CN115382463A - Preparation method of composite modified visible fragrant bead, product and application thereof - Google Patents

Preparation method of composite modified visible fragrant bead, product and application thereof Download PDF

Info

Publication number
CN115382463A
CN115382463A CN202211088266.7A CN202211088266A CN115382463A CN 115382463 A CN115382463 A CN 115382463A CN 202211088266 A CN202211088266 A CN 202211088266A CN 115382463 A CN115382463 A CN 115382463A
Authority
CN
China
Prior art keywords
particles
composite modified
visual
preparation
mixing
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN202211088266.7A
Other languages
Chinese (zh)
Other versions
CN115382463B (en
Inventor
孔浩辉
林宝敏
欧阳璐斯
罗贯洲
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
China Tobacco Guangdong Industrial Co Ltd
Original Assignee
China Tobacco Guangdong Industrial Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by China Tobacco Guangdong Industrial Co Ltd filed Critical China Tobacco Guangdong Industrial Co Ltd
Priority to CN202211088266.7A priority Critical patent/CN115382463B/en
Publication of CN115382463A publication Critical patent/CN115382463A/en
Application granted granted Critical
Publication of CN115382463B publication Critical patent/CN115382463B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Classifications

    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01JCHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2/00Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic
    • B01J2/02Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by dividing the liquid material into drops, e.g. by spraying, and solidifying the drops
    • B01J2/06Processes or devices for granulating materials, e.g. fertilisers in general; Rendering particulate materials free flowing in general, e.g. making them hydrophobic by dividing the liquid material into drops, e.g. by spraying, and solidifying the drops in a liquid medium
    • 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
    • A24D1/00Cigars; Cigarettes
    • A24D1/04Cigars; Cigarettes with mouthpieces or filter-tips
    • 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
    • A24D3/0225Applying additives to filter materials with solid additives, e.g. incorporation of a granular product
    • 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
    • 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
    • C11B9/0061Essential oils; Perfumes compounds containing a six-membered aromatic ring not condensed with another ring
    • 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
    • C11B9/0069Heterocyclic compounds
    • C11B9/0073Heterocyclic compounds containing only O or S as heteroatoms
    • C11B9/008Heterocyclic compounds containing only O or S as heteroatoms the hetero rings containing six atoms

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Cigarettes, Filters, And Manufacturing Of Filters (AREA)

Abstract

The invention provides a preparation method of a composite modified visual aromatic bead, a product and application thereof, wherein the preparation method comprises the following steps: mixing an inorganic material, an ionic surfactant and water, stirring, and filtering to obtain a first material; mixing the first material, the thickening agent, sodium bicarbonate, the colorant, the auxiliary agent and water, and stirring to obtain a suspension; dropwise adding the suspension into a calcium salt solution, and standing to obtain a second material; sequentially carrying out first washing, short-chain fatty acid aqueous solution soaking and second washing on the second material, and drying to obtain visible particles; and mixing the visual particles with essence and/or spice to obtain the composite modified visual fragrant bead. The composite modified visual aromatic bead provided by the invention has the advantages of good appearance effect, high granularity and uniformity, low breakage rate, high product quality, high biological safety and good perfuming effect.

Description

Preparation method of composite modified visible fragrant bead, product and application thereof
Technical Field
The invention belongs to the field of cigarette manufacturing, and particularly relates to a preparation method of composite modified visual aromatic beads, and a product and application thereof.
Background
With the promotion of tar and harm reduction work, the tar content in cigarette smoke is continuously reduced, the requirements on cigarette aroma enhancement and supplement technologies are higher and higher, so that the research and development of the filter tip aroma enhancement and supplement method are rapidly developed, and the aroma enhancement technologies such as tow aroma enhancement, aroma line, bead blasting, dropping pill, microcapsule, nano-particle and the like are developed and applied. However, these techniques have certain disadvantages, such as poor long-term storage fragrance stability of filament bundles and fragrance threads, high cost of bead blasting and dropping pills, and introduction of other unpleasant odors, and potential safety hazard of inhalation of microcapsules and nanoparticles into the lung.
New technologies of flavor slow-release particles have recently been developed in this industry, such as flavor slow-release agent particles for cigarette filters (201510300776. X, 201610488221.7), porous solid flavor beads for cigarettes (201910888311.9), large particle solid flavor bead cigarette filter rods (201810886849.1, 2018000887493.3, 201810887483.x, 2019000314422.9, 201910314412.5, 201810885888.x, 201811016014.7) and the like.
However, the existing technology for manufacturing the aroma sustained-release particles has some defects: (1) Granulating by adopting a common extrusion method, a spray drying method, a granulator granulation method and the like, wherein the obtained granules have small granularity, low roundness and poor hardness; if the granularity or roundness is to be improved, the production cycle is greatly prolonged, and if the hardness of the particles is to be ensured, the density is increased, and the essence adsorption capacity is reduced; (2) By adopting the improved large-particle granulation method, although the granularity and the roundness of the obtained particles are obviously improved, the production period is as long as 2-4 days, and the batch preparation capability is weak. In addition, the particles prepared by the prior art are dull in color, colorless/light in color or poor in color uniformity, so that the appearance is not good, and the particles are not suitable for manufacturing visual filters.
On the other hand, with the continuous improvement of living standard of people, consumers at present pay more and more attention to the visual enjoyment of the product while pursuing the taste and physiological satisfaction of smoke. Therefore, how to better highlight the fragrance personality and the appearance personality of the product and attract the eyes of consumers becomes an important consideration index of new products on the market.
Therefore, how to provide a filter tip aroma-enhancing and aroma-supplementing product which can better highlight the aroma personality and the appearance personality of the product and has a simple and quick preparation process becomes a problem to be solved urgently at present.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide the composite modified visual aromatic bead and the preparation method and the application thereof, the composite modified visual aromatic bead provided by the invention has the advantages of uniformity, visual and visible particle size, full roundness and bright color, and the visual particles endow the product with bright characteristics and are matched with the aroma characteristics to strengthen the cognition of consumers on the aroma of the product; and the fragrance is released evenly and smoothly, so that no bad smell is introduced and the harmfulness of the smoke is increased.
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the invention provides a preparation method of a composite modified visual fragrant bead, which comprises the following steps:
(1) Mixing an inorganic material, an ionic surfactant and water, stirring, and filtering to obtain a first material;
(2) Mixing the first material obtained in the step (1), a thickening agent, sodium bicarbonate, a coloring agent, an auxiliary agent and water, and stirring to obtain a suspension;
(3) Dropwise adding the suspension obtained in the step (2) into a calcium salt solution, and standing to obtain a second material;
(4) Sequentially carrying out first washing, short-chain fatty acid aqueous solution soaking and second washing on the second material obtained in the step (3), and drying to obtain visible particles;
(5) And (5) mixing the visual particles obtained in the step (4) with essence and/or spice to obtain the composite modified visual fragrant bead.
In the method, the suspension is dropwise added into the calcium salt solution, so that the suspension liquid drops expand and are solidified into particles, and the solidified particles not only have higher porosity than the stirring granulation adsorption material, but also are beneficial to storage and slow release of the fragrance components; but also the expansion and solidification operation leaves an operable space for the addition of other materials, and other materials without adsorption pores can construct particle pores in the particle expansion process, so that the influence of the addition of other substances on the slow release effect of the particle fragrance is reduced; the finally prepared product has good appearance effect, high granularity and uniformity, low crushing rate, high product quality, high biological safety and good flavoring effect; meanwhile, the preparation method is simple and easy to operate, and the time period for manufacturing the spherical particles is far shorter than that of the existing method.
The ionic surfactant is adopted to modify the inorganic material, so that the adsorption capacity of the material to pigments is greatly enhanced, the pigment is not easy to elute and fade, and the particles are endowed with the required bright color and keep long-term stability; the sodium bicarbonate is adopted for modification again, so that the adsorption force of the particles to pigments can be further improved, the color of the particles is more bright and bright, the porosity of the particles is improved, and the adsorption storage amount and the slow release effect of aroma components are well improved.
In the present invention, in step (1), the inorganic material includes any one of bentonite, kaolin, a molecular sieve, silica or alumina, or a combination of at least two of them.
Preferably, the bentonite comprises any one of montmorillonite, clay or modified bentonite or a combination of at least two of the foregoing.
Preferably, in step (1), the ionic surfactant is a cationic surfactant.
Preferably, in step (1), the ionic surfactant comprises any one of cetyltrimethylammonium bromide, dodecyltrimethylammonium bromide, dioctyldimethylammonium bromide or cetyldimethylethylammonium bromide or a combination of at least two thereof.
In the invention, in the step (1), the mass ratio of the inorganic material to the ionic surfactant is (5-20): 1 (wherein, 5-20 can be 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, etc.).
Preferably, in step (1), the volume of water is 5-20mL (for example, 5mL, 7mL, 9mL, 11mL, 13mL, 15mL, 17mL, 19mL, 20mL, etc.) based on the sum of the masses of the inorganic material and the ionic surfactant being 1 g.
Preferably, in step (1), the stirring time is 2-6h (for example, 2h, 2.5h, 3h, 3.5h, 4h, 4.5h, 5h, 5.5h, 6h, etc.).
Preferably, in step (1), the step of draining further comprises water washing.
In the present invention, in the step (2), the thickener includes a food grade thickener.
Preferably, in the step (2), the thickening agent comprises any one or a combination of at least two of sodium alginate, gum arabic, cyclodextrin or carrageenan.
Preferably, in the step (2), the colorant comprises any one of orange pigment, bright blue pigment, cherry fruit-flavor essence or curcumin or a combination of at least two of the above.
Preferably, in step (2), the auxiliary agent comprises any one of sodium carbonate, potassium carbonate or sodium thiosulfate or a combination of at least two of the sodium carbonate, the potassium carbonate and the sodium thiosulfate.
In the present invention, in the step (2), the mass ratio of the first material to the thickener is (5-20): 1 (wherein, "5-20" may be 5, 7, 9, 11, 13, 15, 17, 19, 20, etc.).
Preferably, in step (2), the mass ratio of the first material to the sodium bicarbonate is (1-10): 1 (wherein "1-10" may be 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, etc.).
Preferably, in the step (2), the mass ratio of the first material to the colorant is (30-300): 1 (wherein, "30-300" may be 30, 50, 80, 100, 120, 150, 180, 200, 220, 250, 270, 300, etc.), preferably (30-250): 1, and more preferably (50-200): 1.
Preferably, in the step (2), the mass ratio of the sodium bicarbonate to the auxiliary agent is (5-25): 1 (wherein, the '5-25' can be 5, 7, 9, 11, 13, 15, 17, 19, 21, 23, 25, and the like).
Preferably, in step (2), the stirring time is 30-60min (for example, 30min, 35min, 40min, 45min, 50min, 55min, 60min, etc.).
In the present invention, in the step (3), the mass concentration of the calcium salt solution is 0.5 to 15% (for example, 0.5%, 1%, 3%, 5%, 7%, 9%, 11%, 13%, 15%, etc. may be used).
Preferably, the calcium salt comprises calcium chloride.
Preferably, in step (3), the dropping rate is 10 to 120 drops/min (e.g., 10 drops/min, 20 drops/min, 30 drops/min, 40 drops/min, 50 drops/min, 60 drops/min, 70 drops/min, 80 drops/min, 90 drops/min, 100 drops/min, 110 drops/min, 120 drops/min, etc.), and the volume of each drop of suspension is 0.04 to 0.1mL (e.g., 0.04mL, 0.05mL, 0.06mL, 0.07mL, 0.08mL, 0.09mL, 0.1mL, etc.).
Preferably, in step (3), the standing time is at least 30min (for example, 30min, 40min, 50min, 60min, 70min, 80min, 90min, etc.).
In the present invention, in the step (4), the short chain fatty acid includes any one of acetic acid, propionic acid or butyric acid or a combination of at least two thereof.
Preferably, in step (4), the aqueous solution of short-chain fatty acids has a mass concentration of short-chain fatty acids of 0.1-5% (e.g., 0.1%, 1%, 1.5%, 2%, 2.5%, 3%, 3.5%, 4%, 4.5%, 5%, etc. are possible).
Preferably, in step (4), the soaking time is 10-60min (for example, 10min, 20min, 30min, 40min, 50min, 60min, etc.).
In the invention, in the step (5), the essence comprises any one of sweet orange oil, peppermint oil or allyl caproate or a combination of at least two of the sweet orange oil, the peppermint oil and the allyl caproate.
Preferably, in step (5), the perfume comprises an artificial perfume and/or a plant extract.
Preferably, the artificial aroma comprises ethyl maltol and/or vanillin.
Preferably, the plant extract comprises stevioside.
Preferably, the plant extract is colorless, pale in color, or the same or similar in color to the pigment.
Preferably, in step (5), the specific step of mixing comprises spraying the essence onto the surface of the visible particles or immersing the visible particles in a perfume solution.
In a second aspect, the invention provides a composite modified visual fragrant bead prepared by the preparation method of the first aspect.
In a third aspect, the invention provides a use of the composite modified visual aromatic bead according to the second aspect in preparing cigarettes.
Compared with the prior art, the invention has the following beneficial effects:
(1) By adopting the method of dropwise adding the turbid liquid into the calcium salt solution, the turbid liquid drops are expanded and solidified into particles, and the solidified particles not only have higher porosity than the stirring granulation adsorption material, but also are beneficial to storage and slow release of the fragrance components; but also the expansion and solidification operation leaves operable space for the addition of other materials, and other materials without adsorption pores can construct particle pores in the particle expansion process, thereby reducing the influence of the addition of other substances on the slow release effect of the particle fragrance; the finally prepared product has good appearance effect, high granularity and uniformity, low breakage rate, high product quality, high biological safety and good perfuming effect; meanwhile, the preparation method is simple and easy to operate, and the time period for manufacturing the spherical particles is far shorter than that of the existing method.
(2) According to the invention, the ionic surfactant and the sodium bicarbonate are adopted to modify the inorganic material, the granularity, uniformity and crushing rate of the modified visual slow-release particles meet the requirements, the visual slow-release particles are bright and bright in color, stable and not easy to fade, the biological safety is higher, and the adsorption storage capacity and the slow-release effect of the aroma components are well improved.
(3) The composite modified visual aroma beads provided by the invention are uniform, visual and visible in granularity, full in roundness and bright in color, and the visual particles endow the product with distinct characteristics and are matched with aroma characteristics to strengthen the cognition of consumers on the aroma of the product; and the fragrance is released evenly and smoothly, and bad smell is not introduced, and the harmfulness of smoke is not increased. Therefore, the aroma characteristic and the personalized characteristic of a new product are enhanced through good aroma slow-release capacity and smoke quality improvement effect, color and aroma characteristic association and visual enhancement of taste memory, the aim of overcoming the problem that the homogeneity of market products is serious day by day is achieved, consumers can be endowed with better product experience, and the added value of the product is increased.
Drawings
Fig. 1 is an appearance diagram of the composite modified visual aromatic bead provided in example 1.
Fig. 2 is an appearance diagram of the composite modified visual incense bead provided in example 2.
Fig. 3 is an appearance diagram of the composite modified visual aromatic bead provided in example 3.
Fig. 4 is an appearance diagram of a comparative example of the composite modified visual aromatic bead provided in comparative example 1.
Fig. 5 is an appearance diagram of a comparative example of the composite modified visual aromatic bead provided in comparative example 2.
Fig. 6 is an appearance diagram of a comparative example of the composite modified visual aromatic bead provided in comparative example 3.
Fig. 7 is a schematic structural view of a visual filter cigarette manufactured in the sensory evaluation.
Fig. 8 is an appearance diagram of a visual filter cigarette manufactured in the sensory evaluation.
Detailed Description
The technical solution of the present invention is further described below by way of specific embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitation of the present invention.
In the following examples, orange pigment was purchased from Jiangsu Yihe Biotech, inc., cherry fruit flavor was purchased from Baizun/Angel Yeast, inc., brilliant blue pigment was purchased from Jiangsu Yihe Biotech, inc., CTAB was purchased from Shanghai Boao Biotech, inc., and flavor and essential oil were purchased from Shenzhen Boton flavor, inc.
Example 1
The embodiment provides a composite modified visual fragrant bead, which is prepared by the following steps:
(1) Uniformly mixing montmorillonite and CTAB powder according to the mass ratio of 10; and mixing the solid mixture with water according to the solid-liquid ratio of 1.
(2) Dissolving sodium alginate (the mass ratio of the first material to the sodium alginate is 10; naHCO is additionally used 3 (first Material and NaHCO) 3 The mass ratio of (1) to (4) is as follows, dispersing a first material by an aqueous solution, fully stirring to form a suspension containing the first material, and uniformly mixing the suspension containing the first material with an aqueous solution of sodium alginate; then, a colorant (orange pigment) (the mass ratio of the first material to the colorant is 150) and sodium carbonate (the mass ratio of sodium bicarbonate to sodium carbonate is 5.
(3) Dropping the suspension into CaCl containing 8% (m/V) 2 The second material was obtained after standing for 40min in the aqueous solution of (1) (60 drops/min, each drop having a volume of 0.08 mL).
(4) And (3) washing the second material with water for several times, soaking the washed second material in 2% (m/V) acetic acid aqueous solution for 30min, washing with water for several times, and drying to obtain the visual particles.
(5) And spraying sweet orange oil on the visual particles, and carrying out cold drying to obtain the composite modified visual fragrant beads. The appearance of which is shown in fig. 1.
Example 2
The embodiment provides a composite modified visual fragrant bead, which is prepared by the following steps:
(1) Uniformly mixing aluminum trioxide and dodecyl trimethyl ammonium bromide according to the mass ratio of 5; then the solid mixture is mixed with water according to the solid-liquid ratio of 1.
(2) Dissolving carrageenan (the mass ratio of the first material to the carrageenan is 20; naHCO is additionally used 3 (first Material and NaHCO) 3 1) dispersing a first material in an aqueous solution, fully stirring to form a suspension containing the first material, and uniformly mixing the suspension containing the first material and a carrageenan aqueous solution; then, adding a coloring agent (cherry fruity essence) (the mass ratio of the first material to the coloring agent is 200.
(3) Dripping the suspension into CaCl containing 0.5% (m/V) 2 The second material was obtained by standing the aqueous solution of (1) for 50min (10 drops/min, each drop having a volume of 0.1 mL).
(4) And (3) washing the second material with water for several times, soaking the washed second material in 0.1% (m/V) propionic acid aqueous solution for 10min, washing with water for several times, and drying to obtain the visual particles.
(5) Spraying peppermint oil on the visual particles, and cooling and drying to obtain the composite modified visual aromatic bead. The appearance of which is shown in fig. 2.
Example 3
The embodiment provides a composite modified visual aromatic bead, which is prepared by the following steps:
(1) Uniformly mixing diatomite and bis-octaalkyl dimethyl ammonium bromide according to the mass ratio of 20; and mixing the solid mixture with water according to the solid-liquid ratio of 1.
(2) Dissolving cyclodextrin (the mass ratio of the first material to cyclodextrin is 5; naHCO is additionally used 3 (first Material and NaHCO) 3 The mass ratio of (1) dispersing a first material in an aqueous solution, fully stirring to form a suspension containing the first material, and uniformly mixing the suspension containing the first material and a cyclodextrin aqueous solution; then, a colorant (brilliant blue pigment) (the mass ratio of the first material to the colorant is 30: 1) and sodium thiosulfate (the mass ratio of sodium bicarbonate to sodium thiosulfate is 25: 1) were added, and stirring was continued for 60min to obtain a suspension.
(3) Dropping the suspension into CaCl containing 15% (m/V) 2 In an aqueous solution of (3 drops/min)Each drop of the second material is 0.04 mL), standing for 60min, and taking out to obtain a second material;
(4) Washing the second material with water for several times, soaking the washed second material in 5% (m/V) butyric acid aqueous solution for 60min, washing with water for several times, and drying to obtain visible particles;
(5) And soaking the visual particles in ethyl maltol ethanol solution, and performing cold drying to obtain the composite modified visual fragrant beads. The appearance of which is shown in fig. 3.
Example 4
This example provides a composite modified visual aromatic bead, which is different from example 1 only in that the preparation method is the same as example 1 except that the dropping parameter is 160 drops/min, and the volume of each drop is 0.14 mL.
Comparative example 1
The comparative example provides a composite modified visual aromatic bead comparative sample which is prepared by adopting a common granulation method, and the preparation method comprises the following steps:
mixing montmorillonite with sodium alginate, sodium carbonate and water (the mixture ratio of the materials is consistent with that in example 1, and the addition amount of the water is to make the slurry pasty) to obtain slurry; stirring the mixture for 2 hours by adopting a stirring granulation method, and then granulating on a swinging granulator; and soaking the obtained particles in an orange pigment solution, drying, and mixing with menthol to obtain the composite modified visual aromatic bead contrast sample. The appearance is shown in fig. 4.
Comparative example 2
The comparative example provides a composite modified visual aromatic bead comparative sample which is prepared by adopting a spherical die pressing molding method, and the preparation method comprises the following steps:
mixing and grinding montmorillonite, sodium alginate, sodium carbonate and water (the mixture ratio of the materials is consistent with that in example 1, and the adding amount of the water is to make the slurry pasty) to obtain slurry; sieving the slurry, pouring the slurry into a spherical mold for compression molding, drying for 24 hours at the temperature of below 25 ℃, and drying for 3 hours at the temperature of 45 ℃ to obtain a spherical blank; calcining the spherical embryo body at 1300 ℃ for 4 hours to obtain slow-release particles; and soaking the obtained particles in an orange pigment solution, drying, and mixing with menthol to obtain the composite modified visual aromatic bead contrast sample. The appearance of which is shown in fig. 5.
Comparative example 3
The comparative example provides a composite modified visual aromatic bead comparative sample, which is different from the example 1 only in that the step (1) is omitted, and montmorillonite is directly used as a first material to carry out the steps (2) to (5); and in step (2), no sodium bicarbonate was added, the rest being identical to example 1. The appearance is shown in fig. 6.
Examples 1-3 provide products in which the example 1 particles are orange, the example 2 particles are medium red, and the example 3 particles are azure (the appearance of the product of example 1 is shown in fig. 1, the appearance of the product of example 2 is shown in fig. 2, and the appearance of the product of example 3 is shown in fig. 3). The appearance of comparative example 1 is shown in fig. 4, and the difference in morphology between the products is large, and the products are not smooth and have poor appearance. The appearance of comparative example 2 is shown in fig. 5, and although the roundness and uniformity of the particles are good, the color between the particles is not uniform, most of the particles are white, and part of the particles are yellowish to yellow, so that the dyeing effect is poor; and the manufacturing cycle is as long as 3 days, and the mass production capacity is limited by the number of molds. The appearance of comparative example 3 is shown in fig. 6, and although the roundness and uniformity of the particles are acceptable, the color of the particles is dull and not very uniform, most of the particles are plain, a small part of the particles are yellowish, and the dyeing effect is poor. The product particles disclosed by the invention have better appearance effect, are mellow and have small difference, can endow the product with better color and luster, improve the attractiveness, can be matched with the type feeling of essence, and improve the use experience.
Test example 1
Appearance evaluation: particle size and roundness, particle breakage rate, and particle color
The products provided in examples 1 to 4 and comparative examples 1 to 3 were evaluated for appearance properties by the following methods:
(1) The particle size and roundness detection method comprises the following steps: and placing the composite modified visible fragrant bead and the steel ruler on a blue flat plate. Using high-pixel imaging equipment to collect pictures, and then adopting Image J software to analyze the pictures so as to obtain the particle projection area (mm) 2 ) And the long diameter and the short diameter of the particle projection are calculated to obtain the particlesParticle size is expressed by "projected area of particle", and particle roundness is expressed by "area of circle ratio" ("area of circle ratio = projected area/area of maximum circle").
(2) The particle breakage rate detection method comprises the following steps: the composite modified visual fragrant beads are put into a box with a cover, and the volume of the particles accounts for less than 10% of the volume of the box. After the box cover is covered, the box is placed into a rotating box, and then the collision condition possibly met by the particles in the storage and transportation process is simulated by adopting a rotating box method according to YC/T151.2-2001 standard. After rotation, the particles in the box are taken out and sieved, and the weight difference of the particles before and after rotation is weighed and calculated, so that the particle crushing rate in the rotation process is obtained. And evaluating the hardness of the particles and the applicability of the particles in the processes of production, storage and transportation by using the particle crushing rate.
(3) And (3) color judgment: the color of the granules is judged by comparing with a 24-color standard color card.
The results are shown in table 1 below:
TABLE 1
Figure BDA0003836051970000121
Figure BDA0003836051970000131
The data show that compared with the common granulation method, the product provided by the invention can obviously improve the granularity, the uniformity, the roundness and the coloring uniformity of the product, reduce the crushing rate and obviously improve the product quality; meanwhile, the roundness of the product can be obviously improved by controlling the dripping parameters, and the appearance effect is improved. In comparative example 2, although the appearance and quality of the product were also excellent, the color was not uniform among particles; and the adopted spherical mold compression molding method has longer production period and weaker batch preparation capability.
As can be seen from a comparison of example 1 and example 4, the dropping parameters affect the appearance of the particles, and the uniformity and roundness of the particles are affected.
It can be seen from the comparison between example 1 and comparative example 3 that the coloring effect of the particles is affected without modifying the ionic surfactant and the sodium bicarbonate, and the color of the particles is obviously lightened under the same pigment amount and process conditions.
Test example 2
And (3) safety evaluation: smoke component detection and biosafety evaluation
The products provided in examples 1-3 and comparative examples 1-3 (with the added weight of 0.135-0.145 g) were respectively put into hollow filter cigarettes to obtain visual filter cigarettes (the cigarette filter structure is that, from the end of the filter, a 15mm tow segment + a 5mm hollow segment + a 10mm tow segment, and the composite modified visual aromatic beads are completely filled in the hollow segment, the structure diagram is shown in fig. 7, and the appearance diagram is shown in fig. 8), and smoke components released during smoking of the hollow filter and a blank filter (without any added particles, the filter is a 30mm acetate filter) are detected, so that the safety of the visual particles is analyzed in a contrast way, and the detection method is as follows:
(1) The tar, nicotine and moisture of the cigarette are measured according to GB/T19609-2004, GB/T23203.1-2008 and GB/T23355-2009. And respectively measuring the release amount of 7 harmful components such as mainstream smoke CO, benzo [ alpha ] pyrene (Ba P), HCN, NNK, ammonia, phenol, crotonaldehyde and the like of the cigarette sample according to the measuring methods of GB/T23356-2009, GB/T21130-2007, YC/T253-2019, CRMN DEG 75, YC/T377-2019, YC/T255-2008 and YC/T254-2008, and calculating the hazard index H value of the cigarette sample by adopting a Shehler formula according to the method of tobacco and smoke chemical components. Since the physiological satisfaction of different cigarette samples is different, according to the WHO evaluation method, the unit nicotine value is used to perform the transverse comparison of different samples ("a certain component value of the unit nicotine = the detected component value/nicotine value").
(2) And carrying out biological evaluation on the smoke safety according to YQ/T42-2013, YQ 3-2011 and YQ/T43-2013.
The results of the analysis of the effect of the particles on the hazard of the smoke are shown in table 2 below:
TABLE 2
Figure BDA0003836051970000141
The data show that the composite modified visual aromatic bead provided by the invention does not bring negative effects on cigarette samples, but obviously improves the smoking safety of the cigarette samples, and can selectively reduce the release amount of CO, ammonia, baP, NNK and crotonaldehyde, so that the H value of nicotine per unit is obviously reduced, and the harmfulness of smoke is reduced; and the IC50 of the flue gas 24h cells is greatly improved, which shows that the product can reduce the biological toxicity of the flue gas to a certain extent.
Test example 3
Sensory evaluation
The products provided in examples 1 to 3 and comparative examples 1 to 3 were respectively put into hollow filter cigarettes to prepare visual filter cigarettes (the structure of the cigarette filter is that, starting from the end of the filter, a 15mm tow segment + a 5mm hollow segment + a 10mm tow segment, composite modified visual aromatic beads are completely filled into the hollow segment, the structural schematic diagram is shown in fig. 7, the appearance diagram is shown in fig. 8, no particles are added to a blank sample, and the filter is a 30mm acetate filter). And (3) evaluating the cigarettes and the blank samples by a person qualified for professional cigarette sensory evaluation by adopting a flavor profile analysis method, and recording the result. The 13 indexes of the smoke characteristics are scored (according to the scoring standard established by YC/T497-2014), and the perfuming strength and the suitability are evaluated. The score is divided into unit increments of 0.5, the score is divided into 10 points, and finally the result is averaged, and 1 decimal place is reserved.
Wherein: the indexes of the smoke score take the smoke quality as a measurement standard, such as: the lower the "miscellaneous" concentration, the higher the score; "stiff" but less comfortable, with a low score.
The term of adding fragrance strength, the more obvious the additional fragrance, the higher the score; wherein 1-3 are sensible, 4-6 are obvious for external perfuming, and 7-9 are strong for external perfuming.
The harmony index, the better the harmony of the smoke of the cigarette after the introduction of the additional aroma, the higher the score, and otherwise the score is reduced.
The results are shown in table 3 below:
TABLE 3
Figure BDA0003836051970000151
Figure BDA0003836051970000161
The data show that the product provided by the invention can effectively improve the quality of smoke, endow the cigarette with more obvious additional aroma and has no great negative influence on the harmony of the smoke. In addition, the adsorption storage capacity of the particles to the aroma components is large, so that the perfuming strength is overlarge during smoking, and the aroma coordination and the smoking quality are influenced. This can be easily solved by reducing the loading of the beads in the filter.
Test example 4
Evaluation of fragrance sustained-release capability:
cigarette samples prepared by the sensory evaluation are taken as objects (blank samples are subjected to filter flavoring in a tow spraying mode), a rotary disc smoking machine (model RM20H manufactured by Borgwaldt KC Instrument company) is adopted, and a mouth-to-mouth smoking detection module is configured, and tar, nicotine and moisture on the cigarette mouth-to-mouth smoke trapping filter sheet are measured by referring to GB/T19609-2004, GB/T23203.1-2008 and GB/T23355-2009. And (4) with reference to YC/T286-2009, measuring the content of the flavor components on the cigarette mouth-by-mouth smoke trapping filter disc in an externally added menthol sample preparation mode (the flavor and the aroma in all particles are replaced by the same amount of menthol). The matching of the visual granular flavor slow-release capacity and the smoke is analyzed by adopting the ratio of the mouth-by-mouth flavor component ratio (single-mouth flavor component content/total flavor component content) to the mouth-by-mouth tar ratio (single-mouth tar content/total tar content), and the test results are shown in the following table 4:
TABLE 4
Figure BDA0003836051970000171
According to the data, the composite modified visual aromatic bead has good matching performance of the slow release capacity of the aromatic component and the concentration of smoke one by one, and the ratio of the concentration of the aromatic component to the concentration of tar is stabilized within the range of 0.92-1.08 except for the first mouth (ignition suction mouth), which shows that the slow release capacity of the aroma is good and meets the requirements of the essence slow release material.
The applicant states that the present invention is illustrated by the above examples of the process of the present invention, but the present invention is not limited to the above process steps, i.e. it is not meant that the present invention must rely on the above process steps to be carried out. It will be apparent to those skilled in the art that any modification of the present invention, equivalent substitutions of selected materials and additions of auxiliary components, selection of specific modes and the like, which are within the scope and disclosure of the present invention, are contemplated by the present invention.

Claims (10)

1. A preparation method of composite modified visible fragrant beads is characterized by comprising the following steps:
(1) Mixing an inorganic material, an ionic surfactant and water, stirring, and filtering to obtain a first material;
(2) Mixing the first material obtained in the step (1), a thickening agent, sodium bicarbonate, a coloring agent, an auxiliary agent and water, and stirring to obtain a suspension;
(3) Dropwise adding the suspension obtained in the step (2) into a calcium salt solution, and standing to obtain a second material;
(4) Sequentially carrying out first washing, short-chain fatty acid aqueous solution soaking and second washing on the second material obtained in the step (3), and drying to obtain visible particles;
(5) And (3) mixing the visual particles obtained in the step (4) with essence and/or spice to obtain the composite modified visual aromatic bead.
2. The preparation method according to claim 1, wherein in the step (1), the inorganic material comprises any one of bentonite, kaolin, molecular sieve, silicon dioxide or aluminum oxide or a combination of at least two of the bentonite, the kaolin, the molecular sieve, the silicon dioxide and the aluminum oxide;
preferably, the bentonite comprises any one of montmorillonite, clay or modified bentonite or a combination of at least two of montmorillonite, clay or modified bentonite;
preferably, in step (1), the ionic surfactant is a cationic surfactant;
preferably, in step (1), the ionic surfactant comprises any one of cetyltrimethylammonium bromide, dodecyltrimethylammonium bromide, dioctyldimethylammonium bromide or cetyldimethylethylammonium bromide or a combination of at least two thereof.
3. The production method according to claim 1 or 2, wherein in the step (1), the mass ratio of the inorganic material to the ionic surfactant is (5-20): 1;
preferably, in the step (1), the volume of water is 5-20mL calculated by the sum of the mass of the inorganic material and the mass of the ionic surfactant being 1 g;
preferably, in the step (1), the stirring time is 2-6h;
preferably, in step (1), the step of draining further comprises water washing.
4. The method according to any one of claims 1 to 3, wherein in the step (2), the thickener comprises a food grade thickener;
preferably, in the step (2), the thickening agent comprises any one or a combination of at least two of sodium alginate, gum arabic, cyclodextrin or carrageenan;
preferably, in the step (2), the colorant comprises any one of orange pigment, bright blue pigment, cherry fruit flavor or curcumin or a combination of at least two of the orange pigment, the bright blue pigment, the cherry fruit flavor or the curcumin;
preferably, in step (2), the auxiliary agent comprises any one of sodium carbonate, potassium carbonate or sodium thiosulfate or a combination of at least two of the sodium carbonate, the potassium carbonate and the sodium thiosulfate.
5. The production method according to any one of claims 1 to 4, wherein in the step (2), the mass ratio of the first material to the thickener is (5-20): 1;
preferably, in the step (2), the mass ratio of the first material to the sodium bicarbonate is (1-10): 1;
preferably, in the step (2), the mass ratio of the first material to the colorant is (30-300): 1;
preferably, in the step (2), the mass ratio of the sodium bicarbonate to the auxiliary agent is (5-25): 1;
preferably, in the step (2), the stirring time is 30-60min.
6. The method according to any one of claims 1 to 5, wherein in the step (3), the mass concentration of the calcium salt solution is 0.5 to 15%;
preferably, the calcium salt comprises calcium chloride;
preferably, in the step (3), the dropping rate is 10 to 120 drops/min, and the volume of each drop of suspension is 0.04 to 0.1mL;
preferably, in step (3), the time for the standing is at least 30min.
7. The process according to any one of claims 1 to 6, wherein in the step (4), the short-chain fatty acid comprises any one of acetic acid, propionic acid or butyric acid or a combination of at least two thereof;
preferably, in the step (4), the mass concentration of the short-chain fatty acid in the aqueous solution of the short-chain fatty acid is 0.1-5%;
preferably, in the step (4), the soaking time is 10-60min.
8. The method according to any one of claims 1 to 7, wherein in the step (5), the essence comprises any one of sweet orange oil, peppermint oil or allyl caproate or a combination of at least two of the sweet orange oil, the peppermint oil and the allyl caproate;
preferably, in step (5), the perfume comprises an artificial synthetic perfume and/or a plant extract;
preferably, the artificial aroma comprises ethyl maltol and/or vanillin;
preferably, the plant extract comprises stevioside;
preferably, in step (5), the specific step of mixing comprises spraying the essence onto the surface of the visible particles or immersing the visible particles in a perfume solution.
9. A composite modified visual fragrant bead prepared by the preparation method of any one of claims 1-8.
10. Use of the composite modified visual flavor bead according to claim 9 in the preparation of cigarettes.
CN202211088266.7A 2022-09-07 2022-09-07 Preparation method of composite modified visual aromatic beads, product and application thereof Active CN115382463B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202211088266.7A CN115382463B (en) 2022-09-07 2022-09-07 Preparation method of composite modified visual aromatic beads, product and application thereof

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202211088266.7A CN115382463B (en) 2022-09-07 2022-09-07 Preparation method of composite modified visual aromatic beads, product and application thereof

Publications (2)

Publication Number Publication Date
CN115382463A true CN115382463A (en) 2022-11-25
CN115382463B CN115382463B (en) 2023-11-17

Family

ID=84127032

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202211088266.7A Active CN115382463B (en) 2022-09-07 2022-09-07 Preparation method of composite modified visual aromatic beads, product and application thereof

Country Status (1)

Country Link
CN (1) CN115382463B (en)

Citations (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6427461A (en) * 1987-07-23 1989-01-30 Japan Tobacco Inc Fragrance particle for tobacco and its production
WO2009094859A1 (en) * 2008-01-25 2009-08-06 Rj Reynolds Tobacco Company Process for manufacturing breakable capsules useful in tobacco products
CN102578711A (en) * 2012-01-19 2012-07-18 湖北中烟工业有限责任公司 Sodium alginate microparticles for cigarette filter and filtered cigarette
CN103039442A (en) * 2013-01-21 2013-04-17 海南大学 Method for preparing drug-loading nanocomposite through ball-milling modification of mineral soil and application
CN103933597A (en) * 2014-04-28 2014-07-23 福州大学 Method for preparing essence sustained-release porous capsule from bentonite
CN104856223A (en) * 2015-04-29 2015-08-26 湖北中烟工业有限责任公司 Tobacco solid fragrant bead and preparation method of same
CN104959127A (en) * 2015-06-05 2015-10-07 滁州卷烟材料厂 Tranquillizing soothing health-care composite adsorbent for cigarette filter and preparation method thereof
CN104973931A (en) * 2015-05-05 2015-10-14 马鞍山科邦生态肥有限公司 Highly-efficient biomass charcoal coated fertilizer and preparation method thereof
CN106824060A (en) * 2016-11-17 2017-06-13 徐浩强 A kind of preparation method of eliminating smell agent
CN109198721A (en) * 2018-08-06 2019-01-15 江西中烟工业有限责任公司 A kind of middle branch cigarette filter tip and preparation method thereof containing bulky grain solid-state perfume (or spice) pearl
CN111418889A (en) * 2020-03-16 2020-07-17 云南中烟工业有限责任公司 Neroli oil capsule dry bead, preparation method thereof and application thereof in tobacco
CN112656024A (en) * 2020-12-02 2021-04-16 云南养瑞科技集团有限公司 Preparation method of cooling and aroma-enhancing particles for HNB (household Natural gas) cigarettes and cooling and aroma-enhancing particles for HNB cigarettes
CN112871127A (en) * 2021-01-18 2021-06-01 江苏特丰新材料科技有限公司 Preparation method of high-porosity lithium ion sieve particles
CN114190587A (en) * 2021-12-24 2022-03-18 山东中烟工业有限责任公司 Cigarette functional filter stick with perfuming carrier, preparation method and application thereof
CN114762534A (en) * 2021-01-12 2022-07-19 云南恩典科技产业发展有限公司 Low-temperature slow-release microcrystalline granules and preparation method and application thereof

Patent Citations (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS6427461A (en) * 1987-07-23 1989-01-30 Japan Tobacco Inc Fragrance particle for tobacco and its production
WO2009094859A1 (en) * 2008-01-25 2009-08-06 Rj Reynolds Tobacco Company Process for manufacturing breakable capsules useful in tobacco products
CN102578711A (en) * 2012-01-19 2012-07-18 湖北中烟工业有限责任公司 Sodium alginate microparticles for cigarette filter and filtered cigarette
CN103039442A (en) * 2013-01-21 2013-04-17 海南大学 Method for preparing drug-loading nanocomposite through ball-milling modification of mineral soil and application
CN103933597A (en) * 2014-04-28 2014-07-23 福州大学 Method for preparing essence sustained-release porous capsule from bentonite
CN104856223A (en) * 2015-04-29 2015-08-26 湖北中烟工业有限责任公司 Tobacco solid fragrant bead and preparation method of same
CN104973931A (en) * 2015-05-05 2015-10-14 马鞍山科邦生态肥有限公司 Highly-efficient biomass charcoal coated fertilizer and preparation method thereof
CN104959127A (en) * 2015-06-05 2015-10-07 滁州卷烟材料厂 Tranquillizing soothing health-care composite adsorbent for cigarette filter and preparation method thereof
CN106824060A (en) * 2016-11-17 2017-06-13 徐浩强 A kind of preparation method of eliminating smell agent
CN109198721A (en) * 2018-08-06 2019-01-15 江西中烟工业有限责任公司 A kind of middle branch cigarette filter tip and preparation method thereof containing bulky grain solid-state perfume (or spice) pearl
CN111418889A (en) * 2020-03-16 2020-07-17 云南中烟工业有限责任公司 Neroli oil capsule dry bead, preparation method thereof and application thereof in tobacco
CN112656024A (en) * 2020-12-02 2021-04-16 云南养瑞科技集团有限公司 Preparation method of cooling and aroma-enhancing particles for HNB (household Natural gas) cigarettes and cooling and aroma-enhancing particles for HNB cigarettes
CN114762534A (en) * 2021-01-12 2022-07-19 云南恩典科技产业发展有限公司 Low-temperature slow-release microcrystalline granules and preparation method and application thereof
CN112871127A (en) * 2021-01-18 2021-06-01 江苏特丰新材料科技有限公司 Preparation method of high-porosity lithium ion sieve particles
CN114190587A (en) * 2021-12-24 2022-03-18 山东中烟工业有限责任公司 Cigarette functional filter stick with perfuming carrier, preparation method and application thereof

Also Published As

Publication number Publication date
CN115382463B (en) 2023-11-17

Similar Documents

Publication Publication Date Title
CN108065456B (en) Tobacco particle-containing heating non-combustion tobacco product and preparation method thereof
RU2325824C2 (en) Improvement of smoking products
CN104883876B (en) Low-density is coated with animal litter composition
CN109198721B (en) Medium cigarette filter tip containing large-particle solid aromatic beads and preparation method thereof
CN115430353B (en) Modified visual coloring fragrance slow-release particles and preparation method and application thereof
CN115318197B (en) Visual fragrance slow-release granule and preparation method and application thereof
CN110801049B (en) Cigarette filter tip aroma sustained-release particles and preparation method thereof
CN110283661A (en) A kind of quick-fried pearl of cigarette gel and preparation method thereof
CN115382463A (en) Preparation method of composite modified visible fragrant bead, product and application thereof
CN106179145A (en) A kind of solid microcapsule containing Folium Camelliae sinensis characteristic perfume and preparation method thereof
CN115382462B (en) Preparation method of colored fragrant beads, product and application thereof
CN115337860B (en) Preparation method of colorful herbal fragrant beads, product and application thereof
CN108851213B (en) Cigarette filter rod containing large-particle solid aromatic beads and preparation method thereof
CN115153090B (en) Visual coloring fragrance slow-release particles and preparation method and application thereof
CN115316705A (en) Preparation method of colored slow-release fragrant bead, product and application thereof
CN115433634B (en) Alkali modified visual coloring fragrance slow-release particles and preparation method and application thereof
CN114133983A (en) Aroma-enhancing spice, slow-release aroma-carrying particle and preparation method and application thereof
CN115337858B (en) Visual herbal fragrance slow-release particles and preparation method and application thereof
TW201328614A (en) Filter for a smoking article
CN115337859B (en) Acid modified visual fragrance slow-release particles and preparation method and application thereof
CN107663808A (en) A kind of functional plants particle cigarette coating formation paper and preparation method thereof
JP6535810B2 (en) Filter for smoking article, smoking article, and method of manufacturing filter for smoking article
CN111165869A (en) Cigarette treated by low harm cigarette increasing
CN105661637B (en) Residue porous material and application thereof after a kind of tobacco is extracted
CN109603777A (en) A kind of temperature response type cigarette discoloration adsorbent material and preparation method thereof, cigarette filter

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant