CN110747061B - Smoked plum tobacco flavoring particle material and preparation method and application thereof - Google Patents
Smoked plum tobacco flavoring particle material and preparation method and application thereof Download PDFInfo
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- CN110747061B CN110747061B CN201911102212.XA CN201911102212A CN110747061B CN 110747061 B CN110747061 B CN 110747061B CN 201911102212 A CN201911102212 A CN 201911102212A CN 110747061 B CN110747061 B CN 110747061B
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- dark plum
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, 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
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/025—Recovery by solvent extraction
-
- A—HUMAN NECESSITIES
- A24—TOBACCO; CIGARS; CIGARETTES; SIMULATED SMOKING DEVICES; SMOKERS' REQUISITES
- A24D—CIGARS; CIGARETTES; TOBACCO SMOKE FILTERS; MOUTHPIECES FOR CIGARS OR CIGARETTES; MANUFACTURE OF TOBACCO SMOKE FILTERS OR MOUTHPIECES
- A24D3/00—Tobacco smoke filters, e.g. filter-tips, filtering inserts; Filters specially adapted for simulated smoking devices; Mouthpieces for cigars or cigarettes
- A24D3/02—Manufacture of tobacco smoke filters
- A24D3/0204—Preliminary operations before the filter rod forming process, e.g. crimping, blooming
- A24D3/0212—Applying additives to filter materials
- A24D3/0225—Applying additives to filter materials with solid additives, e.g. incorporation of a granular product
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, 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
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/022—Refining
Abstract
The invention relates to a smoked plum tobacco flavoring granular material as well as a preparation method and application thereof, belonging to the technical field of cigarettes. The method comprises the steps of dark plum pretreatment, water extraction of dark plum pulp and nutlet, alcohol extraction of dark plum pulp and nutlet, concentration of an extracting solution, preparation of dark plum shell activated carbon, preparation of flavoring particle materials for cigarettes and the like. The flavoring granular material for the cigarettes prepared by the invention is used for the cigarettes, so that the fragrance of the cigarettes is fully developed, the richness and the sweet and rich taste are obviously improved, the smoke is soft and delicate, the stimulation is reduced, the smoking quality is obviously improved, the energy consumption and the production cost can be greatly reduced, the utilization rate of raw materials is improved, and the flavoring granular material has a good application prospect.
Description
Technical Field
The invention belongs to the technical field of cigarettes, and particularly relates to a smoked plum flavoring granular material for cigarettes as well as a preparation method and application thereof.
Background
Along with the increasing attention and improvement of living standard and health consciousness of people, in order to improve the smoking safety of cigarettes, harm and tar reduction become important components of Chinese cigarettes, but as the tar content of the cigarettes is gradually reduced, the herbal fragrance of the cigarettes is weakened, so that the fragrance quality and quantity of the cigarette leaf formula can be made up by adding the flavoring particle material for cigarettes into the cigarette filter stick, the effects of increasing fragrance, keeping moisture, reducing thorns and removing impurities are achieved, the cigarette fragrance is more full, the sensory quality of the cigarettes is effectively improved, and the pleasure and the satisfaction of consumers during smoking are improved.
Dark plum is neutral and sweet, mainly contains acid esters (citric acid, malic acid, and the like), saccharides (fructose, glucose, sucrose, and the like), aldehydes and ketones and other components, wherein the main functional component is organic acid, and has the physiological functions of promoting the production of body fluid to quench thirst, eliminating phlegm and stopping cough, diminishing inflammation and relieving pain, eliminating fatigue, delaying senility, and the like. The essence for tobacco has the effects of reducing stimulation, softening and smoothing smoke, weakening miscellaneous gas, improving comfort and the like. For example, the invention patent 201510336648.0 discloses a method for preparing a filter stick and a cigarette thereof, which adopts hot reflux combined with ultrasonic extraction to extract plum pulp by using glycerol triacetate, uniformly spraying a solution with the mass concentration of 2-5% of the plum pulp on a tow according to 7-8% of the weight of acetate fiber. The extract not only can improve the nicotinic acid, the fruity flavor, the production of body fluid and the aftertaste, but also has the advantages of simple process, low cost and convenient industrial production. The invention patent 201510341255.9 cleans, dries and dries the plum fruit, crushes and then carries out water reflux and enzyme preparation extraction respectively, ethanol sedimentation, water and n-butyl alcohol extraction, and propylene glycol is added after concentration to obtain the spice. Not only improves the utilization rate of the plum, but also has simple method and reduced cost. Meanwhile, the spice has strong and vivid aroma, can obviously improve the aroma quality of cigarettes, soften and smooth smoke, increase the sweet feeling of oral cavities and improve the smoke permeability. Patent 201610103679.6 the 80 mesh residue obtained after extracting fruits such as plum, apple and tomato, and KOH powder are mixed in proportion of 1:2-6, heating to 500-650 ℃ at a speed of 5-20 ℃/min in an argon atmosphere, preserving heat for 10-25min, cleaning with 5-15% HCl to remove KOH, cleaning with distilled water until the pH value is neutral, and finally drying at 110 ℃ to constant weight.
The method does not comprehensively aim at extraction and application according to different parts (pulp, kernel and shell) of the dark plum, and the yield is low. Therefore, how to overcome the defects of the prior art and improve the application range of different parts of the dark plums so as to achieve the purpose of improving the utilization rate of the dark plums is an urgent problem to be solved in the technical field of the existing cigarettes.
Disclosure of Invention
The invention aims to provide a smoked plum flavoring granular material for cigarettes as well as a preparation method and application thereof, aiming at the defects that the conventional smoked plum raw material is low in utilization rate and is not purposefully and effectively applied. The invention not only can bring better effects such as flavoring and the like to cigarettes, greatly save energy consumption, reduce production cost, but also can improve the utilization rate of the raw materials of the dark plums and expand the application approaches of the dark plums.
In order to realize the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of a smoked plum flavored granular material for cigarettes comprises the following steps:
step (1), dark plum pretreatment:
knocking dried dark plum products, sorting kernels, pulps and shells, and crushing for later use;
step (2), water extraction of dark plum pulp and kernels:
mixing the dark plum pulp obtained in the step (1), nutlet and water, sealing, standing and extracting in a shade place, filtering, and taking filtrate to obtain water extract of the dark plum pulp and the nutlet; wherein the mass ratio of the total mass of the dark plum pulp and the dark plum kernel to the water is 1:4-7;
and (3) extracting smoked plum pulp and kernels with alcohol:
mixing the solid matter filtered in the step (2) with absolute ethyl alcohol according to a mass ratio of 1:6-9, sealing, standing in a shade place for extraction, filtering, and collecting filtrate to obtain fructus mume pulp and kernel alcoholic extractive solution;
step (4), concentrating the extracting solution:
carrying out forward osmosis concentration on the water extract of the dark plum pulp and the dark plum kernel obtained in the step (2) until the solid content is 45 +/-2%, and then heating, decompressing and concentrating until the solid content is 65 +/-2% to obtain a water extract concentrate;
heating and concentrating the alcohol extract of the dark plum pulp and the dark plum kernel obtained in the step (3) under reduced pressure to enable the solid content to reach 65 +/-2% so as to obtain an alcohol extract concentrate;
step (5), preparing the dark plum shell activated carbon:
sieving the smoked plum shell particles obtained in the step (1), taking the smoked plum shell particles of 20-60 meshes, and performing activation treatment to obtain hollow porous smoked plum activated carbon particles with strong adsorption capacity;
step (6), preparation of the flavoring granular material for the cigarettes:
dissolving the ethanol extract, the water extract and the tobacco essence obtained in the step (4) in absolute ethanol, uniformly spraying the obtained ethanol solution to the 30-60-mesh dark plum activated carbon particles obtained in the step (5), and placing the particles in a shade place for balancing to obtain the smoked plum tobacco flavoring particle material;
the essence for the cigarettes is one or a mixture of more of Chinese date tincture, walnut shell extract, chamomile extract, fenugreek absolute, carotene and iris extract;
the total mass of the alcohol extract concentrate and the water extract concentrate, and the mass ratio of the tobacco essence to the dark plum activated carbon particles is 1:0.1-1:10-100;
the mass ratio of the absolute ethyl alcohol to the dark plum active carbon particles is 1:3-5.
Further, preferably, the dried dark plum product is of the first grade, and the production place is Yunnan Dali.
Further, preferably, in the step (2), 200-mesh filter cloth is adopted for filtering; in the step (3), 300-mesh filter cloth is adopted for filtration.
Further, preferably, in the step (2), the standing extraction time is 18-24h; in the step (3), standing and extracting for 12-16h; in the step (6), the standing and balancing time is 0.5-1h.
Further, it is preferable that the specific method of the activation treatment is:
mixing the dark plum shell particles obtained in the step (1) with ZnCl with the mass concentration of 30-50% 2 Mixing the solutions according to the mass ratio of 2-4 to 1, activating at 600-700 ℃ for 10-30min, eluting with deionized water to neutrality, and drying at 100-110 ℃ for 1-2h to obtain the dark plum activated carbon particles.
The invention also provides the smoked plum tobacco flavoring granular material prepared by the preparation method of the smoked plum tobacco flavoring granular material.
The invention also provides application of the smoked plum tobacco flavoring granular material in preparation of a cigarette additive.
Preferably, the application method comprises the following steps: adding the added amount of the flavoring granular material for the smoked plum cigarettes into a binary composite filter stick or a ternary composite filter stick; when the additive is added into a binary composite filter stick, the additive is added according to the additive amount of 1.5-3mg/mm, and the additive length is 10-15mm; when the additive is added into the ternary composite filter stick, the additive is added according to the addition amount of 20-50 mg/cig.
In the step (2), the mass ratio of the total mass of the dark plum pulp and the dark plum kernel to the water is 1:4-7, wherein the mass of the dark plum pulp and the kernel is not specially limited, and the dark plum pulp and the kernel can be used according to the proportion of the kernel and the pulp separated from each dark plum. For example, 1000 pieces of dark plums are used as raw materials, and the raw materials are the pulp of the 1000 pieces of dark plums and the 1000 pieces of dark plum kernels.
In the step (6), the total mass of the alcohol extract and the water extract, the mass ratio of the tobacco essence to the dark plum activated carbon particles is 1:0.1-1:10-100. The amount of the alcohol extract concentrate and the water extract concentrate is not particularly limited in the present invention, for example, 1000 pieces of smoked plums are used as the raw material, and the 1000 pieces of smoked plums are the pulp of the 1000 pieces of smoked plums and the alcohol extract concentrate and the water extract concentrate of the 1000 pieces of smoked plums obtained according to the steps (2) to (4).
The water in step (2) of the present invention may be pure water or tap water.
The positive osmosis concentration in the step (4) adopts a drawing agent comprising high fructose corn syrup and saturated saline solution (the mass ratio is 3: concentrating 0.5-5, and collecting the concentrated solution when the solid content reaches 45 + -2%.
In the invention, the reduced pressure concentration is carried out under the heating condition, and the heating temperature of the reduced pressure concentration of the water extract is preferably 50-70 ℃; the heating temperature of the alcohol extract after decompression concentration is as follows: 40-60 ℃.
The invention can be applied to cigarettes to effectively increase the fruit sweet and fragrance, not only reduce the stimulation and soften the smoke, but also cover or remove the miscellaneous gas, improve the coordination sense and the comfort sense, greatly improve the smoking quality of the cigarettes compared with the prior products and have good application prospect.
The shade place is a dark and dry place.
Compared with the prior art, the invention has the beneficial effects that:
1. the dark plum aqueous extract and the dark plum alcohol extract prepared by the invention have complete and light fragrance components and obvious characteristic fragrance and effect;
2. the flavoring granular material for the cigarettes prepared by the invention can obviously and effectively increase the fruity and sweet aroma, not only can reduce the stimulation, soften and refine the smoke, cover or remove the miscellaneous gas, improve the coordination sense and comfort sense of the smoke, and greatly improve the smoking quality.
3. The flavoring granular material for the cigarettes prepared by the invention not only can greatly improve the utilization rate of the raw materials of the dark plums and keep the small molecular fragrant substances of the dark plums as much as possible, but also has simpler preparation process (the dark plum pulp, the nutlet and the shell can be purchased separately, and the shell can be sent to prepare the active carbon), can save energy consumption, greatly reduces the cost and is convenient for large-scale and industrial production.
Detailed Description
The present invention will be described in further detail with reference to examples.
It will be appreciated by those skilled in the art that the following examples are illustrative of the invention only and should not be taken as limiting the scope of the invention. The examples do not specify particular techniques or conditions, and are performed according to the techniques or conditions described in the literature in the art or according to the product specifications. The materials or equipment used are not indicated by manufacturers, but are all conventional products available by purchase.
The percentage numbers are percentages by mass unless otherwise indicated.
In the embodiment of the invention, the raw materials are preferably first-grade dark plum dried products produced by Yunan Dali, the diameter of the fruit particles is about 3.3cm,346 particles/kg, and the mass percentages of pulp, kernel, shell and loss in dark plum obtained by knocking, sorting and weighing are 31.65%, 7.77%, 58.97% and 1.36% respectively.
Example 1
A preparation method of a smoked plum flavored granular material for cigarettes comprises the following steps:
step (1), dark plum pretreatment:
knocking dried dark plum products, sorting kernels, pulps and shells, and crushing for later use;
step (2), water extraction of dark plum pulp and kernels:
mixing the dark plum pulp obtained in the step (1), nutlet and water, sealing, standing and extracting in a shade place, filtering, and taking filtrate to obtain water extract of the dark plum pulp and the nutlet; wherein the mass ratio of the total mass of the dark plum pulp and the dark plum kernel to the water is 1:5;
and (3) alcohol extraction of dark plum pulp and kernels:
mixing the solid matter filtered in the step (2) with absolute ethyl alcohol according to a mass ratio of 1:7, sealing and placing the mixture in a shade place for standing and extracting after mixing, and taking filtrate after filtering to obtain alcohol extract of dark plum pulp and nutlet;
step (4), concentrating the extracting solution:
carrying out forward osmosis concentration on the water extract of the dark plum pulp and the nuts obtained in the step (2) until the solid content is 45 +/-1%, and then heating at 50 ℃ and carrying out reduced pressure concentration until the solid content is 65 +/-1% to obtain a water extract concentrate;
heating and concentrating the alcohol extract of the dark plum pulp and the dark plum kernel obtained in the step (3) at 40 ℃ under reduced pressure to enable the solid content to reach 65 +/-1% so as to obtain an alcohol extract concentrate;
step (5), preparing the dark plum shell activated carbon:
sieving the smoked plum shell particles obtained in the step (1), taking 20-60 meshes, and performing activation treatment to obtain hollow porous smoked plum activated carbon particles with strong adsorption capacity;
step (6), preparation of the flavoring granular material for cigarettes:
dissolving the ethanol extract, the water extract and the tobacco essence obtained in the step (4) in absolute ethyl alcohol, uniformly spraying the obtained ethanol solution to the smoked plum active carbon particles with the particle size of 30-60 meshes obtained in the step (5), and placing the smoked plum active carbon particles in a shade place for balancing to obtain smoked plum flavored particle materials for tobacco;
the tobacco essence is Chinese date tincture;
the total mass of the ethanol extract concentrate and the water extract concentrate, and the mass ratio of the tobacco essence to the dark plum activated carbon particles is 1:0.1:10;
the mass ratio of the absolute ethyl alcohol to the dark plum activated carbon particles is 1:5.
adding the added amount of the flavoring granular material for the smoked plum cigarettes into a binary composite filter stick or a ternary composite filter stick; when the additive is added into a binary composite filter stick, the additive is added according to the addition amount of 2mg/mm, and the addition length is 13mm; when the additive is added into the ternary composite filter stick, the additive is added according to the addition amount of 30 mg/cig.
Example 2
A preparation method of a smoked plum flavored granular material for cigarettes comprises the following steps:
step (1), dark plum pretreatment:
knocking dried dark plum products, sorting kernels, pulps and shells, and crushing for later use;
step (2), water extraction of dark plum pulp and kernels:
mixing the dark plum pulp obtained in the step (1), nutlet and water, sealing, standing and extracting in a shade place, filtering, and taking filtrate to obtain water extract of the dark plum pulp and the nutlet; wherein the mass ratio of the total mass of the dark plum pulp and the dark plum kernel to the water is 1:4;
and (3) alcohol extraction of dark plum pulp and kernels:
mixing the solid matter filtered in the step (2) with absolute ethyl alcohol according to the mass ratio of 1:6, sealing, placing in a shade place, standing, extracting, filtering, and taking filtrate to obtain fructus mume pulp and kernel ethanol extractive solution;
step (4), concentrating the extracting solution:
carrying out forward osmosis concentration on the water extract of the dark plum pulp and the nuts obtained in the step (2) until the solid content is 45 +/-2%, and then heating at 70 ℃ and carrying out reduced pressure concentration until the solid content is 65 +/-2% to obtain a water extract concentrate;
heating and concentrating the alcohol extract of the dark plum pulp and the dark plum kernel obtained in the step (3) at 60 ℃ under reduced pressure to enable the solid content to reach 65 +/-2% so as to obtain an alcohol extract concentrate;
step (5), preparing the dark plum shell activated carbon:
sieving the smoked plum shell particles obtained in the step (1), taking 20-60 meshes, and performing activation treatment to obtain hollow porous smoked plum activated carbon particles with strong adsorption capacity;
step (6), preparation of the flavoring granular material for cigarettes:
dissolving the ethanol extract, the water extract and the tobacco essence obtained in the step (4) in absolute ethanol, uniformly spraying the obtained ethanol solution to the 30-60-mesh dark plum activated carbon particles obtained in the step (5), and placing the particles in a shade place for balancing to obtain the smoked plum tobacco flavoring particle material;
the tobacco essence is a walnut shell extract;
the total mass of the alcohol extract concentrate and the water extract concentrate, and the mass ratio of the tobacco essence to the dark plum activated carbon particles is 1:1:100, respectively;
the mass ratio of the absolute ethyl alcohol to the dark plum active carbon particles is 1:4.
the dried dark plum product is classified as the first grade, and the production place is Yunan Dali.
In the step (2), 200-mesh filter cloth is adopted for filtering; in the step (3), 300-mesh filter cloth is adopted for filtration.
In the step (2), standing and extracting for 18h; in the step (3), standing and extracting for 12 hours; in the step (6), the standing and balancing time is 0.5h.
The specific method of the activation treatment comprises the following steps:
mixing the dark plum shell particles obtained in the step (1) with ZnCl with the mass concentration of 30 percent 2 And (2) mixing the solutions according to a mass ratio of 2.
Adding the adding amount of the smoked plum tobacco flavoring particle material into a binary composite filter stick or a ternary composite filter stick; when the additive is added into a binary composite filter stick, the additive is added according to the addition amount of 1.5mg/mm, and the addition length is 10mm; when the additive is added into the ternary composite filter stick, the additive amount is 20 mg/cig.
Example 3
A preparation method of a smoked plum flavored granular material for cigarettes comprises the following steps:
step (1), dark plum pretreatment:
knocking dried dark plum products, sorting kernels, pulps and shells, and crushing for later use;
step (2), water extraction of dark plum pulp and kernels:
mixing the dark plum pulp obtained in the step (1), nutlet and water, sealing, standing and extracting in a shade place, filtering, and taking filtrate to obtain water extract of the dark plum pulp and the nutlet; wherein the mass ratio of the total mass of the dark plum pulp and the dark plum kernel to the water is 1:7;
and (3) extracting smoked plum pulp and kernels with alcohol:
mixing the solid matter filtered in the step (2) with absolute ethyl alcohol according to the mass ratio of 1:9, sealing and placing the mixture in a shade place for standing and extracting after mixing, filtering and taking filtrate to obtain alcohol extract of dark plum pulp and nutlet;
step (4), concentrating the extracting solution:
carrying out forward osmosis concentration on the water extract of the dark plum pulp and the nutlet obtained in the step (2) until the solid content is 45 +/-0.5%, and then heating at 60 ℃ and carrying out reduced pressure concentration until the solid content is 65 +/-0.5% to obtain a water extract concentrate;
heating and concentrating the alcohol extract of the dark plum pulp and the dark plum kernel obtained in the step (3) at 50 ℃ under reduced pressure to enable the solid content to reach 65 +/-0.5% so as to obtain an alcohol extract concentrate;
step (5), preparing the dark plum shell activated carbon:
sieving the smoked plum shell particles obtained in the step (1), taking the smoked plum shell particles of 20-60 meshes, and performing activation treatment to obtain hollow porous smoked plum activated carbon particles with strong adsorption capacity;
step (6), preparation of the flavoring granular material for the cigarettes:
dissolving the ethanol extract, the water extract and the tobacco essence obtained in the step (4) in absolute ethyl alcohol, uniformly spraying the obtained ethanol solution to the smoked plum active carbon particles with the particle size of 30-60 meshes obtained in the step (5), and placing the smoked plum active carbon particles in a shade place for balancing to obtain smoked plum flavored particle materials for tobacco;
the tobacco essence is a chamomile extract;
the total mass of the alcohol extract concentrate and the water extract concentrate, and the mass ratio of the tobacco essence to the dark plum activated carbon particles is 1:0.3:32.5;
the mass ratio of the absolute ethyl alcohol to the dark plum active carbon particles is 1:3.
the grade of the dried dark plum product is first grade, and the producing area is Yunnan Dali.
In the step (2), 200-mesh filter cloth is adopted for filtering; in the step (3), 300-mesh filter cloth is adopted for filtration.
In the step (2), standing and extracting for 24 hours; in the step (3), standing and extracting for 16h; in the step (6), the standing and balancing time is 1h.
The specific method of the activation treatment comprises the following steps:
mixing the dark plum shell particles obtained in the step (1) with ZnCl with the mass concentration of 50% 2 Mixing the solutions according to a mass ratio of 4.
Adding the added amount of the flavoring granular material for the smoked plum cigarettes into a binary composite filter stick or a ternary composite filter stick; when the additive is added into a binary composite filter stick, the additive is added according to the addition amount of 3mg/mm, and the addition length is 15mm; when the additive is added into the ternary composite filter stick, the additive amount is 50 mg/cig.
Example 4
A preparation method of a smoked plum flavored granular material for cigarettes comprises the following steps:
step (1), dark plum pretreatment:
knocking dried dark plum products, sorting kernels, pulps and shells, and crushing for later use;
step (2), water extraction of dark plum pulp and kernels:
mixing the dark plum pulp obtained in the step (1), nutlet and water, sealing, standing and extracting in a shade place, filtering, and taking filtrate to obtain water extract of the dark plum pulp and the nutlet; wherein the mass ratio of the total mass of the dark plum pulp and the dark plum kernel to the water is 1:6;
and (3) extracting smoked plum pulp and kernels with alcohol:
mixing the solid matter filtered in the step (2) with absolute ethyl alcohol according to a mass ratio of 1:8, sealing and placing the mixture in a shade place for standing and extracting after mixing, and taking filtrate after filtering to obtain alcohol extract of dark plum pulp and nutlet;
step (4), concentrating the extracting solution:
carrying out forward osmosis concentration on the water extract of the dark plum pulp and the nuts obtained in the step (2) until the solid content is 45 +/-2%, and then heating at 60 ℃ and carrying out reduced pressure concentration until the solid content is 65 +/-0.5% to obtain a water extract concentrate;
heating and decompressing and concentrating the alcohol extract of the dark plum pulp and the nuts obtained in the step (3) at 50 ℃ to enable the solid content to reach 65 +/-2% so as to obtain alcohol extract concentrate;
step (5), preparing the dark plum shell activated carbon:
sieving the smoked plum shell particles obtained in the step (1), taking the smoked plum shell particles of 20-60 meshes, and performing activation treatment to obtain hollow porous smoked plum activated carbon particles with strong adsorption capacity;
step (6), preparation of the flavoring granular material for cigarettes:
dissolving the ethanol extract, the water extract and the tobacco essence obtained in the step (4) in absolute ethyl alcohol, uniformly spraying the obtained ethanol solution to the smoked plum active carbon particles with the particle size of 30-60 meshes obtained in the step (5), and placing the smoked plum active carbon particles in a shade place for balancing to obtain smoked plum flavored particle materials for tobacco;
the essence for cigarettes is a mixture of fenugreek absolute, carotene and an iris tectorum extract, and the mass ratio is 1:1:1;
the total mass of the alcohol extract concentrate and the water extract concentrate, and the mass ratio of the tobacco essence to the dark plum activated carbon particles is 1:0.4:70;
the mass ratio of the absolute ethyl alcohol to the dark plum active carbon particles is 1:4.5.
the dried dark plum product is classified as the first grade, and the production place is Yunan Dali.
In the step (2), 200-mesh filter cloth is adopted for filtering; in the step (3), 300-mesh filter cloth is adopted for filtration.
In the step (2), standing and extracting for 20 hours; in the step (3), standing and extracting for 15h; in the step (6), the standing and balancing time is 0.8h.
The specific method of the activation treatment comprises the following steps:
mixing the dark plum shell particles obtained in the step (1) with ZnCl with the mass concentration of 40% 2 And mixing the solutions according to a mass ratio of 3.
Adding the added amount of the flavoring granular material for the smoked plum cigarettes into a binary composite filter stick or a ternary composite filter stick; when the additive is added into a binary composite filter stick, the additive is added according to the addition amount of 2mg/mm, and the addition length is 13mm; when the additive is added into the ternary composite filter stick, the additive is added according to the addition amount of 40 mg/cig.
Application example 1
A preparation method of a smoked plum flavored granular material for cigarettes comprises the following steps:
step (1), dark plum pretreatment:
knocking dried dark plum products, sorting kernels, pulps and shells, and crushing for later use;
step (2), water extraction of dark plum pulp and kernels:
mixing the dark plum pulp, the kernel and water obtained in the step (1), sealing, standing and extracting for 18h in a shade place, filtering by adopting 200-mesh filter cloth, and taking filtrate to obtain water extract of the dark plum pulp and the kernel, wherein the solid content is 13.7% by detection, and the yield is 38.30%; wherein the mass ratio of the total mass of the dark plum pulp and the dark plum kernel to the water is 1:4;
and (3) alcohol extraction of dark plum pulp and kernels:
mixing the solid matter filtered in the step (2) with absolute ethyl alcohol according to a mass ratio of 1:9, sealing and placing the mixture in a shade place for standing and extracting for 12 hours, filtering the mixture by adopting 300-mesh filter cloth, and taking filtrate to obtain alcohol extract of dark plum pulp and nutlet;
step (4), concentrating the extracting solution:
carrying out forward osmosis concentration on the water extract of the dark plum pulp and the dark plum kernel obtained in the step (2) (the mass ratio of a drawing agent to the saturated salt water is 3;
heating and concentrating the alcohol extract of the dark plum pulp and the dark plum kernel obtained in the step (3) at 50 ℃ under reduced pressure to enable the solid content to reach 65 +/-2% so as to obtain an alcohol extract concentrate;
the yield of the ethanol extract concentrate is 13.45 percent, and the comprehensive yield of the water extract and the ethanol extract concentrate is 51.75 percent;
step (5), preparing the dark plum shell activated carbon:
sieving the smoked plum shell particles obtained in the step (1), taking the smoked plum shell particles of 20-60 meshes, and performing activation treatment to obtain hollow porous smoked plum activated carbon particles with strong adsorption capacity;
step (6), preparation of the flavoring granular material for the cigarettes:
dissolving the ethanol extract, the water extract and the tobacco essence obtained in the step (4) in absolute ethyl alcohol, uniformly spraying the obtained ethanol solution to the smoked plum active carbon particles with the particle size of 30-60 meshes obtained in the step (5), and placing the smoked plum active carbon particles in a shade place for balancing for 1 hour to obtain smoked plum tobacco flavoring particle materials;
the essence for the cigarettes is Chinese date tincture;
the total mass of the alcohol extract concentrate and the water extract concentrate, and the mass ratio of the tobacco essence to the dark plum activated carbon particles is 1:0.1:13.75;
the mass ratio of the absolute ethyl alcohol to the dark plum active carbon particles is 1:5.
the grade of the dried dark plum product is first grade, and the production place is Yunnan Dali.
The specific method of the activation treatment comprises the following steps:
mixing the dark plum shell particles obtained in the step (1) with ZnCl with the mass concentration of 30% 2 Mixing the solutions according to a mass ratio of 2:1, activating at 600 ℃ for 10min, eluting with deionized water to neutrality, and drying at 110 ℃ for 1h to obtain the dark plum activated carbon particles, wherein the yield is 50.36%, and the specific surface area is 1065.17m 2 /g。
Preparing a filter rod by adding the flavoring particles for the cigarettes obtained in the step (6) according to the adding amount of 2.0mg/mm and the adding length of 10mm, rolling the cigarettes (refer to a certain grade of cigarettes produced in Yunyan, the same below), taking the cigarettes added with the particle materials for the cigarettes as samples, and evaluating according to related sensory quality standards, wherein compared with the control samples (no particle materials are added, the same below), sensory evaluation results are as follows:
the richness of the cigarette fragrance is increased and the cigarette is developed thoroughly, the sweetness and sweetness of the cigarette are improved obviously, the taste is fine and soft, and the stimulation is weakened.
Application example 2
A preparation method of a smoked plum flavored granular material for cigarettes comprises the following steps:
step (1), dark plum pretreatment:
knocking dried dark plum products, sorting kernels, pulps and shells, and crushing for later use;
step (2), water extraction of dark plum pulp and kernels:
mixing the dark plum pulp, the kernel and water obtained in the step (1), sealing, standing and extracting for 18h in a shade place, filtering by adopting 200-mesh filter cloth, and taking filtrate to obtain water extract of the dark plum pulp and the kernel, wherein the solid content is 11.7% and the extraction rate is 44.22% by detection; wherein the mass ratio of the total mass of the dark plum pulp and the dark plum kernel to the water is 1:5;
and (3) alcohol extraction of dark plum pulp and kernels:
mixing the solid matter filtered in the step (2) with absolute ethyl alcohol according to a mass ratio of 1:8, sealing and placing the mixture in a shade place for standing and extracting for 12 hours, filtering the mixture by adopting 300-mesh filter cloth, and taking filtrate to obtain alcohol extract of dark plum pulp and nutlet;
step (4), concentrating the extracting solution:
carrying out forward osmosis concentration on the water extract of the dark plum pulp and the kernel obtained in the step (2) until the solid content is 45 +/-2%, and then heating at 60 ℃ and carrying out reduced pressure concentration until the solid content is 65 +/-2% to obtain a water extract concentrate;
heating and concentrating the alcohol extract of the dark plum pulp and the dark plum kernel obtained in the step (3) at 50 ℃ under reduced pressure to enable the solid content to reach 65 +/-2%, and recycling the ethanol recovered from the alcohol extract concentrate;
the yield of the alcohol extract concentrate is 12.51 percent, and the comprehensive yield of the water extract concentrate and the alcohol extract concentrate is 56.72 percent;
step (5), preparing the dark plum shell activated carbon:
sieving the smoked plum shell particles obtained in the step (1), taking the smoked plum shell particles of 20-60 meshes, and performing activation treatment to obtain hollow porous smoked plum activated carbon particles with strong adsorption capacity;
step (6), preparation of the flavoring granular material for the cigarettes:
dissolving the ethanol extract, the water extract and the tobacco essence obtained in the step (4) in absolute ethanol, uniformly spraying the obtained ethanol solution on the dark plum active carbon particles with the particle size of 30-60 meshes obtained in the step (5), and placing the dark plum active carbon particles in a shade place for balancing for 1h to obtain the smoked plum flavoring particle material for tobacco;
the essence for the cigarette is walnut shell extract;
the total mass of the ethanol extract concentrate and the water extract concentrate, and the mass ratio of the tobacco essence to the dark plum activated carbon particles is 1:0.2:20;
the mass ratio of the absolute ethyl alcohol to the dark plum active carbon particles is 1:4.
the grade of the dried dark plum product is first grade, and the production place is Yunnan Dali.
The specific method of the activation treatment comprises the following steps:
mixing the dark plum shell particles obtained in the step (1) with ZnCl with the mass concentration of 35% 2 Mixing the solutions according to a mass ratio of 3 2 /g。
Preparation of flavored particle filter sticks and cigarette evaluation thereof: preparing a filter stick by adding the cigarette flavoring particles obtained in the step (6) according to the adding amount of 1.8mg/mm and the adding length of 12mm, rolling cigarettes, taking the cigarettes added with the cigarette particle materials as samples, evaluating according to relevant sensory quality standards, and comparing with control cigarettes, obtaining sensory evaluation results as follows:
the richness of the cigarette fragrance is increased and the cigarette is developed thoroughly, the sweetness and the taste of the cigarette are obviously increased, the cigarette is fine and smooth, and the stimulation is weakened.
Application example 3
A preparation method of a smoked plum flavored granular material for cigarettes comprises the following steps:
step (1), dark plum pretreatment:
knocking dried dark plum products, sorting kernels, pulps and shells, and crushing for later use;
step (2), water extraction of dark plum pulp and kernels:
mixing the dark plum pulp, the kernel and water obtained in the step (1), sealing, standing and extracting for 18h in a shade place, filtering by adopting 200-mesh filter cloth, and taking filtrate to obtain water extract of the dark plum pulp and the kernel, wherein the solid content is 10.7% and the extraction rate is 51.94% by detection; wherein the mass ratio of the total mass of the dark plum pulp and the dark plum kernel to the water is 1:6;
and (3) alcohol extraction of dark plum pulp and kernels:
mixing the solid matter filtered in the step (2) with absolute ethyl alcohol according to a mass ratio of 1:7, sealing and placing the mixture in a shade place for standing and extracting for 16 hours, filtering the mixture by adopting 300-mesh filter cloth, and taking filtrate to obtain alcohol extract of dark plum pulp and nutlet;
step (4), concentrating the extracting solution:
carrying out forward osmosis concentration on the water extract of the dark plum pulp and the kernel obtained in the step (2) until the solid content is 45 +/-2%, and then heating at 60 ℃ and carrying out reduced pressure concentration until the solid content is 65 +/-2% to obtain a water extract concentrate;
heating and concentrating the alcohol extract of the dark plum pulp and the nuts obtained in the step (3) at 50 ℃ under reduced pressure to ensure that the solid content of the alcohol extract reaches 65 +/-2 percent, and recycling the ethanol recovered from the obtained alcohol extract;
the yield of the ethanol extract concentrate is 9.59 percent, and the comprehensive yield of the water extract and the ethanol extract concentrate is 61.53 percent;
step (5), preparing the dark plum shell activated carbon:
sieving the smoked plum shell particles obtained in the step (1), taking 20-60 meshes, and performing activation treatment to obtain hollow porous smoked plum activated carbon particles with strong adsorption capacity;
step (6), preparation of the flavoring granular material for cigarettes:
dissolving the ethanol extract, the water extract and the tobacco essence obtained in the step (4) in absolute ethyl alcohol, uniformly spraying the obtained ethanol solution to the dark plum active carbon particles with the particle size of 30-60 meshes obtained in the step (5), and placing the dark plum active carbon particles in a shade place for balancing for 1 hour to obtain a dark plum tobacco flavoring particle material;
the tobacco essence is walnut shell extract and chamomile extract (mass ratio 3;
the total mass of the alcohol extract concentrate and the water extract concentrate, and the mass ratio of the tobacco essence to the dark plum activated carbon particles is 1:0.3:32.5;
the mass ratio of the absolute ethyl alcohol to the dark plum active carbon particles is 1:3.
the grade of the dried dark plum product is first grade, and the production place is Yunnan Dali.
The specific method of the activation treatment comprises the following steps:
mixing the dark plum shell particles obtained in the step (1) with ZnCl with the mass concentration of 40% 2 Mixing the solutions according to a mass ratio of 4; the yield thereof was 58.19%, and the specific surface area thereof was 1209.35m 2 /g。
Preparation of flavored particle filter sticks and cigarette evaluation thereof: preparing a filter rod by adding the flavoring particles for the cigarettes obtained in the step (6) according to the adding amount of 1.5mg/mm and the adding length of 15mm, rolling the cigarettes, taking the cigarettes added with the tobacco particle materials as samples, evaluating according to related sensory quality standards, and comparing with the control samples, obtaining sensory evaluation results as follows:
the cigarette has the advantages of full-blown cigarette fragrance, remarkably improved richness and sweet and rich taste, smoothness, mellowness and reduced irritation.
Application example 4
A preparation method of a smoked plum flavored granular material for cigarettes comprises the following steps:
step (1), dark plum pretreatment:
knocking dried dark plum products, sorting kernels, pulps and shells, and crushing for later use;
step (2), water extraction of dark plum pulp and kernels:
mixing the dark plum pulp, the nuts and water obtained in the step (1), sealing, placing in a shade place, standing and extracting for 18 hours, filtering by adopting 200-mesh filter cloth, and taking filtrate to obtain water extract of the dark plum pulp and the nuts; wherein the mass ratio of the total mass of the dark plum pulp and the dark plum kernel to the water is 1:7, detecting that the solid content is 9.7 percent, and the yield is 56.08 percent;
and (3) extracting smoked plum pulp and kernels with alcohol:
mixing the solid matter filtered in the step (2) with absolute ethyl alcohol according to a mass ratio of 1:6, sealing and placing the mixture in a shade place for standing and extracting for 12 hours, filtering the mixture by adopting 300-mesh filter cloth, and taking filtrate to obtain alcohol extract of dark plum pulp and nutlet;
step (4), concentrating the extracting solution:
carrying out forward osmosis concentration on the water extract of the dark plum pulp and the kernel obtained in the step (2) until the solid content is 45 +/-2%, and then heating at 65 ℃ and carrying out reduced pressure concentration until the solid content is 65 +/-2% to obtain a water extract concentrate;
heating and concentrating the alcohol extract of the dark plum pulp and the dark plum kernel obtained in the step (3) at 45 ℃ under reduced pressure to enable the solid content to reach 65 +/-2%, and recycling the ethanol recovered from the alcohol extract concentrate;
the yield of the ethanol extract concentrate is 8.49 percent, and the comprehensive yield of the water extract and the ethanol extract concentrate is 64.57 percent;
step (5), preparing the dark plum shell activated carbon:
sieving the smoked plum shell particles obtained in the step (1), taking 20-60 meshes, and performing activation treatment to obtain hollow porous smoked plum activated carbon particles with strong adsorption capacity;
step (6), preparation of the flavoring granular material for cigarettes:
dissolving the ethanol extract, the water extract and the tobacco essence obtained in the step (4) in absolute ethanol, uniformly spraying the obtained ethanol solution on the dark plum active carbon particles with the particle size of 30-60 meshes obtained in the step (5), and placing the dark plum active carbon particles in a shade place for balancing for 1h to obtain the smoked plum flavoring particle material for tobacco;
the essence for cigarettes is a mixture of jujube tincture, carotene and iris extract (mass ratio is 1;
the total mass of the alcohol extract concentrate and the water extract concentrate, and the mass ratio of the tobacco essence to the dark plum activated carbon particles is 1:0.4:70;
the mass ratio of the absolute ethyl alcohol to the dark plum active carbon particles is 1:3.
the grade of the dried dark plum product is first grade, and the production place is Yunnan Dali.
The specific method of the activation treatment comprises the following steps:
subjecting the product obtained in step (1)Smoked plum shell particles and ZnCl with mass concentration of 50% 2 Mixing the solutions according to a mass ratio of 4 2 /g。
Preparation of flavored particle filter sticks and cigarette evaluation thereof: and (3) rolling the ternary filter stick and the cigarette thereof by using the flavoring particles for the cigarette obtained in the step (6) according to the addition of 25mg/cig, taking the cigarette added with the cigarette particle material as a sample, and evaluating according to a relevant sensory quality standard, wherein the sensory evaluation result is as follows compared with a control sample cigarette:
the cigarette has the advantages of full-blown fragrance, obviously increased richness and sweetness, fineness, elegance and reduced irritation.
Comparative test
Comparative example 1
Comparative example 1 differs from the process of the invention in that: if the smoked plum crushed particles are directly flavored, the other related cigarette samples are prepared in the same application example.
The results show that: the dark plum shell particles are not carbonized and activated, a mutually communicated porous hierarchical structure is not formed, the spice adsorption capacity is weak, the perfuming effect is not obvious, and the smoke fragrance is not rich, fine, elegant and transparent.
Comparative example 2
Comparative example 2 differs from the process of the invention in that: if the smoked plum crushed particles are subjected to boiling dry perfuming and granulation, other related cigarette samples are prepared in the same application example.
The results show that: the smoked plum flavored particles are not uniformly molded (a part of shells, pulps and nuts are molded respectively), the yield is not high (less than or equal to 35%), the shell particles are not carbonized and activated, a mutually communicated porous hierarchical structure is not formed, the spice adsorption capacity is weak, the flavoring effect is not remarkable, and the tobacco fragrance is not rich, fine, smooth and permeable.
Comparative example 3
Comparative example 3 differs from the process of the invention in that: if the smoked plum shell particles are only made into carbonized materials (subsequent treatments such as activation and the like are not carried out), the preparation of other related cigarette samples is the same as the application example.
The results show that: the smoked plum shell carbonized particle material has few holes, does not form a high specific surface, has weak adsorption capacity, has insignificant perfuming effect, and has insufficient tobacco fragrance, fineness, smoothness and hair penetration.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (8)
1. A preparation method of a smoked plum flavoring granular material for cigarettes is characterized by comprising the following steps:
step (1), dark plum pretreatment:
knocking dried dark plum products, sorting kernels, pulps and shells, and crushing for later use;
step (2), water extraction of dark plum pulp and kernels:
mixing the dark plum pulp obtained in the step (1), nutlet and water, sealing, standing and extracting in a shade place, filtering, and taking filtrate to obtain water extract of the dark plum pulp and the nutlet; wherein the mass ratio of the total mass of the dark plum pulp and the dark plum kernel to the water is 1:4-7;
and (3) alcohol extraction of dark plum pulp and kernels:
mixing the solid matter filtered in the step (2) with absolute ethyl alcohol according to a mass ratio of 1:6-9, sealing, standing in a shade place, filtering, and collecting filtrate to obtain fructus mume pulp and kernel ethanol extractive solution;
step (4), concentrating the extracting solution:
carrying out forward osmosis concentration on the water extract of the dark plum pulp and the dark plum kernel obtained in the step (2) until the solid content is 45 +/-2%, and then heating, decompressing and concentrating until the solid content is 65 +/-2% to obtain a water extract concentrate;
heating and concentrating the alcohol extract of the dark plum pulp and the dark plum kernel obtained in the step (3) under reduced pressure to enable the solid content to reach 65 +/-2% so as to obtain an alcohol extract concentrate;
step (5), preparing the dark plum shell activated carbon:
sieving the smoked plum shell particles obtained in the step (1), taking the smoked plum shell particles of 20-60 meshes, and performing activation treatment to obtain hollow porous smoked plum activated carbon particles with strong adsorption capacity;
step (6), preparation of the flavoring granular material for the cigarettes:
dissolving the ethanol extract, the water extract and the tobacco essence obtained in the step (4) in absolute ethanol, uniformly spraying the obtained ethanol solution to the dark plum activated carbon particles obtained in the step (5), and standing and balancing in a shade place to obtain a smoked plum tobacco flavoring particle material;
the essence for the cigarettes is one or a mixture of more of Chinese date tincture, walnut shell extract, chamomile extract, fenugreek absolute, carotene and iris extract;
the total mass of the alcohol extract concentrate and the water extract concentrate, and the mass ratio of the tobacco essence to the dark plum activated carbon particles is 1:0.1-1:10-100;
the mass ratio of the absolute ethyl alcohol to the dark plum activated carbon particles is 1:3-5.
2. The preparation method of the smoked plum flavored granular material for the smoked plum claim 1, wherein the smoked plum dry product is of the first grade, and the production place is Yunnan Dali.
3. The preparation method of the smoked plum flavored granular material for cigarettes as claimed in claim 1, wherein in the step (2), 200-mesh filter cloth is adopted for filtering; in the step (3), 300-mesh filter cloth is adopted for filtration.
4. The preparation method of the perfuming granular material for smoked plum cigarettes according to claim 1, wherein in the step (2), the standing extraction time is 18-24h; in the step (3), standing and extracting for 12-16h; in the step (6), the standing and balancing time is 0.5-1h.
5. The preparation method of the smoked plum flavored granular material for cigarettes according to claim 1, wherein the specific method of activation treatment comprises the following steps:
mixing the dark plum shell particles obtained in the step (1) with ZnCl with the mass concentration of 30-50% 2 Mixing the solutions according to the mass ratio of 2-4 to 1, activating at 600-700 ℃ for 10-30min, eluting with deionized water to neutrality, and drying at 100-110 ℃ for 1-2h to obtain the dark plum activated carbon particles.
6. The smoked plum tobacco flavoring granular material prepared by the preparation method of the smoked plum tobacco flavoring granular material as claimed in any one of claims 1 to 5.
7. The smoked plum flavored granular material for cigarettes as claimed in claim 6 is applied to preparation of cigarette additives.
8. The smoked plum tobacco flavoring granular material as the application of the smoked plum tobacco flavoring granular material as the cigarette additive, which is characterized in that the smoked plum tobacco flavoring granular material is added into a binary composite filter stick or a ternary composite filter stick; when the additive is added into the binary composite filter stick, the additive is added according to the additive amount of 1.5-3mg/mm, and the adding length is 10-15mm; when the additive is added into the ternary composite filter stick, the additive is added according to the addition amount of 20-50 mg/cig.
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| CN111972706A (en) * | 2020-08-27 | 2020-11-24 | 广西中烟工业有限责任公司 | Preparation method of chestnut shell activated carbon binary composite flavored filter stick |
| CN112646661A (en) * | 2020-12-15 | 2021-04-13 | 云南中烟新材料科技有限公司 | Preparation method and application of smoked plum tobacco flavor |
| CN113180293A (en) * | 2021-04-26 | 2021-07-30 | 河南中烟工业有限责任公司 | Fiber for filter stick |
| CN113180290A (en) * | 2021-04-26 | 2021-07-30 | 河南中烟工业有限责任公司 | Composite filter stick and preparation method |
| CN113455699A (en) * | 2021-07-12 | 2021-10-01 | 河南中烟工业有限责任公司 | Heating cigarette with uniform fragrance release amount by mouth |
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