip-shaped material D, putting the strip-shaped material D into the rounding machine to form spherical particles, and taking out the wet particles after shaping to dry to obtain the perfuming liquid microcapsule E.
Preferably, in the step (1), the water bath heating temperature is in the range of 50-60 ℃ and the time is 30-40 min.
Preferably, the specific conditions of high-speed shearing in the step (2) are as follows: the shearing speed is 8000-12000rpm, and the time is 15-25 min; wherein the homogenization pressure and times are as follows: the pressure is 1000-1200bar, and the homogenizing and emulsifying times are 3-4 times.
Preferably, in the step (4), the aperture of the screen mesh is 0.2-0.4 mm; the rounding machine has the following specific conditions: the rotating speed range is 200-600 r/min.
Preferably, the grain diameter of the flavoring microcapsule granules for cigarettes obtained by screening is 40-100 meshes.
Preferably, in step (4), the drying conditions are: and the temperature is 20-25 ℃.
The invention also discloses an application of the flavoring microcapsule particles for cigarettes in cigarette filters, which comprises the prepared flavoring liquid microcapsule, wherein the prepared flavoring liquid microcapsule is added into the cigarette filters.
The invention has the beneficial effects that: compared with the prior art, the flavoring microcapsule particle for the cigarettes and the preparation method thereof and the application in the cigarettes have the following beneficial effects:
(1) the invention provides a preparation method of flavoring particles for cigarettes and application of the flavoring particles in cigarette filters.
(2) In the using process, only a certain amount or weight of particles loaded with fragrant substances are needed to be added into the cigarette filter, and the fragrant substances are released when the mainstream smoke of the cigarette passes through, so that the aim of perfuming the filter is fulfilled, and the smoke volume and the richness of the cigarette are effectively improved;
(3) the essence in the prepared flavoring particles for cigarettes is in a microcapsule state, and can play a role in slow release of fragrance in the storage and use processes;
(4) the emulsified essence is mixed with a filler and then extruded into a ball (dried at room temperature of 25 ℃) so that the essence content loss is less. The material is wet particles in the production process, the generated dust is less, the environment is friendly, the particle size is uniform, the fluidity is good, and the fragrance of the particles is obvious.
Drawings
FIG. 1 is a diagram of a substance of a granule of a perfuming microcapsule for tobacco prepared in example 1 of the present invention;
FIG. 2 is a 500 times enlarged view of a perfuming microcapsule granule for tobacco prepared in example 1 of the present invention;
FIG. 3 is a gas detection chromatogram of example 1 and comparative examples 1 and 2 of the present invention.
Detailed Description
In order to more clearly express the present invention, the present invention will be further described below with reference to examples.
The invention discloses a perfuming microcapsule particle for cigarettes, which comprises a composite wall material, an essence core material and a filler; the composite wall material can be emulsified and embedded with the essence core material to form an oil-in-water film with certain strength; the filler can stably adhere or adsorb the emulsion formed by the wall material and the essence core material, and has certain anti-collapse performance. The composite wall material comprises the following components in parts by weight: 25-28 parts of modified starch, 5.5-7.5 parts of sodium caseinate, 22-25 parts of maltodextrin, 6-9 parts of beta-cyclodextrin, 5-7 parts of Arabic gum, 4.5-7.5 parts of glucose and 1-2 parts of sucrose ester;
modified starch models include, but are not limited to, national starch HI-CAP100, French Roguet CO01, national TWS 502; maltodextrin types included: but are not limited to, a degree of hydrolysis DE value of 5-10, 10-15, 15-20; modified starch and maltodextrin are emulsified, and the spray drying method can achieve high drying efficiency and high powder yield, and the material process in the drying process cannot exceed the wet bulb temperature of the surrounding hot air, so the method is suitable for the drying mode. Sources of sodium caseinate include, but are not limited to, new zealand Milk Products, new zealand permanent; the beta-cyclodextrin, the Arabic gum, the glucose and the sucrose ester are sourced from domestic high-quality manufacturers. The interaction of the sodium caseinate and the Arabic gum constructs a carrier material of the nanoparticles, so that the carrier material has more outstanding bearing effect and targeted delivery effect on the embedded active substances, and can realize the slow release and controlled release of the active substances, and the perfuming particles in the cigarette industry are established.
The essence core material is specifically oil-soluble essence, and the weight parts of the essence core material are 80-85 parts; not limited to milk-flavored essences, coffee essences, chocolate essences, citrus essences, mint essences, spearmint essences, fruit essences, or various natural essential oils and various savory essences;
the filler comprises the following components in parts by weight: lactose 118-146 parts and microcrystalline cellulose 146-175 parts.
Selecting specific edible materials for compounding, mainly preparing modified starch, sodium caseinate, maltodextrin, beta-cyclodextrin, Arabic gum, glucose and sucrose ester into a solution, forming an emulsion with an essence core material to form a composite wall material for wrapping essence, and then adsorbing the composite wall material by fillers such as lactose, microcrystalline cellulose and the like; drying to form the perfuming liquid microcapsule. The adopted modified starch, maltodextrin, sodium caseinate and Arabic gum respectively adopt a compounding and complex coacervation method, and play a key role in microencapsulation of the essence and the spice. The filler adopts lactose and microcrystalline cellulose, so that the particles are not adhered; in the prior art, the microcapsules prepared by adopting carboxymethyl cellulose and maltodextrin as filling agents are sticky, and the granule forming effect is poor; the uniformity of particle size was not good. Therefore, the prepared finished product has good fragrance slow-release effect, is beneficial to storage and is suitable for industrial large-scale production.
Based on the selection and matching of the materials, the invention adopts a more suitable preparation method to ensure the slow release of the fragrance and the uniformity of the grain diameter; the method specifically comprises the following steps:
(1) weighing 25-28 parts of modified starch, 5.5-7.5 parts of sodium caseinate, 22-25 parts of maltodextrin, 6-9 parts of beta-cyclodextrin, 5-7 parts of Arabic gum, 4.5-7.5 parts of glucose and 1-2 parts of sucrose ester in sequence according to parts by weight; dissolving the wall material in 160 parts of water by using a water bath heating high-speed shearing machine to obtain a wall material solution A; wherein the water bath heating temperature range is 50-60 ℃, the time is 30-40min, and the shearing speed is 8000-12000 rpm; wherein the water bath heating equipment can adopt a constant temperature water bath kettle;
(2) weighing 80-85 parts of essence core material, adding the essence core material into the wall material solution A obtained in the step (1), and uniformly mixing under water bath heating and high-speed shearing, wherein the shearing speed is 8000-; the shears may use, for example, an IKA-T18 shear; then homogenizing and emulsifying by a high-pressure homogenizer to obtain emulsion B; wherein the homogenizing pressure and times are as follows: the pressure is 1000-1200bar, and the homogenizing and emulsifying times are 3-4 times; the homogenizer may use, for example, an ATS homogenizer; the dissolution speed is proper, and the material is stable;
(3) weighing 118-146 parts of lactose and 146-175 parts of microcrystalline cellulose; adding the emulsion B prepared in the step (2) into lactose and microcrystalline cellulose, and uniformly mixing to prepare a wet soft material C;
(4) putting the wet soft material C obtained in the step (3) into a screen mesh, and performing extrusion molding by using an extrusion rounding machine to obtain a strip-shaped material D, wherein the aperture of the screen mesh is 0.2-0.4 mm; and then placing the strip material D in a rounding machine to form spherical particles, wherein the rounding machine has the specific conditions that: the rotating speed range is 200-600 r/min; after shaping, taking out the wet particles, and drying at the ambient temperature of 20-25 ℃ to obtain a perfuming liquid microcapsule E; and (3) putting the wet soft material into a screen, performing extrusion molding by using a basic rounding machine to obtain small segments of powder particles, putting the small segments of powder particles into the rounding machine to form spherical particles, taking out the wet particles after shaping, and drying the wet particles at the ambient temperature of 20-25 ℃ to obtain the flavoring particles. The whole preparation process does not adopt a high-temperature drying technology; the center of the prior art is heated and dried at high temperature to prepare powder essence, and then the powder essence is granulated by a wet method, so that the preparation method completely destroys the fragrance of the essence, and is very not beneficial to the preparation of the variety, concentration and harmony of the essence and the fragrance preservation; the preparation method is to prepare the microcapsule nano emulsion on site, does not need high-temperature drying, is directly dried at room temperature after wet granulation, has milder processing conditions, and can reduce the possible adverse effect of the processing process on the essence.
Example 1
Preparation of perfuming microcapsule particle 1 for cigarette
(1) Taking 28 parts by weight of modified starch, 22 parts by weight of maltodextrin, 6 parts by weight of cyclodextrin, 5.5 parts by weight of sodium caseinate, 7 parts by weight of Arabic gum, 4.5 parts by weight of glucose, 1 part by weight of sucrose ester and 120 parts by weight of water, and shearing and stirring for 30min at the rotating speed of 8000rpm in a water bath at 50 ℃ to prepare a wall material solution;
(2) adding 85 parts by weight of dried orange peel essence into the wall material solution, and continuously shearing and stirring for 15min in a water bath at 50 ℃ and at the rotating speed of 8000rpm to fully and uniformly mix the dried orange peel essence;
(3) homogenizing and emulsifying the emulsion obtained in the step 2 for 3 times under the pressure of 1000bar of a high-pressure homogenizer to obtain nano emulsion;
(4) adding the nano emulsion obtained in the step 3 into a filler containing 118 parts of lactose and 175 parts of microcrystalline cellulose, and uniformly mixing to obtain a wet soft material;
(5) and (3) putting the wet soft material obtained in the step (4) into a screen with the thickness of 0.3mm, extruding and molding by using an extrusion spheronizer at the extrusion speed of 30r/min to obtain fine powder particles, putting the prepared small powder particles into the spheronizer with the rotation speed set to 200r/min to form spherical particles, taking out the wet particles after shaping, and drying the wet particles at the room temperature of 25 ℃ for 24 hours to obtain the flavoring microcapsule particles 1 for the cigarettes.
Example 2
Preparation of perfuming microcapsule particle 2 for cigarette
(1) Taking 28 parts by weight of modified starch, 22 parts by weight of maltodextrin, 6 parts by weight of cyclodextrin, 5.5 parts by weight of sodium caseinate, 7 parts by weight of Arabic gum, 4.5 parts by weight of glucose, 1 part by weight of sucrose ester and 120 parts by weight of water, and shearing and stirring for 30min at the rotating speed of 8000rpm in a water bath at 50 ℃ to prepare a wall material solution;
(2) adding 85 parts by weight of dried orange peel essence into the wall material solution, and continuously shearing and stirring for 15min in a water bath at 50 ℃ and at the rotating speed of 8000rpm to fully and uniformly mix the dried orange peel essence;
(3) homogenizing and emulsifying the emulsion obtained in the step 2 for 3 times under the pressure of 1000bar of a high-pressure homogenizer to obtain nano emulsion;
(4) adding the nano emulsion obtained in the step 3 into a filler containing 118 parts of lactose and 175 parts of microcrystalline cellulose, and uniformly mixing to obtain a wet soft material;
(5) and (3) putting the wet soft material obtained in the step (4) into a screen with the thickness of 0.3mm, extruding and molding by using an extrusion spheronizer at the extrusion speed of 30r/min to obtain fine powder particles, putting the prepared small powder particles into the spheronizer with the rotation speed set to 200r/min to form spherical particles, taking out the wet particles after shaping, and drying the wet particles at the room temperature of 25 ℃ for 24 hours to obtain the flavoring microcapsule particles 2 for the cigarettes.
Example 3
Preparation of perfuming microcapsule particle 3 for cigarette
(1) Taking 26 parts by weight of modified starch, 24 parts by weight of maltodextrin, 8 parts by weight of cyclodextrin, 6 parts by weight of sodium caseinate, 6 parts by weight of Arabic gum, 5.5 parts by weight of glucose, 1.5 parts by weight of sucrose ester and 140 parts by weight of water, and shearing, stirring and dissolving for 35min in a 54 ℃ water bath at the rotating speed of 10000rpm to prepare a wall material solution;
(2) adding 83 parts by weight of dried orange peel essence into the wall material solution, and continuously shearing and stirring for 20min in 54 ℃ water bath at 10000rpm to fully mix the dried orange peel essence uniformly;
(3) homogenizing and emulsifying the emulsion obtained in the step 2 for 3 times under the pressure of 1100bar of a high-pressure homogenizer to obtain nano emulsion;
(4) adding the nano emulsion obtained in the step 3 into a filler containing 120 parts of lactose and 173 parts of microcrystalline cellulose, and uniformly mixing to obtain a wet soft material;
(5) and (3) putting the wet soft material in the step (4) into a screen with the thickness of 0.3mm, extruding and molding by using an extrusion spheronizer at the extrusion speed of 50r/min to obtain fine powder particles, putting the prepared small powder particles into the spheronizer with the rotation speed of 400r/min to form spherical particles, taking out the wet particles after shaping, and drying the wet particles at the room temperature of 25 ℃ for 30 hours to obtain the flavoring microcapsule particles 3 for the cigarettes.
Example 4
Preparation of perfuming microcapsule particle 4 for cigarette
(1) Taking 25 parts by weight of modified starch, 25 parts by weight of maltodextrin, 6 parts by weight of cyclodextrin, 7.5 parts by weight of sodium caseinate, 5 parts by weight of Arabic gum, 7.5 parts by weight of glucose, 2 parts by weight of sucrose ester and 160 parts by weight of water, shearing, stirring and dissolving at 50 ℃ and 8000rpm for 40min to prepare a wall material solution;
(2) adding 80 parts by weight of Tieguanyin tea essence into the wall material solution, and continuously shearing and stirring at 50 ℃ and 8000rpm for 15min to fully and uniformly mix the Tieguanyin tea essence;
(3) homogenizing and emulsifying the emulsion obtained in the step 2 for 3 times under the pressure of 1200bar of a high-pressure homogenizer to obtain nano emulsion;
(4) and (3) adding the nano emulsion obtained in the step (3) into a filler containing 118 parts of lactose and 175 parts of microcrystalline cellulose, and uniformly mixing to obtain a wet soft material.
(5) And (3) putting the wet soft material in the step (4) into a screen with the thickness of 0.3mm, extruding and molding by using an extrusion spheronizer at the extrusion speed of 30r/min to obtain fine powder particles, putting the prepared small powder particles into the spheronizer with the rotation speed set to 200r/min to form spherical particles, taking out the wet particles after shaping, and drying the wet particles at the room temperature of 25 ℃ for 24 hours to obtain the perfuming microcapsule particles for cigarettes (4).
The particle products obtained in examples 1 to 4 are detected by a scanning electron microscope to know the particle size of each flavoring particle, and then a 40-100 mesh screen is selected for sieving to obtain the flavoring particles for cigarettes in example 1, wherein the particle size of 90% or more of the flavoring particles for cigarettes in example 1 is between 40 and 100 meshes, the particle size of 92% or more of the flavoring particles for cigarettes in example 2 is between 40 and 100 meshes, the particle size of 91% or more of the flavoring particles for cigarettes in example 3 is between 40 and 100 meshes, and the particle size of 93% or more of the flavoring particles for cigarettes in example 4 is between 40 and 100 meshes, so that the particle size uniformity obtained by the preparation method disclosed by the invention is better as can be seen from examples 1 to 4. The perfuming liquid microcapsule 1 obtained in example 1 was observed by means of a microscope, referring to fig. 1 and 2, fig. 1 is a physical diagram of the corresponding perfuming liquid microcapsule 1, and fig. 2 is a 500-fold enlarged view of the perfuming liquid microcapsule 1.
0.05g of the flavoring liquid microcapsules prepared in the embodiments 1 to 4 are added into filter tow to obtain filter sticks 1 to 4, and a smoking panel consisting of 12 persons carries out formal smoking on the filter sticks 1 to 4, and meanwhile, sensory comfort is independently evaluated and compared with common cigarettes randomly available in the market; the results of the overall sensory tests obtained are shown in Table 1, the tests being carried out according to the national standards (GB 5606.4-2005).
TABLE 1
Figure BDA0002334077540000091
Figure BDA0002334077540000101
Comparative example 1
According to the microcapsule preparation habit in the prior art, purchasing orange powder essence on the market;
then adding purified water for dissolving to obtain the essence emulsion concentration obtained in the step 3 in the embodiment 1, namely preparing the orange powder essence water solution with the concentration of 25%, further performing the step (4) and the step (5) in the embodiment 1, adding the mixture into a filler containing 118 parts of lactose and 175 parts of microcrystalline cellulose, and uniformly mixing to obtain a wet soft material. And then putting the wet soft material into a screen with the thickness of 0.3mm, extruding and molding at the extrusion speed of 30r/min by using an extrusion spheronizer to obtain fine powder particles, putting the prepared small powder particles into the spheronizer with the rotation speed set to 200r/min to form spherical particles, taking out the wet particles after shaping, and drying at the room temperature of 25 ℃ for 24 hours to obtain the flavoring particles 5.
Comparative example 2
According to the preparation habit in the prior art, an orange powder essence solution with the same essence concentration (25%) as in example 1 is purchased on the market;
then, the preparation was carried out according to the steps (4) and (5) of example 1, that is, the mixture was added to a filler containing 118 parts of lactose and 175 parts of microcrystalline cellulose, and mixed uniformly to prepare a wet soft material. And then putting the wet soft material into a screen with the thickness of 0.3mm, extruding and molding at the extrusion speed of 30r/min by using an extrusion spheronizer to obtain fine powder particles, putting the prepared small powder particles into the spheronizer with the rotation speed set to 200r/min to form spherical particles, taking out the wet particles after shaping, and drying at the room temperature of 25 ℃ for 24 hours to obtain the flavoring particles 6.
And the GCMS is used for detecting the components of the orange fragrance in the embodiment 1 and the comparative examples 1 and 2, the sample injection method adopts static staring control, the operation mode is continuous heating at 90 ℃ for 1h, and the obtained gas phase detection chromatogram of the components of the orange fragrance is shown in figure 3.
And (4) analyzing results: in example 1 and comparative examples 1 and 2, the gas chromatograms of the three perfuming granules mainly have three peaks, and the corresponding substances are limonene, anethole and eugenol. The change of the aroma concentration in the perfuming particles is determined according to the peak abundance changes of the three substances, and the higher the peak abundance is, the higher the content is. The peak abundance of the three perfuming granule fragrance compounds is as follows from large to small: example 1, comparative example 2. Correspondingly, the fragrance stability is better and the fragrance is stronger in the example 1 of the invention, while the fragrance concentration and stability of the perfuming granule (comparative example 1) prepared by using the prepared powder essence are inferior to those of the example 1 of the invention, and the fragrance loss of the perfuming granule (comparative example 2) prepared by directly using the essence is more serious.
The invention has the advantages that:
(1) the preparation method of the flavoring particles for cigarettes and the application of the flavoring particles for cigarettes in cigarette filters provided by the invention have the advantages that the essence is emulsified to prepare the essence nano emulsion, and after various fillers are mixed with each other, the particles are prepared by an extrusion rolling method, and the flavoring particles for cigarettes are prepared by airing and drying;
(2) in the using process, only a certain amount or weight of particles loaded with fragrant substances are needed to be added into the cigarette filter, and the fragrant substances are released when the mainstream smoke of the cigarette passes through, so that the aim of perfuming the filter is fulfilled, and the smoke volume and the richness of the cigarette are effectively improved;
(3) the essence in the prepared flavoring particles for cigarettes is in a microcapsule state, and can play a role in slow release of fragrance in the storage and use processes;
(4) the emulsified essence is mixed with a filler and then extruded into a round shape (dried at room temperature of 25 ℃), and the essence content loss is little. The material is wet particles in the production process, the generated dust is less, the environment is friendly, the particle size is uniform, the fluidity is good, and the fragrance of the particles is obvious.
The above disclosure is only one or more specific embodiments of the present invention, but the present invention is not limited thereto, and any variations that can be made by those skilled in the art are intended to fall within the scope of the present invention.

Claims (10)

1. The perfuming microcapsule particle for the cigarette is characterized by comprising a composite wall material which can be emulsified and embedded with an essence core material to form an oil-in-water film and a solid filler which can be stably adhered or adsorb the emulsion;
the composite wall material comprises the following components in parts by weight: 25-28 parts of modified starch, 5.5-7.5 parts of sodium caseinate, 22-25 parts of maltodextrin, 6-9 parts of beta-cyclodextrin, 5-7 parts of Arabic gum, 4.5-7.5 parts of glucose and 1-2 parts of sucrose ester;
80-85 parts of an essence core material which is oil-soluble essence;
the solid filler comprises the following components in parts by weight: lactose 118-146 parts and microcrystalline cellulose 146-175 parts.
2. The perfuming microcapsule particle for cigarette as claimed in claim 1, wherein the composite wall material comprises the following components in parts by weight: 26-28 parts of modified starch, 5.5-7.5 parts of sodium caseinate, 22-25 parts of maltodextrin, 6-9 parts of beta-cyclodextrin, 5-7 parts of Arabic gum, 4.5-7.5 parts of glucose and 1-2 parts of sucrose ester;
80-85 parts of the essence core material;
the solid filler comprises the following components in parts by weight: 118 parts of lactose and 175 parts of microcrystalline cellulose.
3. The perfuming microcapsule particle for cigarette as claimed in claim 1, wherein the composite wall material comprises the following components in parts by weight: 28 parts of modified starch, 5.5 parts of sodium caseinate, 22 parts of maltodextrin, 6 parts of beta-cyclodextrin, 7 parts of Arabic gum, 4.5 parts of glucose and 1 part of sucrose ester;
85 parts of the essence core material;
the solid filler comprises the following components in parts by weight: 118 parts of lactose and 175 parts of microcrystalline cellulose.
4. A preparation method of perfuming microcapsule particles for cigarettes is characterized by comprising the following steps:
(1) weighing 25-28 parts of modified starch, 5.5-7.5 parts of sodium caseinate, 22-25 parts of maltodextrin, 6-9 parts of beta-cyclodextrin, 5-7 parts of Arabic gum, 4.5-7.5 parts of glucose and 1-2 parts of sucrose ester in sequence according to parts by weight; dissolving the wall material in 160 parts of water by using a water bath heating high-speed shearing machine to obtain a wall material solution A;
(2) weighing 80-85 parts of essence core materials, adding the essence core materials into the wall material solution A obtained in the step (1), and uniformly mixing under water bath heating and high-speed shearing; then homogenizing and emulsifying by a high-pressure homogenizer to obtain emulsion B;
(3) weighing 118-146 parts of lactose and 146-175 parts of microcrystalline cellulose; adding the emulsion B prepared in the step (2) into lactose and microcrystalline cellulose, and uniformly mixing to prepare a wet soft material C;
(4) and (3) putting the wet soft material C obtained in the step (3) into a screen, performing extrusion molding by using an extrusion rounding machine to obtain a strip-shaped material D, putting the strip-shaped material D into the rounding machine to form spherical particles, and taking out the wet particles after shaping to dry to obtain the perfuming liquid microcapsule E.
5. A preparation method of perfuming microcapsule granules for cigarettes according to claim 4, wherein in the step (1), the water bath heating temperature is in the range of 50-60 ℃ and the time is 30-40 min.
6. A preparation method of perfuming microcapsule granules for cigarettes according to claim 4, wherein the specific conditions of high-speed shearing in the step (2) are as follows: the shearing speed is 8000-12000rpm, and the time is 15-25 min; wherein the homogenizing pressure and times are as follows: the pressure is 1000-1200bar, and the homogenizing and emulsifying times are 3-4 times.
7. A method for preparing perfuming microcapsule granules for cigarettes according to claim 4, wherein in step (4), the mesh size is in the range of 0.2-0.4 mm; the rounding machine has the following specific conditions: the rotating speed range is 200-600 r/min.
8. The method for preparing perfuming microcapsule granules for cigarettes according to claim 7, wherein the particle size of the perfuming microcapsule granules for cigarettes obtained by screening is 40-100 meshes.
9. A method for preparing perfuming microcapsule granules for cigarettes according to claim 4, wherein in step (4), the drying conditions are as follows: and the temperature is 20-25 ℃.
10. The use of perfuming microcapsule granules for cigarettes in cigarette filters, characterized in that it comprises perfuming liquid microcapsules prepared according to any one of claims 4 to 9, said perfuming liquid microcapsules prepared being added to cigarette filters.
CN201911348567.7A 2019-12-24 2019-12-24 Perfuming microcapsule particle for cigarette, preparation method thereof and application of perfuming microcapsule particle in cigarette Pending CN113025425A (en)

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Application publication date: 20210625